#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:20:33 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178646 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/57/4075717.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4075717
loop_
_publ_author_name
'Tang, Yongjun'
'Zakharov, Lev N.'
'Rheingold, Arnold L.'
'Kemp, Richard A.'
_publ_section_title
;
 Synthesis and Structural Characterization of Magnesium Amide Complexes
 Containing −N[(R)(SiMe3)] Ligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              836
_journal_paper_doi               10.1021/om049203c
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C23 H53 Mg N3 Si4'
_chemical_formula_weight         508.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.5780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5908(6)
_cell_length_b                   22.8478(11)
_cell_length_c                   11.3638(5)
_cell_measurement_reflns_used    7274
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.31
_cell_volume                     3133.2(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9741
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.139
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0453P)²+1.5532P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                3279
_reflns_number_total             3558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049203csi20041216_122428.cif
_cod_data_source_block           Compound_9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4075717
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'
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
Mg1 Mg 0.0000 0.32322(2) 0.7500 0.01498(13) Uani 1 2 d S
Si1 Si 0.06882(3) 0.349246(13) 0.50197(3) 0.01469(9) Uani 1 1 d .
N1 N 0.10465(8) 0.34985(4) 0.65862(9) 0.01430(19) Uani 1 1 d .
C1 C 0.07956(10) 0.19941(5) 0.71957(12) 0.0225(3) Uani 1 1 d .
H1 H 0.1360(12) 0.2212(6) 0.7016(14) 0.025(4) Uiso 1 1 d .
Si2 Si 0.23115(2) 0.365141(13) 0.75792(3) 0.01414(9) Uani 1 1 d .
N2 N 0.0000 0.22993(6) 0.7500 0.0192(3) Uani 1 2 d S
C2 C 0.08274(12) 0.13899(6) 0.71917(14) 0.0275(3) Uani 1 1 d .
H2 H 0.1400(13) 0.1203(7) 0.7007(14) 0.028(4) Uiso 1 1 d .
C3 C 0.0000 0.10826(8) 0.7500 0.0287(4) Uani 1 2 d S
H3 H 0.0000 0.0663(11) 0.7500 0.044(7) Uiso 1 2 d S
C4 C -0.01699(11) 0.41416(6) 0.43143(11) 0.0216(2) Uani 1 1 d .
H4C H -0.0366(15) 0.4126(8) 0.3416(17) 0.045(5) Uiso 1 1 d .
H4B H 0.0194(15) 0.4491(8) 0.4580(17) 0.045(5) Uiso 1 1 d .
H4A H -0.0840(16) 0.4149(8) 0.4497(17) 0.048(5) Uiso 1 1 d .
C5 C -0.01375(11) 0.28219(6) 0.43896(12) 0.0236(3) Uani 1 1 d .
H5C H 0.0306(15) 0.2467(8) 0.4596(17) 0.047(5) Uiso 1 1 d .
H5B H -0.0382(14) 0.2847(8) 0.3554(18) 0.044(5) Uiso 1 1 d .
H5A H -0.0762(15) 0.2768(8) 0.4661(17) 0.042(5) Uiso 1 1 d .
C6 C 0.18841(11) 0.34731(6) 0.43354(12) 0.0214(3) Uani 1 1 d .
H6C H 0.2355(15) 0.3812(8) 0.4538(16) 0.040(5) Uiso 1 1 d .
H6B H 0.1600(14) 0.3479(7) 0.3442(17) 0.035(4) Uiso 1 1 d .
H6A H 0.2313(14) 0.3123(8) 0.4562(16) 0.039(5) Uiso 1 1 d .
C7 C 0.35021(10) 0.32890(6) 0.71952(12) 0.0231(3) Uani 1 1 d .
H7C H 0.3682(15) 0.3471(7) 0.6576(18) 0.040(5) Uiso 1 1 d .
H7B H 0.4155(15) 0.3294(7) 0.7903(16) 0.035(4) Uiso 1 1 d .
H7A H 0.3300(15) 0.2883(8) 0.6975(17) 0.045(5) Uiso 1 1 d .
C8 C 0.23051(11) 0.33436(6) 0.91194(11) 0.0219(3) Uani 1 1 d .
H8C H 0.2993(16) 0.3407(7) 0.9719(18) 0.042(5) Uiso 1 1 d .
H8B H 0.2190(13) 0.2930(7) 0.9065(14) 0.031(4) Uiso 1 1 d .
H8A H 0.1767(15) 0.3523(7) 0.9460(16) 0.034(4) Uiso 1 1 d .
