data_global

#============================================================================

# 1. SUBMISSION DETAILS 
_publ_contact_author
;
Isabel López-Solera
Departamento de Química Inórganica, Orgánica y Bioquímica
Facultad de Químicas
Universidad Castilla La Mancha
13071-Ciudad Real 
Spain
;
_publ_contact_author_phone        '+34 926 295300 (ext:3477)'   
_publ_contact_author_fax          '+34 926 295318'
_publ_contact_author_email        Mabel.Lopez@uclm.es
_publ_requested_journal           'Organometallics'
_publ_requested_coeditor_name     ?
_publ_contact_letter              ?
;
20th July, 2007
Please consider this CIF submission as supplementary material of
the structure containing in a paper which we are submitting
to Organometallics.
;

#============================================================================

# 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic?
_journal_date_to_coeditor         ?
_journal_date_from_coeditor       ?
_journal_date_accepted            ?
_journal_date_printers_first      ?
_journal_date_printers_final      ?
_journal_date_proofs_out          ?
_journal_date_proofs_in           ?
_journal_coeditor_name            ?
_journal_coeditor_code            ?
_journal_coeditor_notes           ?
_journal_techeditor_code          ?
_journal_techeditor_notes         ?
_journal_coden_ASTM               ?
_journal_name_full                ?
_journal_year                     ?
_journal_volume                   ?
_journal_issue                    ?
_journal_page_first               ?
_journal_page_last                ?
_journal_suppl_publ_number        ?
_journal_suppl_publ_pages         ?

#============================================================================

# 3. TITLE AND AUTHOR LIST
_publ_section_title             
;
Well-defined alkyl heteroscorpionate magnesium complexes as excellent initiators
for the ROP of cyclic esters 
;
# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.
loop_
_publ_author_name               
_publ_author_address            
     'Sánchez-Barba, Luis F.'
;    Departamento de Química Inorgánica y Analítica 
     Universidad Rey Juan Carlos
     Móstoles
     28933-Madrid
     Spain
;     
     'Garcés, Andrés'
;    Departamento de Química Inorgánica y Analítica 
     Universidad Rey Juan Carlos
     Móstoles
     28933-Madrid
     Spain
;     
     'Fajardo, Mariano'
;    Departamento de Química Inorgánica y Analítica 
     Universidad Rey Juan Carlos
     Móstoles
     28933-Madrid
     Spain
;     
     'Alonso-Moreno, Carlos'
;    Departamento de Química Inorgánica y Analítica 
     Universidad Rey Juan Carlos
     Móstoles
     28933-Madrid
     Spain
;     
     'Fernández-Baeza, Juan'
;    Departamento de Química Inórganica, Orgánica y Bioquímica
     Universidad Castilla-La Mancha
     Facultad de Químicas
     Campus de Ciudad Real
     13071-Ciudad Real
     Spain
;     
     'Otero, Antonio'
;    Departamento de Química Inórganica, Orgánica y Bioquímica
     Universidad Castilla-La Mancha
     Facultad de Químicas
     Campus de Ciudad Real
     13071-Ciudad Real
     Spain
;     
     'Antiñolo, Antonio'
;    Departamento de Química Inórganica, Orgánica y Bioquímica
     Universidad Castilla-La Mancha
     Facultad de Químicas
     Campus de Ciudad Real
     13071-Ciudad Real
     Spain
;     
     'Tejeda, Juan'
;    Departamento de Química Inórganica, Orgánica y Bioquímica
     Universidad Castilla-La Mancha
     Facultad de Químicas
     Campus de Ciudad Real
     13071-Ciudad Real
     Spain
;     
     'Lara-Sánchez, Agustín'
;    Departamento de Química Inórganica, Orgánica y Bioquímica
     Universidad Castilla-La Mancha
     Facultad de Químicas
     Campus de Ciudad Real
     13071-Ciudad Real
     Spain
;
     'López-Solera, Isabel'
;    Departamento de Química Inórganica, Orgánica y Bioquímica
     Universidad Castilla-La Mancha
     Facultad de Químicas
     Campus de Ciudad Real
     13071-Ciudad Real
     Spain
;     
       
#============================================================================

data_compound 9
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C40 D4 H60 Cl14 Mg N12' 
_chemical_formula_weight          1237.64 
 
