#========================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and Characterization of One-Dimensional Coordination Polymers based on Self-Assembling, Heteroleptic Copper Dipyrromethene Complexes ; loop _publ_author_name _publ_author_address 'Cohen, Seth M.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; 'Halper, Sara R.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; 'Malachowski, Mitchell R.' ; Department of Chemistry University of San Diego San Diego CA 92110-2492 USA ; 'Delaney, Heather M.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; #========================================================================= data_[Cu(4-pyrdpm)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 Cu N6' _chemical_formula_weight 504.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Aba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, z+1/2' _cell_length_a 8.9282(7) _cell_length_b 8.9150(7) _cell_length_c 28.113(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2237.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 1.007 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.6601 _exptl_absorpt_correction_T_max 0.8240 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6241 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.51 _reflns_number_total 2046 _reflns_number_gt 2017 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.4969P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.021(16) _refine_ls_number_reflns 2046 _refine_ls_number_parameters 162 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 1.0000 0.49907(3) 0.01170(10) Uani 1 2 d S . . N1 N 0.64514(14) 1.06148(15) 0.45101(6) 0.0163(3) Uani 1 1 d . . . N2 N 0.5000 1.0000 0.22598(18) 0.0143(8) Uani 1 2 d S . . N3 N 0.43894(16) 0.85428(15) 0.54710(6) 0.0163(3) Uani 1 1 d . . . N4 N 0.5000 1.0000 0.77249(18) 0.0143(8) Uani 1 2 d S . . C1 C 0.78558(19) 1.10912(19) 0.45908(7) 0.0188(3) Uani 1 1 d . . . H1A H 0.8265 1.1257 0.4898 0.023 Uiso 1 1 calc R . . C2 C 0.86451(19) 1.13135(19) 0.41637(7) 0.0195(3) Uani 1 1 d . . . H2B H 0.9648 1.1654 0.4132 0.023 Uiso 1 1 calc R . . C3 C 0.76822(19) 1.0943(2) 0.38037(7) 0.0194(3) Uani 1 1 d . . . H3A H 0.7894 1.0970 0.3473 0.023 Uiso 1 1 calc R . . C4 C 0.63053(19) 1.05084(19) 0.40177(7) 0.0155(3) Uani 1 1 d . . . C5 C 0.5000 1.0000 0.3794(2) 0.0133(9) Uani 1 2 d S . . C6 C 0.5000 1.0000 0.3264(2) 0.0132(9) Uani 1 2 d S . . C7 C 0.50771(16) 1.1337(2) 0.30047(9) 0.0147(4) Uani 1 1 d . . . H7A H 0.5134 1.2275 0.3164 0.018 Uiso 1 1 calc R . . C8 C 0.50696(16) 1.1275(2) 0.25098(9) 0.0149(4) Uani 1 1 d . . . H8A H 0.5117 1.2194 0.2339 0.018 Uiso 1 1 calc R . . C9 C 0.39085(18) 0.71405(18) 0.53913(7) 0.0185(3) Uani 1 1 d . . . H9A H 0.3740 0.6731 0.5084 0.022 Uiso 1 1 calc R . . C10 C 0.36838(19) 0.6348(2) 0.58196(7) 0.0194(3) Uani 1 1 d . . . H10A H 0.3344 0.5343 0.5853 0.023 Uiso 1 1 calc R . . C11 C 0.40543(18) 0.73191(19) 0.61787(7) 0.0189(3) Uani 1 1 d . . . H11A H 0.4023 0.7112 0.6510 0.023 Uiso 1 1 calc R . . C12 C 0.44943(19) 0.86941(17) 0.59638(7) 0.0154(3) Uani 1 1 d . . . C13 C 0.5000 1.0000 0.6190(2) 0.0120(9) Uani 1 2 d S . . C14 C 0.5000 1.0000 0.6724(2) 0.0128(9) Uani 1 2 d S . . C15 C 0.6337(2) 1.00289(15) 0.69756(9) 0.0146(4) Uani 1 1 d . . . H15A H 0.7272 1.0062 0.6815 0.018 Uiso 1 1 calc R . . C16 C 0.6273(2) 1.00082(14) 0.74710(9) 0.0149(4) Uani 1 1 d . . . H16A H 0.7193 0.9999 0.7640 0.018 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01411(15) 0.01400(15) 0.00699(15) 0.000 0.000 -0.00266(8) N1 0.0187(7) 0.0174(7) 0.0129(7) 0.0004(5) 0.0003(6) -0.0010(5) N2 0.0181(18) 0.0169(18) 0.008(2) 0.000 0.000 0.0001(6) N3 0.0175(7) 0.0185(6) 0.0129(7) -0.0008(5) 0.0007(6) -0.0010(6) N4 0.0159(17) 0.0149(17) 0.012(2) 0.000 0.000 0.0003(5) C1 0.0188(7) 0.0201(8) 0.0175(9) -0.0010(6) -0.0030(7) -0.0004(6) C2 0.0165(7) 0.0208(8) 0.0213(9) 0.0008(7) 0.0026(7) -0.0028(6) C3 0.0199(8) 0.0212(8) 0.0170(8) 0.0002(6) 0.0035(7) -0.0011(6) C4 0.0183(7) 0.0147(8) 0.0135(8) -0.0008(6) 0.0012(6) -0.0001(6) C5 0.021(2) 0.0125(18) 0.006(3) 0.000 0.000 0.0018(7) C6 0.0096(18) 0.0158(19) 0.014(3) 0.000 0.000 -0.0002(6) C7 0.0184(9) 0.0129(9) 0.0128(11) -0.0007(8) -0.0004(6) 0.0003(5) C8 0.0177(9) 0.0157(10) 0.0114(10) 0.0023(8) -0.0009(5) 0.0001(5) C9 0.0194(8) 0.0182(7) 0.0179(9) -0.0024(6) -0.0007(6) -0.0017(6) C10 0.0213(7) 0.0169(7) 0.0201(9) 0.0015(6) -0.0007(7) -0.0032(6) C11 0.0212(8) 0.0197(8) 0.0159(9) 0.0036(6) -0.0006(7) -0.0017(6) C12 0.0157(8) 0.0180(7) 0.0125(8) 0.0013(6) -0.0009(6) -0.0006(6) C13 0.0083(16) 0.0171(19) 0.011(3) 0.000 0.000 0.0017(6) C14 0.020(2) 0.0142(19) 0.004(2) 0.000 0.000 -0.0005(7) C15 0.0125(9) 0.0189(10) 0.0124(11) -0.0005(5) 0.0011(8) -0.0005(5) C16 0.0143(10) 0.0191(10) 0.0111(10) -0.0014(5) -0.0017(9) 0.0005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.9506(16) 2_675 ? Cu1 N1 1.9506(16) . ? Cu1 N3 1.9516(16) 2_675 ? Cu1 N3 1.9516(16) . ? N1 C1 1.343(2) . ? N1 C4 1.394(2) . ? N2 C8 1.338(4) . ? N2 C8 1.338(4) 2_675 ? N3 C9 1.341(2) . ? N3 C12 1.395(2) . ? N4 C16 1.342(4) 2_675 ? N4 C16 1.342(4) . ? C1 C2 1.406(2) . ? C2 C3 1.369(3) . ? C3 C4 1.422(2) . ? C4 C5 1.400(3) . ? C5 C4 1.400(3) 2_675 ? C5 C6 1.489(10) . ? C6 C7 1.399(4) 2_675 ? C6 C7 1.399(4) . ? C7 C8 1.393(3) . ? C9 C10 1.411(2) . ? C10 C11 1.371(3) . ? C11 C12 1.422(2) . ? C12 C13 1.401(3) . ? C13 C12 1.401(3) 2_675 ? C13 C14 1.501(9) . ? C14 C15 1.389(4) 2_675 ? C14 C15 1.389(4) . ? C15 C16 1.394(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 92.33(9) 2_675 . ? N1 Cu1 N3 148.42(6) 2_675 2_675 ? N1 Cu1 N3 96.12(6) . 2_675 ? N1 Cu1 N3 96.12(6) 2_675 . ? N1 Cu1 N3 148.42(6) . . ? N3 Cu1 N3 92.42(10) 2_675 . ? C1 N1 C4 106.06(14) . . ? C1 N1 Cu1 126.30(13) . . ? C4 N1 Cu1 127.35(11) . . ? C8 N2 C8 116.6(4) . 2_675 ? C9 N3 C12 106.13(14) . . ? C9 N3 Cu1 126.47(13) . . ? C12 N3 Cu1 127.16(11) . . ? C16 N4 C16 115.7(4) 2_675 . ? N1 C1 C2 111.61(16) . . ? C3 C2 C1 106.42(15) . . ? C2 C3 C4 107.21(16) . . ? N1 C4 C5 123.1(3) . . ? N1 C4 C3 108.70(15) . . ? C5 C4 C3 128.1(3) . . ? C4 C5 C4 126.6(5) . 2_675 ? C4 C5 C6 116.7(2) . . ? C4 C5 C6 116.7(2) 2_675 . ? C7 C6 C7 117.1(5) 2_675 . ? C7 C6 C5 121.4(2) 2_675 . ? C7 C6 C5 121.4(2) . . ? C8 C7 C6 119.2(3) . . ? N2 C8 C7 123.9(3) . . ? N3 C9 C10 111.72(16) . . ? C11 C10 C9 106.13(15) . . ? C10 C11 C12 107.37(16) . . ? N3 C12 C13 123.5(3) . . ? N3 C12 C11 108.66(14) . . ? C13 C12 C11 127.8(3) . . ? C12 C13 C12 126.1(5) . 2_675 ? C12 C13 C14 116.9(2) . . ? C12 C13 C14 116.9(2) 2_675 . ? C15 C14 C15 118.6(4) 2_675 . ? C15 C14 C13 120.7(2) 2_675 . ? C15 C14 C13 120.7(2) . . ? C14 C15 C16 118.3(3) . . ? N4 C16 C15 124.5(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.988 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.085 #===END #========================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and Characterization of One-Dimensional Coordination Polymers based on Self-Assembling, Heteroleptic Copper Dipyrromethene Complexes ; loop _publ_author_name _publ_author_address 'Cohen, Seth M.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; 'Halper, Sara R.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; 'Malachowski, Mitchell R.' ; Department of Chemistry University of San Diego San Diego CA 92110-2492 USA ; 'Delaney, Heather M.