C9 C 0.26496(9) 0.44647(5) 0.78121(10) 0.0178(2) Uani 1 1 d .
C10 C 0.17108(12) 0.47791(6) 0.81653(13) 0.0258(3) Uani 1 1 d .
H10C H 0.1015(14) 0.4724(7) 0.7522(15) 0.034(4) Uiso 1 1 d .
H10B H 0.1894(14) 0.5197(8) 0.8294(16) 0.040(5) Uiso 1 1 d .
H10A H 0.1619(14) 0.4628(7) 0.8915(16) 0.039(4) Uiso 1 1 d .
C11 C 0.27637(12) 0.47410(6) 0.66244(12) 0.0246(3) Uani 1 1 d .
H11C H 0.3397(13) 0.4570(7) 0.6385(14) 0.030(4) Uiso 1 1 d .
H11B H 0.2895(12) 0.5174(7) 0.6732(14) 0.030(4) Uiso 1 1 d .
H11A H 0.2096(13) 0.4683(7) 0.5974(15) 0.031(4) Uiso 1 1 d .
C12 C 0.37357(12) 0.45606(7) 0.88270(14) 0.0322(3) Uani 1 1 d .
H12C H 0.4358(15) 0.4366(8) 0.8640(15) 0.040(5) Uiso 1 1 d .
H12B H 0.3911(14) 0.4974(8) 0.8937(16) 0.042(5) Uiso 1 1 d .
H12A H 0.3731(14) 0.4412(8) 0.9590(18) 0.042(5) Uiso 1 1 d .
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N1 Mg1 N1 144.41(6) 2_556 .
N1 Mg1 N2 107.79(3) 2_556 .
N1 Mg1 N2 107.79(3) . .
N1 Mg1 Si2 131.18(3) 2_556 .
N1 Mg1 Si2 31.69(3) . .
N2 Mg1 Si2 108.360(11) . .
N1 Mg1 Si2 31.69(3) 2_556 2_556
N1 Mg1 Si2 131.18(3) . 2_556
N2 Mg1 Si2 108.360(11) . 2_556
Si2 Mg1 Si2 143.28(2) . 2_556
N1 Mg1 Si1 141.31(3) 2_556 .
N1 Mg1 Si1 26.74(3) . .
N2 Mg1 Si1 100.604(10) . .
Si2 Mg1 Si1 58.352(8) . .
Si2 Mg1 Si1 114.128(11) 2_556 .
N1 Mg1 Si1 26.74(3) 2_556 2_556
N1 Mg1 Si1 141.31(3) . 2_556
N2 Mg1 Si1 100.604(10) . 2_556
Si2 Mg1 Si1 114.128(11) . 2_556
Si2 Mg1 Si1 58.352(8) 2_556 2_556
Si1 Mg1 Si1 158.79(2) . 2_556
N1 Si1 C4 112.83(5) . .
N1 Si1 C5 110.95(5) . .
C4 Si1 C5 107.10(6) . .
N1 Si1 C6 115.25(5) . .
C4 Si1 C6 105.86(6) . .
C5 Si1 C6 104.17(6) . .
N1 Si1 Mg1 31.66(3) . .
C4 Si1 Mg1 104.67(4) . .
C5 Si1 Mg1 85.72(4) . .
C6 Si1 Mg1 143.26(4) . .
Si2 N1 Si1 127.65(6) . .
Si2 N1 Mg1 110.46(5) . .
Si1 N1 Mg1 121.60(5) . .
N2 C1 C2 122.95(12) . .
N2 C1 H1 116.6(9) . .
C2 C1 H1 120.4(9) . .
N1 Si2 C7 114.49(5) . .
N1 Si2 C8 106.68(5) . .
C7 Si2 C8 105.49(6) . .
N1 Si2 C9 114.88(5) . .
C7 Si2 C9 107.56(6) . .
C8 Si2 C9 107.10(6) . .
N1 Si2 Mg1 37.85(3) . .
C7 Si2 Mg1 132.68(5) . .
C8 Si2 Mg1 69.70(4) . .
C9 Si2 Mg1 118.99(4) . .
C1 N2 C1 117.50(15) 2_556 .
C1 N2 Mg1 121.25(7) 2_556 .
C1 N2 Mg1 121.25(7) . .
C1 C2 C3 118.84(13) . .
C1 C2 H2 119.6(10) . .
C3 C2 H2 121.6(10) . .
C2 C3 C2 118.92(17) . 2_556
C2 C3 H3 120.54(9) . .
C2 C3 H3 120.54(8) 2_556 .
Si1 C4 H4C 111.0(11) . .