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' 
 'Mg'  'Mg'   0.0486   0.0363 
 '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            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    11.453(3) 
_cell_length_b                    14.319(3) 
_cell_length_c                    17.840(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.953(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      2910.0(11) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     180(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.31 
_exptl_crystal_size_mid           0.22
_exptl_crystal_size_min           0.15
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.408 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1276 
_exptl_absorpt_coefficient_mu     0.714 
_exptl_absorpt_correction_type    'Semi-empirical' 
_exptl_absorpt_correction_T_min   0.6343 
_exptl_absorpt_correction_T_max   1
_exptl_absorpt_process_details    'SADABS' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       180(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        'omega scan' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             6084 
_diffrn_reflns_av_R_equivalents   0.0591 
_diffrn_reflns_av_sigmaI/netI     0.0492 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          1.79 
_diffrn_reflns_theta_max          16.52 
_reflns_number_total              1549 
_reflns_number_gt                 1168 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Bruker APEX' 
_computing_cell_refinement        'Bruker SAINT' 
_computing_data_reduction         'Bruker SHELXTL' 
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1723P)²+15.5392P] where P=(Fo²+2Fc²)/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      SHELXL 
_refine_ls_extinction_coef        0.0002(15) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          1549 
_refine_ls_number_parameters      374 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0676 
_refine_ls_R_factor_gt            0.0506 
_refine_ls_wR_factor_ref          0.1795 
_refine_ls_wR_factor_gt           0.1533 
_refine_ls_goodness_of_fit_ref    0.741 
_refine_ls_restrained_S_all       0.741 
_refine_ls_shift/su_max           3.563 
_refine_ls_shift/su_mean          0.673 
 