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; #========================================================================= data_[Cu(4-cydpm)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H40 Cu2 N12' _chemical_formula_weight 1104.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.9165(12) _cell_length_b 16.0218(17) _cell_length_c 12.9956(14) _cell_angle_alpha 90.00 _cell_angle_beta 91.223(2) _cell_angle_gamma 90.00 _cell_volume 2480.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8514 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.47 _exptl_crystal_description Plate _exptl_crystal_colour green _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 0.916 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.675 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20658 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.52 _reflns_number_total 5682 _reflns_number_gt 4481 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+2.5003P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5682 _refine_ls_number_parameters 432 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.00480(3) 0.85651(2) 0.15029(3) 0.01954(12) Uani 1 1 d . . . N1 N 0.0255(2) 0.97741(15) 0.13440(19) 0.0199(5) Uani 1 1 d . . . N2 N 0.1633(2) 0.84105(16) 0.1881(2) 0.0222(6) Uani 1 1 d . . . N3 N -0.1494(2) 0.86298(16) 0.19694(19) 0.0218(5) Uani 1 1 d . . . N4 N -0.0201(2) 0.74544(15) 0.08991(19) 0.0195(5) Uani 1 1 d . . . N5 N 0.7224(3) 1.1984(2) 0.0875(3) 0.0442(8) Uani 1 1 d . . . N6 N -0.7270(3) 0.5405(2) 0.0184(3) 0.0424(8) Uani 1 1 d . . . C1 C -0.0539(3) 1.0337(2) 0.1093(2) 0.0232(7) Uani 1 1 d . . . C2 C -0.0090(3) 1.1129(2) 0.0885(2) 0.0241(7) Uani 1 1 d . . . C3 C 0.1057(3) 1.1043(2) 0.0988(2) 0.0219(6) Uani 1 1 d . . . C4 C 0.1275(2) 1.01966(19) 0.1272(2) 0.0202(6) Uani 1 1 d . . . C5 C 0.2309(2) 0.98294(19) 0.1511(2) 0.0195(6) Uani 1 1 d . . . C6 C 0.2482(2) 0.9008(2) 0.1820(2) 0.0212(6) Uani 1 1 d . . . C7 C 0.3511(3) 0.8627(2) 0.2132(3) 0.0262(7) Uani 1 1 d . . . C8 C 0.3283(3) 0.7825(2) 0.2389(3) 0.0291(7) Uani 1 1 d . . . C9 C 0.2118(3) 0.7714(2) 0.2223(3) 0.0286(7) Uani 1 1 d . . . C10 C 0.3339(2) 1.03601(18) 0.1395(2) 0.0210(6) Uani 1 1 d . . . C11 C 0.3639(3) 1.0642(2) 0.0422(3) 0.0234(7) Uani 1 1 d . . . C12 C 0.4632(3) 1.1079(2) 0.0294(3) 0.0256(7) Uani 1 1 d . . . C13 C 0.5331(3) 1.12353(19) 0.1146(3) 0.0264(7) Uani 1 1 d . . . C14 C 0.5026(3) 1.09766(19) 0.2133(3) 0.0233(7) Uani 1 1 d . . . C15 C 0.4032(3) 1.0544(2) 0.2247(3) 0.0250(7) Uani 1 1 d . . . C16 C 0.6397(3) 1.1661(2) 0.1005(3) 0.0311(8) Uani 1 1 d . . . C17 C -0.1926(3) 0.9216(2) 0.2579(3) 0.0276(7) Uani 1 1 d . . . C18 C -0.3079(3) 0.9091(2) 0.2723(3) 0.0285(7) Uani 1 1 d . . . C19 C -0.3365(3) 0.8391(2) 0.2180(3) 0.0252(7) Uani 1 1 d . . . C20 C -0.2372(2) 0.80929(19) 0.1712(2) 0.0205(6) Uani 1 1 d . . . C21 C -0.2249(2) 0.73732(19) 0.1113(2) 0.0193(6) Uani 1 1 d . . . C22 C -0.1239(2) 0.70661(19) 0.0738(2) 0.0203(6) Uani 1 1 d . . . C23 C -0.1077(3) 0.6305(2) 0.0189(2) 0.0244(7) Uani 1 1 d . . . C24 C 0.0051(3) 0.6244(2) 0.0018(3) 0.0284(7) Uani 1 1 d . . . C25 C 0.0551(3) 0.6958(2) 0.0454(3) 0.0269(7) Uani 1 1 d . . . C26 C -0.3298(2) 0.68907(19) 0.0870(2) 0.0220(7) Uani 1 1 d . . . C27 C -0.3731(3) 0.6849(2) -0.0134(3) 0.0302(8) Uani 1 1 d . . . C28 C -0.4741(3) 0.6451(2) -0.0350(3) 0.0328(8) Uani 1 1 d . . . C29 C -0.5330(3) 0.6088(2) 0.0459(3) 0.0266(7) Uani 1 1 d . . . C30 C -0.4885(3) 0.6097(2) 0.1450(3) 0.0216(6) Uani 1 1 d . . . C31 C -0.3872(3) 0.6501(2) 0.1658(3) 0.0273(7) Uani 1 1 d . . . C32 C -0.6419(3) 0.5703(2) 0.0286(3) 0.0307(8) Uani 1 1 d . . . H1 H -0.130(3) 1.019(2) 0.111(2) 0.022(8) Uiso 1 1 d . . . H2 H -0.051(3) 1.1623(19) 0.070(2) 0.016(8) Uiso 1 1 d . . . H3 H 0.161(3) 1.146(2) 0.086(3) 0.032(10) Uiso 1 1 d . . . H7 H 0.420(3) 0.887(2) 0.220(3) 0.033(10) Uiso 1 1 d . . . H8 H 0.377(3) 0.742(2) 0.262(3) 0.035(10) Uiso 1 1 d . . . H9 H 0.169(3) 0.717(2) 0.230(3) 0.033(10) Uiso 1 1 d . . . H11 H 0.313(3) 1.0527(19) -0.017(2) 0.020(8) Uiso 1 1 d . . . H12 H 0.483(3) 1.1263(18) -0.035(3) 0.017(8) Uiso 1 1 d . . . H14 H 0.553(3) 1.111(2) 0.271(3) 0.040(10) Uiso 1 1 d . . . H15 H 0.385(3) 1.0354(19) 0.295(3) 0.022(8) Uiso 1 1 d . . . H17 H -0.145(3) 0.969(2) 0.288(3) 0.035(10) Uiso 1 1 d . . . H18 H -0.353(3) 0.946(2) 0.318(2) 0.024(9) Uiso 1 1 d . . . H19 H -0.400(3) 0.8108(19) 0.209(2) 0.019(8) Uiso 1 1 d . . . H23 H -0.167(3) 0.5914(19) 0.002(2) 0.017(8) Uiso 1 1 d . . . H24 H 0.044(3) 0.579(2) -0.032(3) 0.037(10) Uiso 1 1 d . . . H25 H 0.131(3) 0.710(2) 0.049(2) 0.025(9) Uiso 1 1 d . . . H27 H -0.337(3) 0.710(2) -0.070(3) 0.047(11) Uiso 1 1 d . . . H28 H -0.499(3) 0.640(2) -0.094(3) 0.020(9) Uiso 1 1 d . . . H30 H -0.525(3) 0.586(2) 0.194(3) 0.036(10) Uiso 1 1 d . . . H31 H -0.350(3) 0.651(2) 0.239(3) 0.048(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01191(18) 0.02154(19) 0.0253(2) -0.00103(17) 0.00267(13) -0.00335(16) N1 0.0148(13) 0.0238(13) 0.0213(13) -0.0049(11) 0.0035(10) 0.0002(10) N2 0.0154(13) 0.0269(14) 0.0245(14) 0.0003(11) 0.0026(10) -0.0007(11) N3 0.0152(12) 0.0236(13) 0.0266(14) -0.0016(11) 0.0026(10) -0.0018(11) N4 0.0133(12) 0.0210(13) 0.0244(14) 0.0024(10) 0.0009(10) -0.0024(10) N5 0.0272(17) 0.055(2) 0.051(2) -0.0018(17) 0.0060(14) -0.0163(16) N6 0.0296(18) 0.0427(19) 0.055(2) 0.0029(16) -0.0055(15) -0.0081(15) C1 0.0150(15) 0.0318(18) 0.0229(16) -0.0027(13) 0.0014(12) 0.0009(13) C2 0.0242(17) 0.0250(16) 0.0230(17) -0.0010(13) 0.0004(13) 0.0031(14) C3 0.0223(16) 0.0236(16) 0.0199(16) -0.0006(13) 0.0042(12) -0.0024(13) C4 0.0193(15) 0.0242(15) 0.0173(15) -0.0027(12) 0.0015(12) -0.0033(12) C5 0.0187(15) 0.0240(15) 0.0159(15) -0.0050(12) 0.0028(11) -0.0022(12) C6 0.0163(15) 0.0281(17) 0.0192(15) -0.0011(13) 0.0024(12) -0.0006(13) C7 0.0180(16) 0.0295(17) 0.0312(18) 0.0021(15) 0.0021(13) -0.0013(14) C8 0.0206(17) 0.0303(18) 0.036(2) 0.0069(15) -0.0006(14) 0.0055(15) C9 0.0256(18) 0.0263(17) 0.0341(19) -0.0001(15) 0.0046(14) -0.0005(14) C10 0.0148(15) 0.0207(15) 0.0276(17) 0.0014(13) 0.0020(12) 0.0028(12) C11 0.0174(16) 0.0263(16) 0.0265(17) 0.0017(14) -0.0014(13) -0.0012(13) C12 0.0174(16) 0.0335(18) 0.0260(18) 0.0052(15) 0.0018(13) -0.0014(14) C13 0.0163(15) 0.0242(16) 0.0387(19) -0.0021(14) 0.0021(13) -0.0020(12) C14 0.0190(16) 0.0218(16) 0.0289(18) -0.0037(14) -0.0042(13) 0.0007(13) C15 0.0244(17) 0.0261(16) 0.0245(18) -0.0029(14) 0.0008(13) 0.0026(13) C16 0.0246(18) 0.0327(18) 0.036(2) 0.0023(15) -0.0014(15) -0.0042(15) C17 0.0258(18) 0.0281(17) 0.0290(18) -0.0031(15) 0.0022(14) -0.0020(14) C18 0.0228(17) 0.0324(18) 0.0305(18) -0.0007(15) 0.0079(14) 0.0052(14) C19 0.0136(15) 0.0306(18) 0.0315(18) 0.0031(14) 0.0009(13) -0.0020(13) C20 0.0149(15) 0.0260(16) 0.0207(15) 0.0057(13) 0.0001(11) -0.0021(12) C21 0.0158(15) 0.0253(16) 0.0168(15) 0.0048(12) 0.0002(11) -0.0041(12) C22 0.0156(15) 0.0237(15) 0.0213(15) 0.0032(13) -0.0011(12) -0.0035(12) C23 0.0236(17) 0.0247(17) 0.0251(17) -0.0013(13) 0.0001(13) -0.0042(13) C24 0.0299(18) 0.0251(18) 0.0304(18) -0.0007(14) 0.0069(14) -0.0001(14) C25 0.0195(17) 0.0308(18) 0.0305(18) 0.0012(14) 0.0047(13) -0.0027(14) C26 0.0151(15) 0.0235(16) 0.0275(17) 