Si1 C4 H4B 111.7(11) . .
H4C C4 H4B 109.0(15) . .
Si1 C4 H4A 111.7(12) . .
H4C C4 H4A 105.1(15) . .
H4B C4 H4A 108.0(16) . .
Si1 C5 H5C 111.8(11) . .
Si1 C5 H5B 109.4(11) . .
H5C C5 H5B 107.6(15) . .
Si1 C5 H5A 114.2(11) . .
H5C C5 H5A 106.8(15) . .
H5B C5 H5A 106.6(15) . .
Si1 C6 H6C 113.1(11) . .
Si1 C6 H6B 109.3(10) . .
H6C C6 H6B 104.9(14) . .
Si1 C6 H6A 111.4(10) . .
H6C C6 H6A 110.2(15) . .
H6B C6 H6A 107.6(14) . .
Si2 C7 H7C 112.1(11) . .
Si2 C7 H7B 110.3(10) . .
H7C C7 H7B 107.4(15) . .
Si2 C7 H7A 108.2(11) . .
H7C C7 H7A 110.1(15) . .
H7B C7 H7A 108.7(14) . .
Si2 C8 H8C 111.4(11) . .
Si2 C8 H8B 110.4(10) . .
H8C C8 H8B 106.8(14) . .
Si2 C8 H8A 113.8(10) . .
H8C C8 H8A 104.5(14) . .
H8B C8 H8A 109.6(13) . .
C12 C9 C10 109.00(11) . .
C12 C9 C11 108.42(11) . .
C10 C9 C11 108.11(10) . .
C12 C9 Si2 111.07(9) . .
C10 C9 Si2 109.56(8) . .
C11 C9 Si2 110.61(8) . .
C9 C10 H10C 109.8(9) . .
C9 C10 H10B 109.2(10) . .
H10C C10 H10B 111.0(13) . .
C9 C10 H10A 111.3(10) . .
H10C C10 H10A 108.1(14) . .
H10B C10 H10A 107.4(14) . .
C9 C11 H11C 111.3(9) . .
C9 C11 H11B 110.6(9) . .
H11C C11 H11B 107.7(12) . .
C9 C11 H11A 109.9(9) . .
H11C C11 H11A 109.3(13) . .
H11B C11 H11A 108.0(13) . .
C9 C12 H12C 111.7(10) . .
C9 C12 H12B 110.9(10) . .
H12C C12 H12B 107.8(14) . .
C9 C12 H12A 114.0(11) . .
H12C C12 H12A 104.7(14) . .
H12B C12 H12A 107.3(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg1 N1 1.9914(9) 2_556
Mg1 N1 1.9914(9) .
Mg1 N2 2.1314(15) .
Mg1 Si2 3.0407(4) .
Mg1 Si2 3.0407(4) 2_556
Mg1 Si1 3.2314(3) .
Mg1 Si1 3.2314(3) 2_556
Si1 N1 1.7071(10) .
Si1 C4 1.8749(12) .
Si1 C5 1.8750(13) .
Si1 C6 1.8821(13) .
N1 Si2 1.7049(10) .
C1 N2 1.3443(14) .
C1 C2 1.3810(17) .
C1 H1 0.937(15) .
Si2 C7 1.8700(13) .
Si2 C8 1.8884(12) .
Si2 C9 1.9079(12) .
N2 C1 1.3443(14) 2_556
C2 C3 1.3818(16) .
C2 H2 0.912(16) .
C3 C2 1.3818(16) 2_556
C3 H3 0.96(3) .
C4 H4C 0.981(19) .
C4 H4B 0.927(19) .
C4 H4A 0.925(19) .
C5 H5C 0.975(19) .
C5 H5B 0.912(19) .
C5 H5A 0.931(19) .
C6 H6C 0.963(18) .
C6 H6B 0.976(18) .
C6 H6A 0.958(18) .
C7 H7C 0.900(19) .
C7 H7B 0.973(18) .
C7 H7A 0.975(19) .
C8 H8C 0.95(2) .
C8 H8B 0.955(16) .
C8 H8A 0.963(18) .
C9 C12 1.5324(17) .
C9 C10 1.5313(17) .
C9 C11 1.5334(17) .
C10 H10C 0.976(17) .
C10 H10B 0.984(18) .
C10 H10A 0.956(18) .
C11 H11C 0.993(16) .
C11 H11B 1.004(16) .
C11 H11A 0.957(16) .
C12 H12C 0.976(18) .
C12 H12B 0.970(18) .
C12 H12A 0.933(19) .