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 
Mg1 Mg 0.5000 0.0000 0.0000 0.038(2) Uani 1 2 d S . . 
C5 C 0.7972(17) 0.1795(10) -0.0284(7) 0.039(4) Uani 1 1 d . . . 
C7 C 0.8336(11) 0.2792(9) -0.0307(8) 0.055(5) Uani 1 1 d . . . 
H7A H 0.7765 0.3136 -0.0628 0.066 Uiso 1 1 calc R . . 
H7B H 0.9086 0.2834 -0.0500 0.066 Uiso 1 1 calc R . . 
H7C H 0.8393 0.3048 0.0193 0.066 Uiso 1 1 calc R . . 
C4 C 0.8518(14) 0.0970(16) -0.0480(8) 0.051(4) Uani 1 1 d . . . 
H4 H 0.9253 0.0919 -0.0654 0.061 Uiso 1 1 calc R . . 
C6 C 0.7985(12) -0.0792(10) -0.0450(7) 0.055(4) Uani 1 1 d . . . 
H6A H 0.8494 -0.1007 -0.0023 0.066 Uiso 1 1 calc R . . 
H6B H 0.8354 -0.0894 -0.0902 0.066 Uiso 1 1 calc R . . 
H6C H 0.7258 -0.1130 -0.0478 0.066 Uiso 1 1 calc R . . 
C3 C 0.775(2) 0.0233(14) -0.0364(8) 0.045(5) Uani 1 1 d . . . 
N4 N 0.4956(12) 0.2090(12) -0.0331(7) 0.036(3) Uani 1 1 d . . . 
C2 C 0.5990(16) 0.2032(10) 0.0221(8) 0.033(4) Uani 1 1 d . . . 
H2 H 0.6281 0.2671 0.0307 0.040 Uiso 1 1 calc R . . 
N3 N 0.4380(14) 0.1281(9) -0.0576(8) 0.036(3) Uani 1 1 d . . . 
N6 N 0.5130(10) 0.0884(10) 0.0977(6) 0.034(3) Uani 1 1 d . . . 
N1 N 0.6774(12) 0.0544(12) -0.0108(6) 0.039(3) Uani 1 1 d . . . 
N2 N 0.6925(14) 0.1504(12) -0.0060(6) 0.036(3) Uani 1 1 d . . . 
C11 C 0.2673(12) 0.0873(9) -0.1502(8) 0.052(4) Uani 1 1 d . . . 
H11A H 0.2805 0.0260 -0.1292 0.063 Uiso 1 1 calc R . . 
H11B H 0.2780 0.0859 -0.2029 0.063 Uiso 1 1 calc R . . 
H11C H 0.1886 0.1067 -0.1441 0.063 Uiso 1 1 calc R . . 
C8 C 0.3523(16) 0.1543(15) -0.1105(10) 0.037(4) Uani 1 1 d . . . 
C9 C 0.3565(15) 0.2513(16) -0.1198(9) 0.039(4) Uani 1 1 d . . . 
H9 H 0.3067 0.2868 -0.1529 0.047 Uiso 1 1 calc R . . 
N5 N 0.6213(10) 0.2089(8) 0.1616(9) 0.037(3) Uani 1 1 d . . . 
H5 H 0.635(10) 0.171(8) 0.207(7) 0.050 Uiso 1 1 d . . . 
C1 C 0.5701(15) 0.1654(15) 0.0983(10) 0.033(4) Uani 1 1 d . . . 
C15 C 0.6623(13) 0.3156(9) 0.2666(7) 0.063(5) Uani 1 1 d . . . 
H15A H 0.7389 0.2889 0.2781 0.075 Uiso 1 1 calc R . . 
H15B H 0.6066 0.2816 0.2927 0.075 Uiso 1 1 calc R . . 
H15C H 0.6635 0.3797 0.2824 0.075 Uiso 1 1 calc R . . 
C14 C 0.7139(14) 0.3665(9) 0.1422(8) 0.067(5) Uani 1 1 d . . . 
H14A H 0.7877 0.3341 0.1455 0.080 Uiso 1 1 calc R . . 