0.0018(13) 0.0007(12) -0.0016(12) C27 0.0269(18) 0.0370(19) 0.0267(19) 0.0053(15) 0.0000(14) -0.0056(15) C28 0.0245(18) 0.041(2) 0.033(2) 0.0043(18) -0.0058(15) -0.0068(16) C29 0.0217(17) 0.0230(15) 0.0352(19) -0.0011(14) 0.0011(14) -0.0092(13) C30 0.0166(15) 0.0243(15) 0.0242(16) 0.0043(14) 0.0041(12) -0.0026(13) C31 0.0211(16) 0.0338(18) 0.0271(17) 0.0024(15) -0.0018(13) -0.0021(14) C32 0.0251(19) 0.0332(19) 0.0336(19) 0.0001(15) -0.0011(14) -0.0014(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.950(2) . ? Cu1 N2 1.957(3) . ? Cu1 N1 1.964(3) . ? Cu1 N4 1.965(2) . ? N1 C1 1.343(4) . ? N1 C4 1.395(4) . ? N2 C9 1.329(4) . ? N2 C6 1.397(4) . ? N3 C17 1.339(4) . ? N3 C20 1.389(4) . ? N4 C25 1.339(4) . ? N4 C22 1.395(4) . ? N5 C16 1.129(4) . ? N6 C32 1.127(4) . ? C1 C2 1.406(5) . ? C2 C3 1.378(4) . ? C3 C4 1.428(4) . ? C4 C5 1.394(4) . ? C5 C6 1.389(4) . ? C5 C10 1.504(4) . ? C6 C7 1.421(4) . ? C7 C8 1.356(5) . ? C8 C9 1.411(5) . ? C10 C11 1.396(4) . ? C10 C15 1.398(4) . ? C11 C12 1.387(4) . ? C12 C13 1.394(5) . ? C13 C14 1.404(5) . ? C13 C16 1.457(5) . ? C14 C15 1.383(4) . ? C17 C18 1.405(5) . ? C18 C19 1.365(5) . ? C19 C20 1.424(4) . ? C20 C21 1.401(4) . ? C21 C22 1.398(4) . ? C21 C26 1.497(4) . ? C22 C23 1.429(4) . ? C23 C24 1.370(5) . ? C24 C25 1.404(5) . ? C26 C31 1.392(4) . ? C26 C27 1.394(4) . ? C27 C28 1.385(5) . ? C28 C29 1.403(5) . ? C29 C30 1.383(5) . ? C29 C32 1.449(5) . ? C30 C31 1.391(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N2 147.06(11) . . ? N3 Cu1 N1 95.84(10) . . ? N2 Cu1 N1 91.62(10) . . ? N3 Cu1 N4 92.11(10) . . ? N2 Cu1 N4 97.05(10) . . ? N1 Cu1 N4 150.40(10) . . ? C1 N1 C4 105.6(3) . . ? C1 N1 Cu1 126.7(2) . . ? C4 N1 Cu1 126.7(2) . . ? C9 N2 C6 106.5(3) . . ? C9 N2 Cu1 127.0(2) . . ? C6 N2 Cu1 126.5(2) . . ? C17 N3 C20 106.2(3) . . ? C17 N3 Cu1 126.7(2) . . ? C20 N3 Cu1 127.0(2) . . ? C25 N4 C22 105.6(3) . . ? C25 N4 Cu1 127.8(2) . . ? C22 N4 Cu1 126.1(2) . . ? N1 C1 C2 112.5(3) . . ? C3 C2 C1 105.8(3) . . ? C2 C3 C4 107.1(3) . . ? C5 C4 N1 123.1(3) . . ? C5 C4 C3 127.8(3) . . ? N1 C4 C3 108.9(3) . . ? C6 C5 C4 126.1(3) . . ? C6 C5 C10 116.6(3) . . ? C4 C5 C10 117.3(3) . . ? C5 C6 N2 124.2(3) . . ? C5 C6 C7 127.7(3) . . ? N2 C6 C7 108.1(3) . . ? C8 C7 C6 107.5(3) . . ? C7 C8 C9 106.5(3) . . ? N2 C9 C8 111.4(3) . . ? C11 C10 C15 119.4(3) . . ? C11 C10 C5 120.0(3) . . ? C15 C10 C5 120.6(3) . . ? C12 C11 C10 120.5(3) . . ? C11 C12 C13 119.5(3) . . ? C12 C13 C14 120.7(3) . . ? C12 C13 C16 119.5(3) . . ? C14 C13 C16 119.8(3) . . ? C15 C14 C13 119.0(3) . . ? C14 C15 C10 120.9(3) . . ? N5 C16 C13 178.5(4) . . ? N3 C17 C18 111.6(3) . . ? C19 C18 C17 106.4(3) . . ? C18 C19 C20 107.2(3) . . ? N3 C20 C21 123.8(3) . . ? N3 C20 C19 108.6(3) . . ? C21 C20 C19 127.6(3) . . ? C22 C21 C20 125.8(3) . . ? C22 C21 C26 117.7(3) . . ? C20 C21 C26 116.5(3) . . ? N4 C22 C21 123.9(3) . . ? N4 C22 C23 109.1(3) . . ? C21 C22 C23 126.9(3) . . ? C24 C23 C22 106.6(3) . . ? C23 C24 C25 106.6(3) . . ? N4 C25 C24 112.1(3) . . ? C31 C26 C27 119.2(3) . . ? C31 C26 C21 119.8(3) . . ? C27 C26 C21 120.9(3) . . ? C28 C27 C26 121.0(3) . . ? C27 C28 C29 119.0(3) . . ? C30 C29 C28 120.4(3) . . ? C30 C29 C32 118.2(3) . . ? C28 C29 C32 121.4(3) . . ? C29 C30 C31 120.0(3) . . ? C26 C31 C30 120.3(3) . . ? N6 C32 C29 177.8(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.473 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.080 #===END #========================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and Characterization of One-Dimensional Coordination Polymers based on Self-Assembling, Heteroleptic Copper Dipyrromethene Complexes ; loop _publ_author_name _publ_author_address 'Cohen, Seth M.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; 'Halper, Sara R.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; 'Malachowski, Mitchell R.' ; Department of Chemistry University of San Diego San Diego CA 92110-2492 USA ; 'Delaney, Heather M.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; #========================================================================= data_[Cu(4-pyrdpm)(acac)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25.33 H22.67 Cu1.33 N4 O2.67' _chemical_formula_weight 510.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.0337(10) _cell_length_b 11.9862(8) _cell_length_c 10.4162(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1752.1(2) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 1.263 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10150 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 27.51 _reflns_number_total 2107 _reflns_number_gt 1900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.0518P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2107 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.117341(17) 0.2500 -0.09021(2) 0.01467(11) Uani 1 2 d S . . C6 C 0.37528(14) 0.2500 0.2237(2) 0.0161(4) Uani 1 2 d S . . N1 N 0.19644(8) 0.13169(10) -0.01065(11) 0.0160(3) Uani 1 1 d . . . N2 N 0.00952(13) 0.2500 0.07852(16) 0.0178(4) Uani 1 2 d S . . C4 C 0.26856(10) 0.14596(13) 0.07989(13) 0.0163(3) Uani 1 1 d . . . C13 C -0.05821(16) 0.2500 -0.2994(2) 0.0230(5) Uani 1 2 d S . . H13 H -0.1139 0.2500 -0.3513 0.028 Uiso 1 2 calc SR . . C3 C 0.29824(11) 0.03960(13) 0.12458(15) 0.0194(3) Uani 1 1 d . . . H3 H 0.3466 0.0252 0.1862 0.023 Uiso 1 1 calc R . . C5 C 0.30120(14) 0.2500 0.12023(19) 0.0153(4) Uani 1 2 d S . . C12 C -0.01988(11) 0.14730(14) -0.26366(14) 0.0219(3) Uani 1 1 d . . . C9 C -0.08349(16) 0.2500 0.0543(2) 0.0214(5) Uani 1 2 d S . . H9 H -0.1037 0.2500 -0.0328 0.026 Uiso 1 2 calc SR . . C1 C 0.18217(11) 0.02174(12) -0.01948(14) 0.0204(3) Uani 1 1 d . . . H1 H 0.1361 -0.0120 -0.0739 0.024 Uiso 1 1 calc R . . C2 C 0.24416(12) -0.03799(14) 0.06218(15) 0.0227(3) Uani 1 1 d . . . H2 H 0.2476 -0.1167 0.0718 0.027 Uiso 1 1 calc R . . C7 C 0.47161(16) 0.2500 0.1973(2) 0.0281(5) Uani 1 2 d S . . H7 H 0.4937 0.2500 0.1110 0.034 Uiso 1 2 calc SR . . C8 C 0.34769(16) 0.2500 0.3507(2) 0.0216(5) Uani 1 2 d S . . H8 H 0.2820 0.2500 0.3728 0.026 Uiso 1 2 calc SR . . C11 C -0.06365(12) 0.04195(15) -0.31415(17) 0.0298(4) Uani 1 1 d . . . H11A H -0.0201 0.0071 -0.3757 0.045 Uiso 1 1 calc R . . H11B H -0.1240 0.0595 -0.3569 0.045 Uiso 1 1 calc R . . H11C H -0.0755 -0.0095 -0.2428 0.045 Uiso 1 1 calc R . . C10 C 0.03549(16) 0.2500 0.2019(2) 0.0276(5) Uani 1 2 d S . . H10 H 0.1016 0.2500 0.2213 0.033 Uiso 1 2 calc SR . . O1 O 0.05114(7) 0.13442(9) -0.18856(10) 0.0214(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01257(16) 0.01787(16) 0.01356(15) 0.000 -0.00197(9) 0.000 C6 0.0158(10) 0.0151(10) 0.0175(10) 0.000 -0.0031(7) 0.000 N1 0.0152(6) 0.0177(6) 0.0151(6) -0.0012(5) -0.0004(5) 0.0005(5) N2 0.0156(9) 0.0186(9) 0.0191(9) 0.000 0.0027(7) 0.000 C4 0.0136(7) 0.0216(8) 0.0136(7) 0.0008(5) 0.0005(5) 0.0004(6) C13 0.0176(11) 0.0338(13) 0.0176(10) 0.000 -0.0054(8) 0.000 C3 0.0183(7) 0.0220(8) 0.0180(7) 0.0025(6) -0.0008(6) 0.0021(6) C5 0.0107(9) 0.0225(11) 0.0126(9) 0.000 0.0012(7) 0.000 C12 0.0165(7) 0.0342(9) 0.0149(7) -0.0051(6) 0.0003(6) -0.0009(6) C9 0.0189(11) 0.0283(12) 0.0169(10) 0.000 0.0004(9) 0.000 C1 0.0207(8) 0.0203(8) 0.0202(7) -0.0025(6) -0.0022(6) -0.0019(6) C2 0.0260(8) 0.0178(8) 0.0242(8) 0.0013(6) -0.0009(7) 0.0004(6) C7 0.0177(11) 0.0495(15) 0.0171(11) 0.000 -0.0002(8) 0.000 C8 0.0156(10) 0.0303(12) 0.0188(11) 0.000 0.0004(8) 0.000 C11 0.0251(9) 0.0351(10) 0.0291(9) -0.0099(7) -0.0067(7) -0.0022(7) C10 0.0145(11) 0.0453(15) 0.0229(11) 0.000 0.0005(9) 0.000 O1 0.0195(5) 0.0240(6) 0.0206(5) -0.0046(4) -0.0063(4) 0.0015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.9575(10) . ? Cu1 O1 1.9575(10) 7_565 ? Cu1 N1 1.9824(12) 7_565 ? Cu1 N1 1.9824(12) . ? Cu1 N2 2.3191(17) . ? C6 C8 1.379(3) . ? C6 C7 1.380(3) . ? C6 C5 1.497(3) . ? N1 C1 1.3362(18) . ? N1 C4 1.3940(18) . ? N2 C9 1.330(3) . ? N2 C10 1.336(3) . ? C4 C5 1.3934(18) . ? C4 C3 1.420(2) . ? C13 C12 1.3941(19) 7_565 ? C13 C12 1.3941(19) . ? C3 C2 1.365(2) . ? C5 C4 1.3934(18) 7_565 ? C12 O1 1.2763(18) . ? C12 C11 1.499(2) . ? C9 C8 1.382(3) 6_556 ? C1 C2 1.412(2) . ? C7 C10 1.381(3) 6_656 ? C8 C9 1.382(3) 6_656 ? C10 C7 1.381(3) 6_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1 90.10(6) . 