H14B H 0.7246 0.4265 0.1658 0.080 Uiso 1 1 calc R . . 
H14C H 0.6847 0.3745 0.0902 0.080 Uiso 1 1 calc R . . 
C16 C 0.5025(13) 0.3547(10) 0.1623(9) 0.068(5) Uani 1 1 d . . . 
H16A H 0.5067 0.4206 0.1720 0.082 Uiso 1 1 calc R . . 
H16B H 0.4481 0.3265 0.1929 0.082 Uiso 1 1 calc R . . 
H16C H 0.4766 0.3442 0.1100 0.082 Uiso 1 1 calc R . . 
C13 C 0.6270(13) 0.3102(11) 0.1816(8) 0.044(4) Uani 1 1 d . . . 
C17 C 0.4804(11) 0.0467(9) 0.1693(8) 0.044(4) Uani 1 1 d . . . 
H17A H 0.5520 0.0331 0.2014 0.053 Uiso 1 1 calc R . . 
H17B H 0.4409 -0.0122 0.1575 0.053 Uiso 1 1 calc R . . 
C18 C 0.4010(12) 0.1072(9) 0.2143(7) 0.050(4) Uani 1 1 d . . . 
H18A H 0.4467 0.1564 0.2394 0.060 Uiso 1 1 calc R . . 
H18B H 0.3677 0.0692 0.2509 0.060 Uiso 1 1 calc R . . 
H18C H 0.3392 0.1339 0.1805 0.060 Uiso 1 1 calc R . . 
C10 C 0.4470(17) 0.2841(13) -0.0714(11) 0.038(4) Uani 1 1 d . . . 
C12 C 0.4916(11) 0.3824(10) -0.0580(7) 0.047(4) Uani 1 1 d . . . 
H12A H 0.4408 0.4252 -0.0872 0.056 Uiso 1 1 calc R . . 
H12B H 0.5696 0.3873 -0.0728 0.056 Uiso 1 1 calc R . . 
H12C H 0.4927 0.3974 -0.0055 0.056 Uiso 1 1 calc R . . 
C20 C 0.8306(17) 0.9006(13) 0.4064(11) 0.089(6) Uani 1 1 d . . . 
D20 D 0.803(10) 0.961(9) 0.381(6) 0.12(4) Uiso 1 1 d . A 1 
Cl1 Cl 0.827(6) 0.801(3) 0.381(11) 0.32(4) Uani 0.56(13) 1 d P B 1 
Cl2 Cl 0.972(6) 0.930(6) 0.395(4) 0.39(9) Uani 0.17(9) 1 d P B 1 
Cl3 Cl 0.801(2) 0.935(4) 0.5121(13) 0.125(14) Uani 0.32(4) 1 d P B 1 
Cl1A Cl 0.833(2) 0.7975(18) 0.3381(17) 0.104(17) Uani 0.44(13) 1 d P B 2 
Cl2A Cl 0.9718(12) 0.9463(8) 0.4129(13) 0.143(9) Uani 0.83(9) 1 d P B 2 
Cl3A Cl 0.7969(9) 0.8576(19) 0.4893(8) 0.111(11) Uani 0.68(4) 1 d P B 2 
C21 C -0.0312(18) 0.0977(17) 0.2406(10) 0.108(8) Uani 1 1 d . . . 
Cl4 Cl -0.0791(4) 0.1298(3) 0.1502(2) 0.0897(19) Uani 1 1 d . D . 
D21 D -0.076(18) 0.082(13) 0.264(12) 0.07(9) Uiso 1 1 d . C 1 
Cl5 Cl 0.1025(19) 0.069(3) 0.2666(15) 0.093(14) Uani 0.29(3) 1 d P D 1 
Cl6 Cl -0.015(4) 0.249(4) 0.283(2) 0.08(2) Uani 0.20(6) 1 d P E 1 
Cl5A Cl 0.0573(12) -0.0075(16) 0.2305(8) 0.132(10) Uani 0.71(3) 1 d P D 2 
Cl6A Cl 0.038(2) 0.177(3) 0.2944(6) 0.177(19) Uani 0.80(6) 1 d P D 2 
Cl7 Cl 0.7069(3) 0.0764(2) 0.31285(18) 0.0519(15) Uani 1 1 d . . . 
 