7_565 ? O1 Cu1 N1 172.22(5) . 7_565 ? O1 Cu1 N1 88.75(5) 7_565 7_565 ? O1 Cu1 N1 88.75(5) . . ? O1 Cu1 N1 172.22(5) 7_565 . ? N1 Cu1 N1 91.34(7) 7_565 . ? O1 Cu1 N2 94.99(4) . . ? O1 Cu1 N2 94.99(4) 7_565 . ? N1 Cu1 N2 92.78(5) 7_565 . ? N1 Cu1 N2 92.78(5) . . ? C8 C6 C7 117.8(2) . . ? C8 C6 C5 119.72(19) . . ? C7 C6 C5 122.46(19) . . ? C1 N1 C4 106.04(12) . . ? C1 N1 Cu1 126.36(10) . . ? C4 N1 Cu1 126.99(10) . . ? C9 N2 C10 116.77(19) . . ? C9 N2 Cu1 119.79(14) . . ? C10 N2 Cu1 123.44(15) . . ? C5 C4 N1 123.54(14) . . ? C5 C4 C3 127.48(14) . . ? N1 C4 C3 108.95(13) . . ? C12 C13 C12 124.0(2) 7_565 . ? C2 C3 C4 107.01(14) . . ? C4 C5 C4 127.02(19) . 7_565 ? C4 C5 C6 116.44(10) . . ? C4 C5 C6 116.44(10) 7_565 . ? O1 C12 C13 124.89(15) . . ? O1 C12 C11 115.65(14) . . ? C13 C12 C11 119.46(15) . . ? N2 C9 C8 123.4(2) . 6_556 ? N1 C1 C2 111.49(13) . . ? C3 C2 C1 106.50(14) . . ? C6 C7 C10 119.0(2) . 6_656 ? C6 C8 C9 119.4(2) . 6_656 ? N2 C10 C7 123.7(2) . 6_556 ? C12 O1 Cu1 127.28(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.484 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.065 #===END #========================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and Characterization of One-Dimensional Coordination Polymers based on Self-Assembling, Heteroleptic Copper Dipyrromethene Complexes ; loop _publ_author_name _publ_author_address 'Cohen, Seth M.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; 'Halper, Sara R.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; 'Malachowski, Mitchell R.' ; Department of Chemistry University of San Diego San Diego CA 92110-2492 USA ; 'Delaney, Heather M.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; #========================================================================= data_[Cu(3-pyrdpm)(acac)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19.50 H18 Cl Cu N3 O2' _chemical_formula_weight 425.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3811(5) _cell_length_b 15.5837(10) _cell_length_c 16.5921(11) _cell_angle_alpha 117.5200(10) _cell_angle_beta 91.7370(10) _cell_angle_gamma 98.9500(10) _cell_volume 1885.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 1.319 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16478 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8431 _reflns_number_gt 6655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1003P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8431 _refine_ls_number_parameters 482 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1472 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu2 Cu 0.32592(4) 0.68427(2) 0.35962(2) 0.01094(11) Uani 1 1 d . . . O3 O 0.4123(2) 0.59143(15) 0.38992(13) 0.0154(4) Uani 1 1 d . . . O4 O 0.3986(2) 0.62496(15) 0.23869(13) 0.0159(4) Uani 1 1 d . . . N5 N 0.2202(3) 0.72934(17) 0.47346(16) 0.0115(5) Uani 1 1 d . . . N4 N 0.2036(3) 0.75912(17) 0.31945(16) 0.0126(5) Uani 1 1 d . . . C24 C 0.0033(3) 0.79535(19) 0.43034(18) 0.0107(5) Uani 1 1 d . . . C37 C 0.4547(3) 0.5457(2) 0.20123(19) 0.0142(6) Uani 1 1 d . . . C28 C 0.2561(3) 0.7159(2) 0.54499(18) 0.0139(6) Uani 1 1 d . . . H28 H 0.3486 0.6909 0.5526 0.017 Uiso 1 1 calc R . . C26 C 0.0256(3) 0.7741(2) 0.57228(19) 0.0144(6) Uani 1 1 d . . . H26 H -0.0694 0.7958 0.5981 0.017 Uiso 1 1 calc R . . C35 C 0.4731(3) 0.5180(2) 0.33593(19) 0.0144(6) Uani 1 1 d . . . C25 C 0.0765(3) 0.76742(19) 0.48862(18) 0.0108(5) Uani 1 1 d . . . C38 C 0.4771(4) 0.5092(2) 0.10228(19) 0.0200(6) Uani 1 1 d . . . H38A H 0.3726 0.4979 0.0673 0.030 Uiso 1 1 calc R . . H38B H 0.5177 0.4474 0.0790 0.030 Uiso 1 1 calc R . . H38C H 0.5556 0.5586 0.0957 0.030 Uiso 1 1 calc R . . C23 C 0.0631(3) 0.7935(2) 0.35169(18) 0.0114(5) Uani 1 1 d . . . C22 C 0.0009(3) 0.8314(2) 0.29635(19) 0.0148(6) Uani 1 1 d . . . H22 H -0.0951 0.8583 0.3027 0.018 Uiso 1 1 calc R . . C21 C 0.1058(4) 0.8216(2) 0.2321(2) 0.0185(6) Uani 1 1 d . . . H21 H 0.0976 0.8410 0.1858 0.022 Uiso 1 1 calc R . . C20 C 0.2291(3) 0.7767(2) 0.24847(19) 0.0164(6) Uani 1 1 d . . . H20 H 0.3182 0.7612 0.2137 0.020 Uiso 1 1 calc R . . C27 C 0.1403(3) 0.7433(2) 0.60860(19) 0.0161(6) Uani 1 1 d . . . H27 H 0.1416 0.7408 0.6647 0.019 Uiso 1 1 calc R . . C34 C 0.5235(4) 0.4557(2) 0.3759(2) 0.0245(7) Uani 1 1 d . . . H34A H 0.6028 0.4971 0.4301 0.037 Uiso 1 1 calc R . . H34B H 0.5727 0.4034 0.3303 0.037 Uiso 1 1 calc R . . H34C H 0.4279 0.4262 0.3933 0.037 Uiso 1 1 calc R . . C36 C 0.4935(4) 0.4924(2) 0.2446(2) 0.0171(6) Uani 1 1 d . . . H36 H 0.5366 0.4348 0.2101 0.021 Uiso 1 1 calc R . . Cu1 Cu 0.15550(4) 0.32015(2) 0.14111(2) 0.01024(11) Uani 1 1 d . . . O2 O 0.0693(2) 0.41290(15) 0.11016(13) 0.0154(4) Uani 1 1 d . . . O1 O 0.0802(2) 0.37988(15) 0.26164(13) 0.0150(4) Uani 1 1 d . . . N2 N 0.2792(3) 0.24686(17) 0.18281(16) 0.0115(5) Uani 1 1 d . . . N1 N 0.2615(3) 0.27440(17) 0.02764(15) 0.0107(5) Uani 1 1 d . . . N3 N 0.9232(3) 0.20370(17) 0.07455(16) 0.0134(5) Uani 1 1 d . . . C5 C 0.4776(3) 0.20780(19) 0.07070(18) 0.0109(5) Uani 1 1 d . . . C1 C 0.2252(3) 0.2880(2) -0.04439(18) 0.0135(6) Uani 1 1 d . . . H1 H 0.1335 0.3138 -0.0518 0.016 Uiso 1 1 calc R . . C7 C 0.4821(3) 0.1751(2) 0.20709(19) 0.0143(6) Uani 1 1 d . . . H7 H 0.5777 0.1480 0.2011 0.017 Uiso 1 1 calc R . . C16 C 0.0238(3) 0.4588(2) 0.29861(19) 0.0137(6) Uani 1 1 d . . . C12 C 0.9246(3) 0.1156(2) 0.0040(2) 0.0155(6) Uani 1 1 d . . . H12 H 1.0265 0.0962 -0.0104 0.019 Uiso 1 1 calc R . . C18 C 0.0087(3) 0.4862(2) 0.16381(19) 0.0140(6) Uani 1 1 d . . . C11 C 0.7790(3) 0.2298(2) 0.09544(19) 0.0133(6) Uani 1 1 d . . . H11 H 0.7769 0.2918 0.1466 0.016 Uiso 1 1 calc R . . C8 C 0.3777(4) 0.1870(2) 0.2722(2) 0.0181(6) Uani 1 1 d . . . H8 H 0.3863 0.1691 0.3194 0.022 Uiso 1 1 calc R . . C2 C 0.3400(3) 0.2593(2) -0.10787(19) 0.0157(6) Uani 1 1 d . . . H2 H 0.3391 0.2616 -0.1641 0.019 Uiso 1 1 calc R . . C4 C 0.4035(3) 0.2353(2) 0.01203(18) 0.0114(5) Uani 1 1 d . . . C6 C 0.4194(3) 0.2112(2) 0.15011(18) 0.0111(5) Uani 1 1 d . . . C13 C 0.7851(3) 0.0510(2) -0.0493(2) 0.0166(6) Uani 1 1 d . . . H13 H 0.7909 -0.0113 -0.0991 0.020 Uiso 1 1 calc R . . C9 C 0.2547(3) 0.2312(2) 0.25480(19) 0.0156(6) Uani 1 1 d . . . H9 H 0.1660 0.2477 0.2898 0.019 Uiso 1 1 calc R . . C15 C -0.0018(4) 0.4951(2) 0.39709(19) 0.0199(6) Uani 