 
_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 
Mg1 N6 2.147(11) . ? 
Mg1 N6 2.147(11) 3_655 ? 
Mg1 N3 2.185(13) 3_655 ? 
Mg1 N3 2.185(13) . ? 
Mg1 N1 2.204(13) 3_655 ? 
Mg1 N1 2.204(13) . ? 
C5 N2 1.367(16) . ? 
C5 C4 1.397(17) . ? 
C5 C7 1.489(17) . ? 
C4 C3 1.404(18) . ? 
C6 C3 1.504(19) . ? 
C3 N1 1.326(17) . ? 
N4 C10 1.361(17) . ? 
N4 N3 1.382(13) . ? 
N4 C2 1.461(16) . ? 
C2 N2 1.443(16) . ? 
C2 C1 1.532(19) . ? 
N3 C8 1.343(15) . ? 
N6 C1 1.282(17) . ? 
N6 C17 1.492(16) . ? 
N1 N2 1.386(13) . ? 
C11 C8 1.493(18) . ? 
C8 C9 1.400(18) . ? 
C9 C10 1.361(16) . ? 
N5 C1 1.367(18) . ? 
N5 C13 1.494(17) . ? 
C15 C13 1.531(17) . ? 
C14 C13 1.509(18) . ? 
C16 C13 1.566(18) . ? 
C17 C18 1.540(16) . ? 
C10 C12 1.509(19) . ? 
C20 Cl1 1.50(6) . ? 
C20 Cl3A 1.68(2) . ? 
C20 Cl2A 1.74(2) . ? 
C20 Cl2 1.71(7) . ? 
C20 Cl1A 1.92(4) . ? 
C20 Cl3 2.01(4) . ? 
C21 Cl5 1.61(2) . ? 
C21 Cl6A 1.64(3) . ? 
C21 Cl4 1.711(18) . ? 
C21 Cl5A 1.84(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 
N6 Mg1 N6 179.998(1) . 3_655 ? 
N6 Mg1 N3 97.0(5) . 3_655 ? 
N6 Mg1 N3 83.0(5) 3_655 3_655 ? 
N6 Mg1 N3 83.0(5) . . ? 
N6 Mg1 N3 97.0(5) 3_655 . ? 
N3 Mg1 N3 179.998(1) 3_655 . ? 
N6 Mg1 N1 97.1(6) . 3_655 ? 
N6 Mg1 N1 82.9(6) 3_655 3_655 ? 
N3 Mg1 N1 85.4(6) 3_655 3_655 ? 
N3 Mg1 N1 94.6(6) . 3_655 ? 
N6 Mg1 N1 82.9(6) . . ? 
N6 Mg1 N1 97.1(6) 3_655 . ? 
N3 Mg1 N1 94.6(6) 3_655 . ? 
N3 Mg1 N1 85.4(6) . . ? 
N1 Mg1 N1 179.999(1) 3_655 . ? 
N2 C5 C4 104.1(12) . . ? 
N2 C5 C7 123.9(17) . . ? 
C4 C5 C7 132(2) . . ? 
C3 C4 C5 107.1(14) . . ? 
N1 C3 C4 111.2(15) . . ? 
N1 C3 C6 122.0(19) . . ? 
C4 C3 C6 127(2) . . ? 
C10 N4 N3 110.2(12) . . ? 
C10 N4 C2 130.1(17) . . ? 
N3 N4 C2 119.5(16) . . ? 
N2 C2 N4 112.0(11) . . ? 
N2 C2 C1 111.1(12) . . ? 
N4 C2 C1 112.5(13) . . ? 
C8 N3 N4 106.2(12) . . ? 
C8 N3 Mg1 138.0(15) . . ? 
N4 N3 Mg1 115.7(14) . . ? 
C1 N6 C17 120.6(12) . . ? 
C1 N6 Mg1 120.5(12) . . ? 
C17 N6 Mg1 117.2(10) . . ? 
C3 N1 N2 104.5(12) . . ? 
C3 N1 Mg1 136.7(15) . . ? 
N2 N1 Mg1 117.1(13) . . ? 
C5 N2 N1 113.1(11) . . ? 
C5 N2 C2 130.3(16) . . ? 
N1 N2 C2 116.6(16) . . ? 
N3 C8 C9 109.2(13) . . ? 
N3 C8 C11 123.2(19) . . ? 
C9 C8 C11 128(2) . . ? 
C10 C9 C8 107.5(13) . . ? 
C1 N5 C13 130.0(13) . . ? 
N6 C1 N5 125.0(14) . . ? 
N6 C1 C2 116.9(17) . . ? 
N5 C1 C2 117.3(17) . . ? 
C14 C13 N5 114.9(11) . . ? 
C14 C13 C15 108.4(12) . . ? 
N5 C13 C15 106.6(12) . . ? 
C14 C13 C16 108.1(12) . . ? 
N5 C13 C16 109.1(11) . . ? 
C15 C13 C16 109.8(12) . . ? 
N6 C17 C18 115.7(10) . . ? 
C9 C10 N4 106.9(13) . . ? 
C9 C10 C12 130(2) . . ? 
N4 C10 C12 122.9(19) . . ? 
Cl1 C20 Cl3A 85(8) . . ? 
Cl1 C20 Cl2A 112(4) . . ? 
Cl3A C20 Cl2A 112.1(14) . . ? 
Cl1 C20 Cl2 101(5) . . ? 
Cl3A C20 Cl2 120(3) . . ? 
Cl2A C20 Cl2 13(3) . . ? 
Cl1 C20 Cl1A 22(7) . . ? 
Cl3A C20 Cl1A 107.3(15) . . ? 
Cl2A C20 Cl1A 104.8(14) . . ? 
Cl2 C20 Cl1A 92(3) . . ? 
Cl1 C20 Cl3 121(8) . . ? 
Cl3A C20 Cl3 36.1(9) . . ? 
Cl2A C20 Cl3 95.1(13) . . ? 
Cl2 C20 Cl3 108(3) . . ? 
Cl1A C20 Cl3 143.4(18) . . ? 
Cl5 C21 Cl6A 68(3) . . ? 
Cl5 C21 Cl4 122.9(15) . . ? 
Cl6A C21 Cl4 117.0(19) . . ? 
Cl5 C21 Cl5A 45.5(13) . . ? 
Cl6A C21 Cl5A 113(2) . . ? 
Cl4 C21 Cl5A 104.8(12) . . ? 
 
_diffrn_measured_fraction_theta_max    0.993 
_diffrn_reflns_theta_full              16.52 
_diffrn_measured_fraction_theta_full   0.993 
_refine_diff_density_max    0.541 
_refine_diff_density_min   -0.206 
_refine_diff_density_rms    0.051 

#=======================================================================


 
data_compound 1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C21 H33 Mg N6' 
_chemical_formula_weight          393.84 
 
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' 
 'Mg'  'Mg'   0.0486   0.0363 
 '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                    12.001(4) 
_cell_length_b                    13.847(5) 
_cell_length_c                    14.450(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  113.049(5) 
_cell_angle_gamma                 90.00 
_cell_volume                      2209.6(13) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     130(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.43 
_exptl_crystal_size_mid           0.34
_exptl_crystal_size_min           0.21
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.184 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              852 
_exptl_absorpt_coefficient_mu     0.099 
_exptl_absorpt_correction_type    'Semi-empirical'
_exptl_absorpt_correction_T_min   0.8709 
_exptl_absorpt_correction_T_max   1
_exptl_absorpt_process_details    'SADABS'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       130(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        'omega scan' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             7094 
_diffrn_reflns_av_R_equivalents   0.0424 
_diffrn_reflns_av_sigmaI/netI     0.0366 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          1.88 
_diffrn_reflns_theta_max          19.07 
_reflns_number_total              1793 
_reflns_number_gt                 1467 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Bruker APEX' 
_computing_cell_refinement        'Bruker SAINT' 
_computing_data_reduction         'Bruker SHELXTL' 
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1751P)²+11.2259P] where P=(Fo²+2Fc²)/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      SHELXL 
_refine_ls_extinction_coef        0.0024(12) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          1793 
_refine_ls_number_parameters      262 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0527 
_refine_ls_R_factor_gt            0.0423 
_refine_ls_wR_factor_ref          0.1401 
_refine_ls_wR_factor_gt           0.1212 
_refine_ls_goodness_of_fit_ref    0.532 
_refine_ls_restrained_S_all       0.532 
_refine_ls_shift/su_max           0.041 
_refine_ls_shift/su_mean          0.001 
 