1 1 d . . . H15A H -0.0861 0.4475 0.4026 0.030 Uiso 1 1 calc R . . H15B H -0.0362 0.5589 0.4208 0.030 Uiso 1 1 calc R . . H15C H 0.1001 0.5028 0.4324 0.030 Uiso 1 1 calc R . . C10 C 0.6323(3) 0.1703(2) 0.04552(19) 0.0125(5) Uani 1 1 d . . . C14 C 0.6360(3) 0.0794(2) -0.02838(19) 0.0155(6) Uani 1 1 d . . . H14 H 0.5380 0.0371 -0.0642 0.019 Uiso 1 1 calc R . . C3 C 0.4540(3) 0.2274(2) -0.07176(19) 0.0144(6) Uani 1 1 d . . . H3 H 0.5481 0.2045 -0.0979 0.017 Uiso 1 1 calc R . . C17 C -0.0139(3) 0.5119(2) 0.25482(19) 0.0160(6) Uani 1 1 d . . . H17 H -0.0579 0.5693 0.2889 0.019 Uiso 1 1 calc R . . C19 C -0.0413(4) 0.5489(2) 0.1237(2) 0.0226(7) Uani 1 1 d . . . H19A H 0.0545 0.5778 0.1059 0.034 Uiso 1 1 calc R . . H19B H -0.0894 0.6017 0.1695 0.034 Uiso 1 1 calc R . . H19C H -0.1213 0.5079 0.0698 0.034 Uiso 1 1 calc R . . C30 C -0.2982(3) 0.7737(2) 0.40665(19) 0.0153(6) Uani 1 1 d . . . H30 H -0.2971 0.7110 0.3563 0.018 Uiso 1 1 calc R . . C33 C -0.1533(3) 0.9248(2) 0.5278(2) 0.0166(6) Uani 1 1 d . . . H33 H -0.0547 0.9672 0.5627 0.020 Uiso 1 1 calc R . . C29 C -0.1506(3) 0.8331(2) 0.45545(19) 0.0121(5) Uani 1 1 d . . . Cl1 Cl 0.83702(11) 1.04424(7) 0.16471(6) 0.0363(2) Uani 1 1 d . . . N6 N -0.4419(3) 0.80086(18) 0.42737(16) 0.0152(5) Uani 1 1 d . . . C31 C -0.4425(3) 0.8897(2) 0.4974(2) 0.0168(6) Uani 1 1 d . . . H31 H -0.5441 0.9092 0.5123 0.020 Uiso 1 1 calc R . . C32 C -0.3020(4) 0.9547(2) 0.5492(2) 0.0185(6) Uani 1 1 d . . . H32 H -0.3066 1.0179 0.5979 0.022 Uiso 1 1 calc R . . Cl2 Cl 0.63987(18) 0.99897(8) 0.28694(8) 0.0648(4) Uani 1 1 d . . . C39 C 0.8270(5) 0.9915(3) 0.2348(3) 0.0412(10) Uani 1 1 d . . . H39A H 0.9202 1.0249 0.2834 0.049 Uiso 1 1 calc R . . H39B H 0.8358 0.9214 0.1990 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu2 0.01042(18) 0.0136(2) 0.00952(19) 0.00529(15) 0.00357(13) 0.00422(13) O3 0.0189(10) 0.0150(10) 0.0126(10) 0.0057(8) 0.0036(8) 0.0068(8) O4 0.0207(11) 0.0163(11) 0.0123(10) 0.0071(9) 0.0061(8) 0.0059(8) N5 0.0098(11) 0.0121(12) 0.0111(11) 0.0038(10) 0.0023(9) 0.0030(9) N4 0.0104(11) 0.0162(12) 0.0117(11) 0.0068(10) 0.0030(9) 0.0028(9) C24 0.0082(12) 0.0079(13) 0.0130(13) 0.0028(11) 0.0014(10) 0.0001(10) C37 0.0122(13) 0.0130(14) 0.0128(13) 0.0031(12) 0.0042(10) -0.0006(11) C28 0.0152(14) 0.0153(14) 0.0122(13) 0.0069(12) 0.0024(11) 0.0041(11) C26 0.0151(14) 0.0141(14) 0.0140(14) 0.0061(12) 0.0061(11) 0.0037(11) C35 0.0122(13) 0.0139(14) 0.0143(14) 0.0042(12) 0.0010(11) 0.0027(11) C25 0.0114(13) 0.0086(13) 0.0103(13) 0.0030(11) 0.0035(10) 0.0007(10) C38 0.0283(16) 0.0174(15) 0.0136(14) 0.0065(13) 0.0104(12) 0.0034(12) C23 0.0104(13) 0.0116(13) 0.0114(13) 0.0050(11) 0.0010(10) 0.0015(10) C22 0.0143(13) 0.0133(14) 0.0159(14) 0.0062(12) -0.0012(11) 0.0032(11) C21 0.0229(15) 0.0193(16) 0.0169(15) 0.0114(13) 0.0011(12) 0.0044(12) C20 0.0176(14) 0.0190(15) 0.0149(14) 0.0098(12) 0.0043(11) 0.0040(12) C27 0.0205(15) 0.0164(15) 0.0111(13) 0.0059(12) 0.0038(11) 0.0047(12) C34 0.0344(18) 0.0232(17) 0.0184(15) 0.0091(14) 0.0044(13) 0.0143(14) C36 0.0197(15) 0.0140(15) 0.0152(14) 0.0041(12) 0.0067(11) 0.0053(11) Cu1 0.00957(18) 0.0129(2) 0.00960(19) 0.00559(15) 0.00345(13) 0.00457(13) O2 0.0186(10) 0.0163(11) 0.0120(10) 0.0056(9) 0.0036(8) 0.0086(8) O1 0.0202(11) 0.0149(10) 0.0127(10) 0.0074(8) 0.0049(8) 0.0073(8) N2 0.0110(11) 0.0137(12) 0.0119(11) 0.0074(10) 0.0029(9) 0.0035(9) N1 0.0110(11) 0.0107(11) 0.0097(11) 0.0039(9) 0.0009(9) 0.0029(9) N3 0.0093(11) 0.0151(12) 0.0163(12) 0.0073(10) 0.0039(9) 0.0031(9) C5 0.0090(12) 0.0093(13) 0.0119(13) 0.0033(11) 0.0019(10) 0.0009(10) C1 0.0157(14) 0.0130(14) 0.0104(13) 0.0042(11) -0.0001(10) 0.0040(11) C7 0.0133(13) 0.0144(14) 0.0141(14) 0.0058(12) 0.0003(11) 0.0027(11) C16 0.0094(13) 0.0152(14) 0.0118(13) 0.0038(12) 0.0020(10) -0.0022(10) C12 0.0140(14) 0.0164(15) 0.0181(14) 0.0086(13) 0.0070(11) 0.0056(11) C18 0.0125(13) 0.0130(14) 0.0157(14) 0.0063(12) 0.0007(11) 0.0023(11) C11 0.0127(13) 0.0116(14) 0.0130(13) 0.0036(11) 0.0020(11) 0.0025(11) C8 0.0217(15) 0.0213(16) 0.0158(14) 0.0115(13) 0.0025(12) 0.0072(12) C2 0.0202(15) 0.0149(14) 0.0104(13) 0.0050(12) 0.0024(11) 0.0023(11) C4 0.0090(12) 0.0112(13) 0.0115(13) 0.0033(11) 0.0031(10) 0.0019(10) C6 0.0073(12) 0.0118(13) 0.0142(13) 0.0060(11) 0.0015(10) 0.0021(10) C13 0.0146(14) 0.0132(14) 0.0183(14) 0.0037(12) 0.0057(11) 0.0047(11) C9 0.0160(14) 0.0198(15) 0.0154(14) 0.0109(12) 0.0083(11) 0.0056(11) C15 0.0284(16) 0.0154(15) 0.0136(14) 0.0049(12) 0.0073(12) 0.0038(12) C10 0.0086(13) 0.0167(14) 0.0156(14) 0.0098(12) 0.0051(10) 0.0041(10) C14 0.0107(13) 0.0137(14) 0.0173(14) 0.0045(12) 0.0015(11) -0.0014(11) C3 0.0157(14) 0.0131(14) 0.0135(14) 0.0055(12) 0.0053(11) 0.0028(11) C17 0.0202(15) 0.0128(14) 0.0134(14) 0.0035(12) 0.0064(11) 0.0074(11) C19 0.0327(18) 0.0203(16) 0.0185(15) 0.0092(13) 0.0054(13) 0.0150(14) C30 0.0123(13) 0.0150(15) 0.0160(14) 0.0045(12) 0.0035(11) 0.0044(11) C33 0.0140(14) 0.0149(15) 0.0191(15) 0.0067(13) 0.0020(11) 0.0020(11) C29 0.0114(13) 0.0109(13) 0.0153(14) 0.0073(12) 0.0026(10) 0.0018(10) Cl1 0.0476(5) 0.0430(5) 0.0324(5) 0.0232(4) 0.0185(4) 0.0272(4) N6 0.0107(11) 0.0152(13) 0.0180(12) 0.0064(11) 0.0029(9) 0.0022(9) C31 0.0134(14) 0.0187(15) 0.0212(15) 0.0100(13) 0.0061(11) 0.0086(11) C32 0.0196(15) 0.0108(14) 0.0192(15) 0.0014(12) 0.0038(12) 0.0049(11) Cl2 0.1024(10) 0.0350(6) 0.0451(6) 0.0104(5) 0.0416(6) 0.0017(6) C39 0.051(2) 0.0144(18) 0.039(2) -0.0023(16) -0.0166(18) 0.0065(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu2 O4 1.9461(19) . ? Cu2 O3 1.9612(19) . ? Cu2 N4 1.976(2) . ? Cu2 N5 1.979(2) . ? Cu2 N6 2.287(2) 1_655 ? O3 C35 1.278(3) . ? O4 C37 1.274(3) . ? N5 C28 1.330(3) . ? N5 C25 1.403(3) . ? N4 C20 1.343(3) . ? N4 C23 1.389(3) . ? C24 C25 1.392(4) . ? C24 C23 1.402(4) . ? C24 C29 1.492(3) . ? C37 C36 1.391(4) . ? C37 C38 1.498(4) . ? C28 C27 1.418(4) . ? C26 C27 1.376(4) . ? C26 C25 1.427(4) . ? C35 C36 1.400(4) . ? C35 C34 1.506(4) . ? C23 C22 1.425(4) . ? C22 C21 1.372(4) . ? C21 C20 1.419(4) . ? Cu1 O1 1.9502(19) . ? Cu1 O2 1.9657(19) . ? Cu1 N1 1.975(2) . ? Cu1 N2 1.978(2) . ? Cu1 N3 2.285(2) 1_455 ? O2 C18 1.274(3) . ? O1 C16 1.270(3) . ? N2 C9 1.340(3) . ? N2 C6 1.395(3) . ? N1 C1 1.341(3) . ? N1 C4 1.397(3) . ? N3 C12 1.333(4) . ? N3 C11 1.340(3) . ? N3 Cu1 2.285(2) 1_655 ? C5 C4 1.396(4) . ? C5 C6 1.400(4) . ? C5 C10 1.497(3) . ? C1 C2 1.413(4) . ? C7 C8 1.374(4) . ? C7 C6 1.428(4) . ? C16 C17 1.392(4) . ? C16 C15 1.497(4) . ? C12 C13 1.382(4) . ? C18 C17 1.400(4) . ? C18 C19 1.511(4) . ? C11 C10 1.390(4) . ? C8 C9 1.417(4) . ? C2 C3 1.382(4) . ? C4 C3 1.421(4) . ? C13 C14 1.391(4) . ? C10 C14 1.387(4) . ? C30 N6 1.340(3) . ? C30 C29 1.390(4) . ? C33 C29 1.381(4) . ? C33 C32 1.397(4) . ? Cl1 C39 1.704(4) . ? N6 C31 1.335(4) . ? N6 Cu2 2.287(2) 1_455 ? C31 C32 1.383(4) . ? Cl2 C39 1.808(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cu2 O3 91.21(8) . . ? O4 Cu2 N4 88.16(9) . . ? O3 Cu2 N4 169.73(9) . . ? O4 Cu2 N5 171.07(9) . . ? O3 Cu2 N5 88.74(9) . . ? N4 Cu2 N5 90.29(9) . . ? O4 Cu2 N6 94.89(9) . 1_655 ? O3 Cu2 N6 91.87(9) . 1_655 ? N4 Cu2 N6 98.40(9) . 1_655 ? N5 Cu2 N6 94.04(9) . 1_655 ? C35 O3 Cu2 126.64(18) . . ? C37 O4 Cu2 126.93(18) . . ? C28 N5 C25 106.0(2) . . ? C28 N5 Cu2 126.86(19) . . ? C25 N5 Cu2 126.43(18) . . ? C20 N4 C23 106.3(2) . . ? C20 N4 Cu2 126.5(2) . . ? C23 N4 Cu2 126.80(18) . . ? C25 C24 C23 126.0(2) . . ? C25 C24 C29 116.8(2) . . ? C23 C24 C29 117.2(2) . . ? O4 C37 C36 125.2(3) . . ? O4 C37 C38 115.3(3) . . ? C36 C37 C38 119.5(3) . . ? N5 C28 C27 112.2(2) . . ? C27 C26 C25 107.1(2) . . ? O3 C35 C36 125.0(3) . . ? O3 C35 C34 115.7(3) . . ? C36 C35 C34 119.4(3) . . ? C24 C25 N5 123.4(2) . . ? C24 C25 C26 127.8(3) . . ? N5 C25 C26 108.8(2) . . ? N4 C23 C24 123.5(2) . . ? N4 C23 C22 109.1(2) . . ? C24 C23 C22 127.2(3) . . ? C21 C22 C23 107.0(2) . . ? C22 C21 C20 106.3(2) . . ? N4 C20 C21 111.3(3) . . ? C26 C27 C28 105.9(2) . . ? C37 C36 C35 124.3(3) . . ? O1 Cu1 O2 90.88(8) . . ? O1 Cu1 N1 171.54(9) . . ? O2 Cu1 N1 88.89(9) . . ? O1 Cu1 N2 88.34(9) . . ? O2 Cu1 N2 169.14(9) . . ? N1 Cu1 N2 90.29(9) . . ? O1 Cu1 N3 94.07(8) . 1_455 ? O2 Cu1 N3 92.07(8) . 1_455 ? N1 Cu1 N3 94.38(9) . 1_455 ? N2 Cu1 N3 98.78(9) . 1_455 ? C18 O2 Cu1 126.55(18) . . ? C16 O1 Cu1 127.26(18) . . ? C9 N2 C6 106.4(2) . . ? C9 N2 Cu1 126.30(19) . . ? C6 N2 Cu1 126.99(18) . . ? C1 N1 C4 106.1(2) . . ? C1 N1 Cu1 126.41(18) . . ? C4 N1 Cu1 126.84(18) . . ? C12 N3 C11 118.1(2) . . ? C12 N3 Cu1 121.67(18) . 1_655 ? C11 N3 Cu1 119.16(18) . 1_655 ? C4 C5 C6 125.9(2) . . ? C4 C5 C10 116.8(2) . . ? C6 C5 C10 117.3(2) . . ? N1 C1 C2 111.7(2) . . ? C8 C7 C6 107.0(2) . . ? O1 C16 C17 125.1(3) . . ? O1 C16 C15 115.6(2) . . ? C17 C16 C15 119.3(3) . . ? N3 C12 C13 123.2(3) . . ? O2 C18 C17 125.3(3) . . ? O2 C18 C19 115.8(2) . . ? C17 C18 C19 118.9(3) . . ? N3 C11 C10 122.9(3) . . ? C7 C8 C9 106.4(2) . . ? C3 C2 C1 106.2(2) . . ? C5 C4 N1 123.6(2) . . ? C5 C4 C3 127.3(3) . . ? N1 C4 C3 109.1(2) . . ? N2 C6 C5 123.3(2) . . ? N2 C6 C7 108.8(2) . . ? C5 C6 C7 127.8(3) . . ? C12 C13 C14 118.4(3) . . ? N2 C9 C8 111.5(2) . . ? C14 C10 C11 118.2(2) . . ? C14 C10 C5 122.4(2) . . ? C11 C10 C5 119.3(2) . . ? C10 C14 C13 119.2(3) . . ? C2 C3 C4 106.8(2) . . ? C16 C17 C18 124.2(3) . . ? N6 C30 C29 123.0(3) . . ? C29 C33 C32 119.5(3) . . ? C33 C29 C30 118.0(3) . . ? C33 C29 C24 122.4(2) . . ? C30 C29 C24 119.5(2) . . ? C31 N6 C30 118.2(2) . . ? C31 N6 Cu2 122.29(19) . 1_455 ? C30 N6 Cu2 118.53(19) . 1_455 ? N6 C31 C32 123.1(3) . . ? C31 C32 C33 118.1(3) . . ? Cl1 C39 Cl2 112.3(2) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 3.438 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.149 #===END #========================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and Characterization of One-Dimensional Coordination Polymers based on Self-Assembling, Heteroleptic Copper Dipyrromethene Complexes ; loop _publ_author_name _publ_author_address 'Cohen, Seth M.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; 'Halper, Sara R.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; 'Malachowski, Mitchell R.' ; Department of Chemistry University of San Diego San Diego CA 92110-2492 USA ; 'Delaney, Heather M.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; #========================================================================= data_[Cu(2-pyrdpm)(acac)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H17 Cu N3 O2' _chemical_formula_weight 382.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.4788(6) _cell_length_b 9.9354(6) _cell_length_c 35.677(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3359.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 1.317 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21289 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7640 _reflns_number_gt 7182 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+0.1579P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(9) _refine_ls_number_reflns 7640 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5497(3) 0.7323(3) 0.86089(7) 0.0194(5) Uani 1 1 d . . . H1 H 0.4739 0.7724 0.8742 0.023 Uiso 1 1 calc R . . C2 C 0.5327(3) 0.6532(3) 0.82839(7) 0.0210(5) Uani 1 1 d . . . H2 H 0.4464 0.6308 0.8164 0.025 Uiso 1 1 calc R . . C3 C 0.6656(3) 0.6150(2) 0.81765(7) 0.0193(5) Uani 1 1 d . . . H3 H 0.6893 0.5615 0.7965 0.023 Uiso 1 1 calc R . . C4 C 0.7611(3) 0.6705(2) 0.84407(6) 0.0141(5) Uani 1 1 d . . . C5 C 0.9083(3) 0.6590(2) 0.84408(7) 0.0131(5) Uani 1 1 d . . . C6 C 0.9997(2) 0.7222(2) 0.86957(7) 0.0141(5) Uani 1 1 d . . . C7 C 1.1487(3) 0.7133(2) 0.87167(7) 0.0170(5) Uani 1 1 d . . . H7 H 1.2080 0.6623 0.8556 0.020 Uiso 1 1 calc R . . C8 C 1.1920(3) 0.7920(2) 0.90129(7) 0.0196(5) Uani 1 1 d . . . H8 H 1.2861 0.8063 0.9095 0.024 Uiso 1 1 calc R . . C9 C 1.0691(2) 0.8466(2) 0.91678(7) 0.0176(5) Uani 1 1 d . . . H9 H 1.0681 0.9057 0.9377 0.021 Uiso 1 1 calc R . . C10 C 0.9711(2) 0.5690(2) 0.81469(7) 0.0135(5) Uani 1 1 d . . . C11 C 0.9263(3) 0.4366(2) 0.81153(7) 0.0164(5) Uani 1 1 d . . . H11 H 0.8559 0.4025 0.8279 0.020 Uiso 1 1 calc R . . C12 C 0.9847(2) 0.3549(3) 0.78441(7) 0.0190(5) Uani 1 1 d . . . H12 H 0.9545 0.2642 0.7816 0.023 Uiso 1 1 calc R . . C13 C 1.0885(3) 0.4078(3) 0.76132(7) 0.0189(5) Uani 1 1 d . . . H13 H 1.1309 0.3545 0.7423 0.023 Uiso 1 1 calc R . . C14 C 1.1287(3) 0.5405(2) 0.76675(7) 0.0195(5) Uani 1 1 d . . . H14 H 1.2006 0.5760 0.7510 0.023 Uiso 1 1 calc R . . C15 C 0.3816(3) 1.0785(3) 0.93400(7) 0.0204(6) Uani 1 1 d . . . H15A H 0.3421 1.0567 0.9094 0.031 Uiso 1 1 calc R . . H15B H 0.3706 1.1750 0.9388 0.031 Uiso 1 1 calc R . . H15C H 0.3317 1.0272 0.9534 0.031 Uiso 1 1 calc R . . C16 C 0.5362(3) 1.0423(2) 0.93469(7) 0.0165(5) Uani 1 1 d . . . C17 C 0.6285(3) 1.1213(2) 0.95519(7) 0.0180(5) Uani 1 1 d . . . H17 H 0.5946 1.2035 0.9654 0.022 Uiso 1 1 calc R . . C18 C 0.7693(3) 1.0858(2) 0.96165(7) 0.0184(5) Uani 1 1 d . . . C19 C 0.8595(3) 1.1707(3) 0.98722(8) 0.0258(6) Uani 1 1 d . . . H19A H 0.8793 1.1206 1.0103 0.039 Uiso 1 1 calc R . . H19B H 0.8093 1.2540 0.9934 0.039 Uiso 1 1 calc R . . H19C H 0.9484 1.1926 0.9746 0.039 Uiso 1 1 calc R . . C20 C 0.3637(3) 0.4023(2) 0.88309(8) 0.0226(6) Uani 1 1 d . . . H20 H 0.3586 0.4718 0.9013 0.027 Uiso 1 1 calc R . . C21 C 0.2515(3) 0.3639(3) 0.85983(7) 0.0247(5) Uani 1 1 d . . . H21 H 0.1595 0.4018 0.8594 0.030 Uiso 1 1 calc R . . C22 C 0.3008(3) 0.2607(2) 0.83781(7) 0.0204(6) Uani 1 1 d . . . H22 H 0.2490 0.2136 0.8192 0.025 Uiso 1 1 calc R . . C23 C 0.4439(3) 0.2373(2) 0.84812(7) 0.0168(5) Uani 1 1 d . . . C24 C 0.5366(3) 0.1409(3) 0.83378(6) 0.0156(5) Uani 1 1 d . . . C25 C 0.6802(3) 0.1300(2) 0.84342(6) 0.0160(5) Uani 1 1 d . . . C26 C 0.7790(3) 0.0325(2) 0.83113(7) 0.0175(5) Uani 1 1 d . . . H26 H 0.7605 -0.0398 0.8144 0.021 Uiso 1 1 calc R . . C27 C 0.9058(3) 0.0612(3) 0.84764(7) 0.0215(6) Uani 1 1 d . . . H27 H 0.9924 0.0147 0.8442 0.026 Uiso 1 1 calc R . . C28 C 0.8815(3) 0.1740(2) 0.87072(7) 0.0196(5) Uani 1 1 d . . . H28 H 0.9516 0.2151 0.8859 0.023 Uiso 1 1 calc R . . C29 C 0.4799(3) 0.0420(2) 0.80605(7) 0.0164(5) Uani 1 1 d . . . C30 C 0.3558(3) -0.0299(2) 0.81361(7) 0.0183(5) Uani 1 1 d . . . H30 H 0.3061 -0.0160 0.8364 0.022 Uiso 1 1 calc R . . C31 C 0.3067(3) -0.1215(2) 0.78742(7) 0.0210(5) Uani 1 1 d . . . H31 H 0.2217 -0.1697 0.7917 0.025 Uiso 1 1 calc R . . C32 C 0.3827(3) -0.1414(3) 0.75512(7) 0.0192(5) Uani 1 1 d . . . H32 H 0.3519 -0.2040 0.7367 0.023 Uiso 1 1 calc R . . C33 C 0.5065(3) -0.0673(2) 