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 
Mg1 Mg 1.17141(11) 0.05887(9) 0.76872(9) 0.0223(5) Uani 1 1 d . . . 
N4 N 0.9569(3) -0.0616(2) 0.6723(2) 0.0192(9) Uani 1 1 d . . . 
N3 N 1.0605(3) -0.0395(2) 0.6585(2) 0.0212(9) Uani 1 1 d . . . 
N1 N 1.0180(3) -0.0466(2) 0.8501(2) 0.0197(9) Uani 1 1 d . . . 
N2 N 1.1385(3) -0.0282(2) 0.8766(2) 0.0217(9) Uani 1 1 d . . . 
C12 C 0.9186(4) 0.0965(3) 0.7424(2) 0.0184(10) Uani 1 1 d . . . 
N6 N 1.0216(3) 0.1409(2) 0.7489(2) 0.0205(9) Uani 1 1 d . . . 
N5 N 0.8179(3) 0.1391(2) 0.7311(2) 0.0241(9) Uani 1 1 d . . . 
C11 C 0.9322(3) -0.0152(3) 0.7532(3) 0.0206(10) Uani 1 1 d . . . 
H11 H 0.8532 -0.0397 0.7477 0.025 Uiso 1 1 calc R . . 
C7 C 0.9520(4) -0.1484(3) 0.5460(3) 0.0268(11) Uani 1 1 d . . . 
H7 H 0.9282 -0.1911 0.4921 0.032 Uiso 1 1 calc R . . 
C19 C 1.1493(3) 0.2729(3) 0.7454(3) 0.0299(11) Uani 1 1 d . . . 
H19A H 1.2093 0.2511 0.8083 0.045 Uiso 1 1 calc R . . 
H19B H 1.1557 0.3415 0.7400 0.045 Uiso 1 1 calc R . . 
H19C H 1.1620 0.2418 0.6910 0.045 Uiso 1 1 calc R . . 
C5 C 0.8759(3) -0.1293(3) 0.9121(3) 0.0282(11) Uani 1 1 d . . . 
H5A H 0.8204 -0.0760 0.8920 0.042 Uiso 1 1 calc R . . 
H5B H 0.8798 -0.1542 0.9753 0.042 Uiso 1 1 calc R . . 
H5C H 0.8486 -0.1791 0.8620 0.042 Uiso 1 1 calc R . . 
C18 C 1.0236(3) 0.2476(3) 0.7408(3) 0.0240(11) Uani 1 1 d . . . 
C3 C 0.9980(4) -0.0960(3) 0.9228(3) 0.0203(10) Uani 1 1 d . . . 
C14 C 0.7050(3) 0.0880(3) 0.7133(3) 0.0273(11) Uani 1 1 d . . . 
H14A H 0.6603 0.1222 0.7463 0.033 Uiso 1 1 calc R . . 
H14B H 0.7232 0.0239 0.7423 0.033 Uiso 1 1 calc R . . 
C6 C 1.0564(3) -0.0933(3) 0.5805(3) 0.0214(10) Uani 1 1 d . . . 
C15 C 0.6273(4) 0.0797(3) 0.6017(3) 0.0353(12) Uani 1 1 d . . . 
H15A H 0.6088 0.1431 0.5729 0.053 Uiso 1 1 calc R . . 
H15B H 0.5534 0.0465 0.5925 0.053 Uiso 1 1 calc R . . 
H15C H 0.6705 0.0442 0.5692 0.053 Uiso 1 1 calc R . . 
C2 C 1.1091(4) -0.1091(3) 0.9992(3) 0.0238(11) Uani 1 1 d . . . 
H2 H 1.1246 -0.1399 1.0602 0.029 Uiso 1 1 calc R . . 
C4 C 1.3279(4) -0.0632(3) 1.0202(3) 0.0349(12) Uani 1 1 d . . . 
H4A H 1.3621 -0.1235 1.0118 0.052 Uiso 1 1 calc R . . 
H4B H 1.3496 -0.0512 1.0906 0.052 Uiso 1 1 calc R . . 
H4C H 1.3586 -0.0120 0.9919 0.052 Uiso 1 1 calc R . . 
C1 C 1.1942(4) -0.0674(3) 0.9684(3) 0.0232(11) Uani 1 1 d . . . 
C20 C 1.3592(4) 0.0788(3) 0.8011(3) 0.0341(12) Uani 1 1 d . . . 
H20 H 1.4191 0.0650 0.8638 0.041 Uiso 1 1 calc R . . 
C9 C 1.1557(4) -0.0865(3) 0.5426(3) 0.0303(11) Uani 1 1 d . . . 
H9A H 1.2081 -0.0335 0.5750 0.045 Uiso 1 1 calc R . . 
H9B H 1.1213 -0.0761 0.4712 0.045 Uiso 1 1 calc R . . 
H9C H 1.2014 -0.1455 0.5572 0.045 Uiso 1 1 calc R . . 
C21 C 1.3873(4) 0.1153(3) 0.7183(3) 0.0358(12) Uani 1 1 d . . . 
H21 H 1.3897 0.0695 0.6722 0.043 Uiso 1 1 calc R . . 
C22 C 1.4099(4) 0.2056(4) 0.7000(3) 0.0387(12) Uani 1 1 d . . . 
H22A H 1.4088 0.2550 0.7433 0.046 Uiso 1 1 calc R . . 
H22B H 1.4267 0.2195 0.6439 0.046 Uiso 1 1 calc R . . 
C8 C 0.8901(3) -0.1287(3) 0.6054(3) 0.0224(11) Uani 1 1 d . . . 
C10 C 0.7760(4) -0.1695(3) 0.6053(3) 0.0357(12) Uani 1 1 d . . . 
H10A H 0.7934 -0.2083 0.6644 0.054 Uiso 1 1 calc R . . 
H10B H 0.7382 -0.2088 0.5465 0.054 Uiso 1 1 calc R . . 
H10C H 0.7224 -0.1179 0.6049 0.054 Uiso 1 1 calc R . . 
C24 C 0.9309(4) 0.2864(3) 0.6419(3) 0.0333(11) Uani 1 1 d . . . 
H24A H 0.9473 0.2604 0.5870 0.050 Uiso 1 1 calc R . . 
H24B H 0.9361 0.3556 0.6414 0.050 Uiso 1 1 calc R . . 
H24C H 0.8511 0.2677 0.6352 0.050 Uiso 1 1 calc R . . 
C25 C 1.0065(4) 0.2967(3) 0.8295(3) 0.0340(12) Uani 1 1 d . . . 
H25A H 0.9281 0.2807 0.8283 0.051 Uiso 1 1 calc R . . 
H25B H 1.0127 0.3654 0.8242 0.051 Uiso 1 1 calc R . . 
H25C H 1.0680 0.2747 0.8914 0.051 Uiso 1 1 calc R . . 
 
 
_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 
Mg1 N6 2.050(3) . ? 
Mg1 N3 2.122(3) . ? 
Mg1 N2 2.126(3) . ? 
Mg1 C20 2.133(4) . ? 
N4 C8 1.354(5) . ? 
N4 N3 1.368(4) . ? 
N4 C11 1.462(5) . ? 
N3 C6 1.335(5) . ? 
N1 C3 1.352(5) . ? 
N1 N2 1.368(4) . ? 
N1 C11 1.442(5) . ? 
N2 C1 1.344(5) . ? 
C12 N5 1.296(5) . ? 
C12 N6 1.350(5) . ? 
C12 C11 1.558(5) . ? 
N6 C18 1.483(5) . ? 
N5 C14 1.459(5) . ? 
C7 C8 1.364(5) . ? 
C7 C6 1.383(5) . ? 
C19 C18 1.524(5) . ? 
C5 C3 1.484(5) . ? 
C18 C24 1.524(5) . ? 
C18 C25 1.533(5) . ? 
C3 C2 1.370(5) . ? 
C14 C15 1.518(5) . ? 
C6 C9 1.497(5) . ? 
C2 C1 1.390(5) . ? 
C4 C1 1.483(6) . ? 
C20 C21 1.454(6) . ? 
C21 C22 1.328(6) . ? 
C8 C10 1.482(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 
N6 Mg1 N3 89.57(13) . . ? 
N6 Mg1 N2 90.69(13) . . ? 
N3 Mg1 N2 86.81(13) . . ? 
N6 Mg1 C20 138.84(16) . . ? 
N3 Mg1 C20 123.10(16) . . ? 
N2 Mg1 C20 113.33(15) . . ? 
C8 N4 N3 111.6(3) . . ? 
C8 N4 C11 128.6(3) . . ? 
N3 N4 C11 119.9(3) . . ? 
C6 N3 N4 105.2(3) . . ? 
C6 N3 Mg1 142.7(3) . . ? 
N4 N3 Mg1 111.9(2) . . ? 
C3 N1 N2 111.5(3) . . ? 
C3 N1 C11 129.1(3) . . ? 
N2 N1 C11 119.4(3) . . ? 
C1 N2 N1 105.3(3) . . ? 
C1 N2 Mg1 142.1(3) . . ? 
N1 N2 Mg1 112.3(2) . . ? 
N5 C12 N6 125.8(3) . . ? 
N5 C12 C11 121.4(3) . . ? 
N6 C12 C11 112.8(3) . . ? 
C12 N6 C18 119.4(3) . . ? 
C12 N6 Mg1 119.1(3) . . ? 
C18 N6 Mg1 121.5(2) . . ? 
C12 N5 C14 123.9(3) . . ? 
N1 C11 N4 110.7(3) . . ? 
N1 C11 C12 113.8(3) . . ? 
N4 C11 C12 113.7(3) . . ? 
C8 C7 C6 107.6(4) . . ? 
N6 C18 C24 113.4(3) . . ? 
N6 C18 C19 105.7(3) . . ? 
C24 C18 C19 107.9(3) . . ? 
N6 C18 C25 111.3(3) . . ? 
C24 C18 C25 109.9(3) . . ? 
C19 C18 C25 108.4(3) . . ? 
N1 C3 C2 106.3(3) . . ? 
N1 C3 C5 123.0(4) . . ? 
C2 C3 C5 130.7(4) . . ? 
N5 C14 C15 111.5(3) . . ? 
N3 C6 C7 109.9(3) . . ? 
N3 C6 C9 120.2(4) . . ? 
C7 C6 C9 129.9(4) . . ? 
C3 C2 C1 107.0(3) . . ? 
N2 C1 C2 109.9(3) . . ? 
N2 C1 C4 120.3(4) . . ? 
C2 C1 C4 129.8(4) . . ? 
C21 C20 Mg1 115.4(3) . . ? 
C22 C21 C20 128.5(4) . . ? 
N4 C8 C7 105.7(3) . . ? 
N4 C8 C10 123.5(4) . . ? 
C7 C8 C10 130.8(4) . . ? 
 
_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              19.07 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    0.423 
_refine_diff_density_min   -0.412 
_refine_diff_density_rms    0.042 


#=======================================================================_eof

# End of Crystallographic Information File