0.74999(7) 0.0188(5) Uani 1 1 d . . . H33 H 0.5598 -0.0826 0.7279 0.023 Uiso 1 1 calc R . . C34 C 0.5432(3) 0.6635(3) 0.97589(8) 0.0294(7) Uani 1 1 d . . . H34A H 0.4849 0.7120 0.9577 0.044 Uiso 1 1 calc R . . H34B H 0.6005 0.7280 0.9901 0.044 Uiso 1 1 calc R . . H34C H 0.4821 0.6136 0.9932 0.044 Uiso 1 1 calc R . . C35 C 0.6381(3) 0.5670(2) 0.95568(7) 0.0229(6) Uani 1 1 d . . . C36 C 0.7839(3) 0.5751(3) 0.96049(8) 0.0235(6) Uani 1 1 d . . . H36 H 0.8194 0.6402 0.9776 0.028 Uiso 1 1 calc R . . C37 C 0.8808(3) 0.4935(3) 0.94178(7) 0.0223(6) Uani 1 1 d . . . C38 C 1.0355(3) 0.5061(3) 0.95026(8) 0.0284(6) Uani 1 1 d . . . H38A H 1.0797 0.4170 0.9491 0.043 Uiso 1 1 calc R . . H38B H 1.0479 0.5438 0.9754 0.043 Uiso 1 1 calc R . . H38C H 1.0798 0.5657 0.9318 0.043 Uiso 1 1 calc R . . Cu1 Cu 0.76044(3) 0.86696(3) 0.908235(8) 0.01468(7) Uani 1 1 d . . . Cu2 Cu 0.66252(3) 0.35692(3) 0.899624(8) 0.01737(7) Uani 1 1 d . . . N1 N 0.6849(2) 0.74394(19) 0.87064(6) 0.0154(4) Uani 1 1 d . . . N2 N 0.9537(2) 0.80581(19) 0.89874(6) 0.0153(4) Uani 1 1 d . . . N3 N 1.0726(2) 0.6219(2) 0.79279(5) 0.0168(4) Uani 1 1 d . . . N4 N 0.4785(2) 0.32875(19) 0.87630(6) 0.0178(5) Uani 1 1 d . . . N5 N 0.7477(2) 0.21599(19) 0.86860(5) 0.0165(4) Uani 1 1 d . . . N6 N 0.5540(2) 0.02372(19) 0.77440(6) 0.0171(4) Uani 1 1 d . . . O1 O 0.57002(17) 0.93596(16) 0.91669(5) 0.0188(4) Uani 1 1 d . . . O2 O 0.83078(19) 0.98314(17) 0.94768(5) 0.0214(4) Uani 1 1 d . . . O3 O 0.5762(2) 0.48187(18) 0.93468(5) 0.0227(4) Uani 1 1 d . . . O4 O 0.84865(19) 0.40505(17) 0.91732(5) 0.0226(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0131(13) 0.0222(12) 0.0229(14) -0.0003(11) 0.0000(10) 0.0021(10) C2 0.0139(12) 0.0241(13) 0.0250(14) -0.0072(12) -0.0039(10) 0.0024(11) C3 0.0193(12) 0.0164(12) 0.0222(13) -0.0067(10) -0.0008(11) 0.0042(11) C4 0.0170(12) 0.0129(10) 0.0125(11) 0.0001(8) 0.0019(10) 0.0012(10) C5 0.0131(12) 0.0096(11) 0.0166(12) 0.0032(9) 0.0023(9) 0.0003(9) C6 0.0128(12) 0.0130(11) 0.0166(13) 0.0023(10) 0.0015(10) 0.0019(9) C7 0.0142(13) 0.0159(11) 0.0210(13) 0.0006(10) 0.0012(10) 0.0004(10) C8 0.0138(12) 0.0207(11) 0.0245(14) -0.0001(11) 0.0005(10) -0.0030(9) C9 0.0169(12) 0.0177(11) 0.0183(12) -0.0022(10) -0.0017(9) -0.0013(10) C10 0.0095(11) 0.0158(11) 0.0152(12) 0.0009(10) -0.0016(9) 0.0026(9) C11 0.0134(12) 0.0171(12) 0.0188(13) 0.0037(10) -0.0016(10) 0.0000(10) C12 0.0200(12) 0.0145(10) 0.0226(13) -0.0049(11) -0.0027(10) -0.0002(11) C13 0.0219(13) 0.0191(12) 0.0156(13) -0.0032(10) 0.0013(10) 0.0046(10) C14 0.0169(13) 0.0233(12) 0.0185(13) 0.0007(10) 0.0043(10) 0.0008(11) C15 0.0160(13) 0.0217(12) 0.0235(14) -0.0050(11) 0.0051(11) 0.0022(10) C16 0.0187(13) 0.0169(12) 0.0140(12) 0.0021(10) 0.0064(10) 0.0019(10) C17 0.0233(13) 0.0143(11) 0.0164(12) -0.0017(10) 0.0051(10) 0.0047(11) C18 0.0247(15) 0.0189(11) 0.0115(12) -0.0002(9) 0.0023(11) -0.0006(11) C19 0.0301(15) 0.0251(13) 0.0222(14) -0.0090(11) -0.0028(12) 0.0032(12) C20 0.0231(14) 0.0169(11) 0.0278(15) -0.0028(10) -0.0004(11) 0.0035(11) C21 0.0205(13) 0.0210(11) 0.0326(14) -0.0001(11) -0.0041(11) 0.0032(13) C22 0.0188(14) 0.0192(12) 0.0233(14) 0.0036(11) -0.0041(10) -0.0020(10) C23 0.0193(13) 0.0153(11) 0.0159(13) 0.0030(10) 0.0009(10) -0.0048(10) C24 0.0214(12) 0.0156(10) 0.0099(11) 0.0066(10) 0.0007(9) -0.0044(11) C25 0.0181(12) 0.0159(11) 0.0141(11) 0.0029(10) 0.0026(9) -0.0035(11) C26 0.0204(14) 0.0169(11) 0.0152(12) 0.0036(10) 0.0044(10) 0.0004(10) C27 0.0201(14) 0.0250(13) 0.0194(14) 0.0059(11) 0.0011(11) 0.0016(11) C28 0.0166(13) 0.0227(12) 0.0195(13) 0.0044(10) -0.0009(10) -0.0017(10) C29 0.0172(13) 0.0148(11) 0.0173(13) 0.0025(10) 0.0000(10) -0.0003(10) C30 0.0154(12) 0.0173(11) 0.0222(13) 0.0023(10) 0.0020(11) -0.0017(10) C31 0.0189(12) 0.0159(12) 0.0282(14) 0.0049(11) -0.0042(10) -0.0034(10) C32 0.0236(13) 0.0149(11) 0.0190(12) -0.0013(11) -0.0070(10) -0.0002(11) C33 0.0204(13) 0.0186(12) 0.0176(13) 0.0001(11) 0.0004(10) 0.0028(11) C34 0.0414(18) 0.0239(15) 0.0230(15) -0.0031(12) 0.0027(13) -0.0001(13) C35 0.0351(17) 0.0177(12) 0.0160(13) 0.0047(10) 0.0018(12) -0.0046(12) C36 0.0317(17) 0.0217(12) 0.0170(13) -0.0039(11) -0.0029(11) -0.0099(12) C37 0.0251(15) 0.0231(13) 0.0187(14) 0.0054(11) -0.0040(11) -0.0071(11) C38 0.0294(16) 0.0266(14) 0.0293(16) 0.0024(13) -0.0087(13) -0.0084(13) Cu1 0.01371(14) 0.01582(13) 0.01452(14) -0.00333(12) 0.00126(11) 0.00099(12) Cu2 0.01699(15) 0.01794(13) 0.01717(15) -0.00202(13) -0.00046(12) -0.00310(13) N1 0.0128(11) 0.0175(10) 0.0160(11) -0.0023(9) 0.0008(8) 0.0000(8) N2 0.0167(11) 0.0149(9) 0.0144(10) -0.0038(8) 0.0014(9) -0.0002(8) N3 0.0153(10) 0.0170(10) 0.0180(10) 0.0012(9) 0.0033(8) 0.0010(9) N4 0.0187(11) 0.0166(10) 0.0181(11) -0.0012(8) -0.0016(9) -0.0006(8) N5 0.0178(11) 0.0175(9) 0.0142(10) 0.0025(8) -0.0005(9) -0.0029(9) N6 0.0191(11) 0.0168(10) 0.0153(11) 0.0021(8) 0.0018(9) 0.0001(9) O1 0.0158(9) 0.0177(8) 0.0227(10) -0.0046(7) 0.0034(7) 0.0006(7) O2 0.0202(10) 0.0232(9) 0.0208(9) -0.0091(8) -0.0032(8) 0.0031(8) O3 0.0248(10) 0.0219(9) 0.0215(10) -0.0047(8) 0.0006(8) -0.0041(8) O4 0.0224(10) 0.0224(9) 0.0230(10) -0.0029(8) -0.0045(8) -0.0049(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.333(3) . ? C1 C2 1.410(4) . ? C2 C3 1.371(3) . ? C3 C4 1.418(3) . ? C4 N1 1.398(3) . ? C4 C5 1.400(3) . ? C5 C6 1.404(3) . ? C5 C10 1.501(3) . ? C6 N2 1.401(3) . ? C6 C7 1.417(3) . ? C7 C8 1.377(3) . ? C8 C9 1.398(3) . ? C9 N2 1.332(3) . ? C10 N3 1.346(3) . ? C10 C11 1.386(3) . ? C11 C12 1.379(3) . ? C12 C13 1.387(4) . ? C13 C14 1.386(3) . ? C14 N3 1.342(3) . ? C15 C16 1.508(3) . ? C16 O1 1.277(3) . ? C16 C17 1.384(4) . ? C17 C18 1.400(4) . ? C18 O2 1.276(3) . ? C18 C19 1.508(4) . ? C20 N4 1.333(3) . ? C20 C21 1.403(4) . ? C21 C22 1.374(4) . ? C22 C23 1.425(3) . ? C23 N4 1.394(3) . ? C23 C24 1.397(3) . ? C24 C25 1.408(3) . ? C24 C29 1.494(3) . ? C25 N5 1.395(3) . ? C25 C26 1.416(3) . ? C26 C27 1.368(4) . ? C27 C28 1.410(4) . ? C28 N5 1.337(3) . ? C29 N6 1.342(3) . ? C29 C30 1.403(3) . ? C30 C31 1.385(3) . ? C31 C32 1.373(4) . ? C32 C33 1.397(4) . ? C33 N6 1.334(3) . ? C34 C35 1.500(4) . ? C35 O3 1.274(3) . ? C35 C36 1.395(4) . ? C36 C37 1.395(4) . ? C37 O4 1.275(3) . ? C37 C38 1.503(4) . ? Cu1 O2 1.9384(17) . ? Cu1 N1 1.951(2) . ? Cu1 O1 1.9542(17) . ? Cu1 N2 1.960(2) . ? Cu2 O4 1.9339(18) . ? Cu2 O3 1.9431(18) . ? Cu2 N4 1.952(2) . ? Cu2 N5 1.959(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.9(2) . . ? C3 C2 C1 106.2(2) . . ? C2 C3 C4 107.1(2) . . ? N1 C4 C5 123.9(2) . . ? N1 C4 C3 108.9(2) . . ? C5 C4 C3 127.2(2) . . ? C4 C5 C6 125.4(2) . . ? C4 C5 C10 116.3(2) . . ? C6 C5 C10 118.3(2) . . ? N2 C6 C5 123.6(2) . . ? N2 C6 C7 107.9(2) . . ? C5 C6 C7 128.4(2) . . ? C8 C7 C6 107.6(2) . . ? C7 C8 C9 106.0(2) . . ? N2 C9 C8 112.0(2) . . ? N3 C10 C11 122.8(2) . . ? N3 C10 C5 117.1(2) . . ? C11 C10 C5 120.0(2) . . ? C12 C11 C10 119.5(2) . . ? C11 C12 C13 118.6(2) . . ? C14 C13 C12 118.2(2) . . ? N3 C14 C13 124.2(2) . . ? O1 C16 C17 125.1(2) . . ? O1 C16 C15 115.6(2) . . ? C17 C16 C15 119.2(2) . . ? C16 C17 C18 123.2(2) . . ? O2 C18 C17 124.9(2) . . ? O2 C18 C19 115.1(2) . . ? C17 C18 C19 120.0(2) . . ? N4 C20 C21 111.2(2) . . ? C22 C21 C20 106.5(2) . . ? C21 C22 C23 107.3(2) . . ? N4 C23 C24 124.3(2) . . ? N4 C23 C22 107.7(2) . . ? C24 C23 C22 128.0(2) . . ? C23 C24 C25 124.8(2) . . ? C23 C24 C29 117.9(2) . . ? C25 C24 C29 117.3(2) . . ? N5 C25 C24 123.6(2) . . ? N5 C25 C26 108.4(2) . . ? C24 C25 C26 128.0(2) . . ? C27 C26 C25 107.8(2) . . ? C26 C27 C28 105.9(2) . . ? N5 C28 C27 111.7(2) . . ? N6 C29 C30 122.1(2) . . ? N6 C29 C24 117.2(2) . . ? C30 C29 C24 120.6(2) . . ? C31 C30 C29 119.1(2) . . ? C32 C31 C30 119.0(2) . . ? C31 C32 C33 118.3(2) . . ? N6 C33 C32 123.7(3) . . ? O3 C35 C36 124.6(3) . . ? O3 C35 C34 115.5(3) . . ? C36 C35 C34 119.9(2) . . ? C35 C36 C37 124.0(3) . . ? O4 C37 C36 124.8(3) . . ? O4 C37 C38 115.4(2) . . ? C36 C37 C38 119.8(3) . . ? O2 Cu1 N1 176.88(8) . . ? O2 Cu1 O1 89.81(7) . . ? N1 Cu1 O1 89.25(8) . . ? O2 Cu1 N2 89.35(8) . . ? N1 Cu1 N2 91.72(8) . . ? O1 Cu1 N2 177.35(8) . . ? O4 Cu2 O3 90.93(8) . . ? O4 Cu2 N4 171.67(8) . . ? O3 Cu2 N4 89.40(8) . . ? O4 Cu2 N5 89.16(8) . . ? O3 Cu2 N5 173.71(8) . . ? N4 Cu2 N5 91.42(9) . . ? C1 N1 C4 105.9(2) . . ? C1 N1 Cu1 125.93(17) . . ? C4 N1 Cu1 127.15(16) . . ? C9 N2 C6 106.5(2) . . ? C9 N2 Cu1 126.14(16) . . ? C6 N2 Cu1 127.10(16) . . ? C14 N3 C10 116.7(2) . . ? C20 N4 C23 107.2(2) . . ? C20 N4 Cu2 124.96(17) . . ? C23 N4 Cu2 127.67(17) . . ? C28 N5 C25 106.2(2) . . ? C28 N5 Cu2 125.58(18) . . ? C25 N5 Cu2 127.81(17) . . ? C33 N6 C29 117.6(2) . . ? C16 O1 Cu1 126.85(17) . . ? C18 O2 Cu1 127.05(17) . . ? C35 O3 Cu2 127.50(18) . . ? C37 O4 Cu2 127.70(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.439 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.066 #===END #========================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and Characterization of One-Dimensional Coordination Polymers based on Self-Assembling, Heteroleptic Copper Dipyrromethene Complexes ; loop _publ_author_name _publ_author_address 'Cohen, Seth M.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; 'Halper, Sara R.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; 'Malachowski, Mitchell R.' ; Department of Chemistry University of San Diego San Diego CA 92110-2492 USA ; 'Delaney, Heather M.' ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; #========================================================================= data_[Cu(4-cydpm)(acac)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H17 Cu N3 O2' _chemical_formula_weight 406.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.9543(10) _cell_length_b 20.6386(18) _cell_length_c 7.6606(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.165(2) _cell_angle_gamma 90.00 _cell_volume 1840.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 1.208 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 218(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6593 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.51 _reflns_number_total 2109 _reflns_number_gt 1982 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+1.3333P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2109 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5000 0.97130(13) 0.7500 0.0429(7) Uani 1 2 d S . . C2 C 0.5000 0.90152(13) 0.7500 0.0354(5) Uani 1 2 d S . . C3 C 0.52662(19) 0.86846(10) 0.9106(3) 0.0407(4) Uani 1 1 d . . . H3 H 0.5449 0.8912 1.0198 0.049 Uiso 1 1 calc R . . C4 C 0.52605(18) 0.80169(9) 0.9091(3) 0.0394(4) Uani 1 1 d . . . H4 H 0.5437 0.7789 1.0182 0.047 Uiso 1 1 calc R . . C5 C 0.5000 0.76774(12) 0.7500 0.0324(5) Uani 1 2 d S . . C6 C 0.5000 0.69528(12) 0.7500 0.0309(5) Uani 1 2 d S . . C7 C 0.40620(16) 0.66493(9) 0.7923(2) 0.0320(4) Uani 1 1 d . . . C8 C 0.30745(17) 0.69424(10) 0.8305(3) 0.0375(4) Uani 1 1 d . . . H8 H 0.2939 0.7389 0.8374 0.045 Uiso 1 1 calc R . . C9 C 0.23567(18) 0.64549(10) 0.8554(3) 0.0423(5) Uani 1 1 d . . . H9 H 0.1630 0.6500 0.8817 0.051 Uiso 1 1 calc R . . C10 C 0.29162(17) 0.58736(10) 0.8340(3) 0.0384(4) Uani 1 1 d . . . H10 H 0.2610 0.5460 0.8450 0.046 Uiso 1 1 calc R . . C11 C 0.40899(18) 0.40627(9) 0.7965(3) 0.0372(4) Uani 1 1 d . . . C12 C 0.3117(2) 0.36868(10) 0.8378(3) 0.0464(5) Uani 1 1 d . . . H12A H 0.2970 0.3836 0.9506 0.070 Uiso 1 1 calc R . . H12B H 0.3314 0.3230 0.8470 0.070 Uiso 1 1 calc R . . H12C H 0.2436 0.3750 0.7428 0.070 Uiso 1 1 calc R . . C13 C 0.5000 0.37526(13) 0.7500 0.0392(6) Uani 1 2 d S . . H13 H 0.5000 0.3297 0.7500 0.047 Uiso 1 2 calc SR . . Cu1 Cu 0.5000 0.532101(14) 0.7500 0.03700(14) Uani 1 2 d S . . N1 N 0.39343(13) 0.59787(8) 0.7963(2) 0.0330(3) Uani 1 1 d . . . N2 N 0.5000 1.02609(12) 0.7500 0.0570(8) Uani 1 2 d S . . O1 O 0.40003(15) 0.46703(6) 0.8080(3) 0.0503(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0499(17) 0.0289(15) 0.0545(17) 0.000 0.0211(14) 0.000 C2 0.0359(12) 0.0222(12) 0.0519(15) 0.000 0.0180(11) 0.000 C3 0.0526(12) 0.0291(10) 0.0417(10) -0.0059(8) 0.0133(9) -0.0015(8) C4 0.0551(11) 0.0270(9) 0.0365(10) 0.0009(7) 0.0116(8) 0.0013(8) C5 0.0372(12) 0.0231(11) 0.0390(13) 0.000 0.0129(10) 0.000 C6 0.0410(13) 0.0212(11) 0.0309(12) 0.000 0.0087(10) 0.000 C7 0.0385(9) 0.0247(9) 0.0340(9) 0.0011(7) 0.0108(7) 0.0023(7) C8 0.0417(10) 0.0291(9) 0.0435(10) 0.0014(8) 0.0138(8) 0.0075(8) C9 0.0385(10) 0.0397(11) 0.0527(12) 0.0034(9) 0.0183(9) 0.0052(8) C10 0.0390(10) 0.0313(10) 0.0473(10) 0.0023(8) 0.0150(8) -0.0015(8) C11 0.0439(10) 0.0274(9) 0.0371(9) 0.0018(7) 0.0026(8) -0.0048(7) C12 0.0537(12) 0.0331(10) 0.0518(12) 0.0025(9) 0.0103(10) -0.0110(9) C13 0.0518(16) 0.0230(12) 0.0402(14) 0.000 0.0052(12) 0.000 Cu1 0.0381(2) 0.02020(19) 0.0566(2) 0.000 0.01903(15) 0.000 N1 0.0375(8) 0.0236(7) 0.0405(8) 0.0017(6) 0.0140(6) -0.0008(6) N2 0.082(2) 0.0267(13) 0.0688(19) 0.000 0.0312(17) 0.000 O1 0.0497(9) 0.0244(7) 0.0843(12) -0.0001(6) 0.0307(9) -0.0020(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.131(4) . ? C1 C2 1.440(4) . ? C2 C3 1.379(2) . ? C2 C3 1.379(2) 2_656 ? C3 C4 1.378(3) . ? C4 C5 1.379(2) . ? C5 C4 1.379(2) 2_656 ? C5 C6 1.495(3) . ? C6 C7 1.386(2) . ? C6 C7 1.386(2) 2_656 ? C7 N1 1.394(2) . ? C7 C8 1.415(3) . ? C8 C9 1.364(3) . ? C9 C10 1.401(3) . ? C10 N1 1.331(3) . ? C11 O1 1.263(2) . ? C11 C13 1.377(3) . ? C11 C12 1.490(3) . ? C13 C11 1.377(3) 2_656 ? Cu1 O1 1.9160(16) . ? Cu1 O1 1.9160(16) 2_656 ? Cu1 N1 1.9486(16) 2_656 ? Cu1 N1 1.9486(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 C2 180.000(1) . . ? C3 C2 C3 120.7(3) . 2_656 ? C3 C2 C1 119.65(13) . . ? C3 C2 C1 119.65(13) 2_656 . ? C4 C3 C2 119.17(19) . . ? C3 C4 C5 121.03(19) . . ? C4 C5 C4 118.9(2) . 2_656 ? C4 C5 C6 120.55(12) . . ? C4 C5 C6 120.55(12) 2_656 . ? C7 C6 C7 126.2(2) . 2_656 ? C7 C6 C5 116.88(12) . . ? C7 C6 C5 116.88(12) 2_656 . ? C6 C7 N1 123.56(18) . . ? C6 C7 C8 127.79(19) . . ? N1 C7 C8 108.61(16) . . ? C9 C8 C7 107.15(17) . . ? C8 C9 C10 106.43(18) . . ? N1 C10 C9 111.74(18) . . ? O1 C11 C13 124.3(2) . . ? O1 C11 C12 114.8(2) . . ? C13 C11 C12 120.89(19) . . ? C11 C13 C11 124.6(3) 2_656 . ? O1 Cu1 O1 90.99(9) . 2_656 ? O1 Cu1 N1 177.01(7) . 2_656 ? O1 Cu1 N1 88.73(7) 2_656 2_656 ? O1 Cu1 N1 88.73(7) . . ? O1 Cu1 N1 177.01(7) 2_656 . ? N1 Cu1 N1 91.70(9) 2_656 . ? C10 N1 C7 106.07(16) . . ? C10 N1 Cu1 126.45(14) . . ? C7 N1 Cu1 127.47(13) . . ? C11 O1 Cu1 127.76(16) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.433 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.095