#------------------------------------------------------------------------------
#$Date: 2019-11-25 22:12:50 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241938 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/17/4131786.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_4131786
loop_
_publ_author_name
'Rauch, Michael'
'Parkin, Gerard'
_publ_section_title
;
 Zinc and Magnesium Catalysts for the Hydrosilylation of Carbon Dioxide.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18162
_journal_page_last               18165
_journal_paper_doi               10.1021/jacs.7b10776
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C44 H58 Mg N6 O2 Si3'
_chemical_formula_weight         811.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.6699(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4147(4)
_cell_length_b                   18.9452(8)
_cell_length_c                   12.4092(5)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.45
_cell_volume                     2175.08(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36173
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.637
_diffrn_reflns_theta_min         1.670
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6775
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       plate
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         6878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0452P)²+0.9190P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5497
_reflns_number_total             6878
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b10776_si_006.cif
_cod_data_source_block           mgocohs10
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4131786
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.992
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Mg Mg 0.59350(6) 0.2500 0.20152(5) 0.01290(12) Uani 1 2 d S T P
O1 O 0.54680(14) 0.2500 0.36671(11) 0.0223(3) Uani 1 2 d S T P
O2 O 0.37210(14) 0.2500 0.22086(11) 0.0211(3) Uani 1 2 d S T P
Si1 Si 0.89296(3) 0.33303(2) 0.30189(3) 0.01458(8) Uani 1 1 d . . .
Si2 Si 0.87395(5) 0.2500 0.08426(4) 0.01319(10) Uani 1 2 d S T P
N11 N 0.61179(10) 0.36497(5) 0.19836(8) 0.01449(19) Uani 1 1 d . . .
N12 N 0.73143(11) 0.46691(5) 0.22903(9) 0.0162(2) Uani 1 1 d . . .
N21 N 0.56708(15) 0.2500 0.02689(12) 0.0138(3) Uani 1 2 d S T P
N22 N 0.65771(15) 0.2500 -0.12702(12) 0.0149(3) Uani 1 2 d S T P
C1 C 0.85023(17) 0.2500 0.22775(13) 0.0132(3) Uani 1 2 d S T P
C2 C 0.4160(2) 0.2500 0.32305(17) 0.0220(4) Uani 1 2 d S T P
H1 H 0.343(3) 0.2500 0.372(2) 0.029(6) Uiso 1 2 d S . P
C101 C 1.07531(14) 0.37370(8) 0.29937(12) 0.0245(3) Uani 1 1 d . . .
H10H H 1.1076 0.4002 0.3673 0.037 Uiso 1 1 calc R U .
H10I H 1.0677 0.4057 0.2365 0.037 Uiso 1 1 calc R U .
H10J H 1.1453 0.3363 0.2930 0.037 Uiso 1 1 calc R U .
C102 C 0.87694(15) 0.33444(7) 0.45046(10) 0.0219(3) Uani 1 1 d . . .
H10A H 0.9597 0.3098 0.4939 0.033 Uiso 1 1 calc R U .
H10B H 0.7872 0.3109 0.4595 0.033 Uiso 1 1 calc R U .
H10C H 0.8756 0.3834 0.4755 0.033 Uiso 1 1 calc R U .
C103 C 0.73917(13) 0.39472(6) 0.23848(10) 0.0149(2) Uani 1 1 d . . .
C104 C 0.51757(13) 0.41973(6) 0.16161(10) 0.0146(2) Uani 1 1 d . . .
C105 C 0.37026(13) 0.41763(7) 0.11500(10) 0.0186(2) Uani 1 1 d . . .
H10E H 0.3188 0.3743 0.1052 0.022 Uiso 1 1 calc R U .
C106 C 0.30256(15) 0.48116(8) 0.08374(11) 0.0233(3) Uani 1 1 d . . .
H10D H 0.2023 0.4815 0.0530 0.028 Uiso 1 1 calc R U .
C107 C 0.37872(16) 0.54504(7) 0.09641(11) 0.0245(3) Uani 1 1 d . . .
H10F H 0.3297 0.5874 0.0712 0.029 Uiso 1 1 calc R U .
C108 C 0.52342(15) 0.54819(7) 0.14468(11) 0.0215(3) Uani 1 1 d . . .
H10G H 0.5743 0.5917 0.1543 0.026 Uiso 1 1 calc R U .
C109 C 0.59108(13) 0.48416(6) 0.17862(10) 0.0163(2) Uani 1 1 d . . .
C110 C 0.84554(14) 0.51621(7) 0.27978(11) 0.0210(3) Uani 1 1 d . . .
H11A H 0.9268 0.4871 0.3204 0.025 Uiso 1 1 calc R U .
C111 C 0.79167(18) 0.56289(8) 0.36382(12) 0.0295(3) Uani 1 1 d . . .
H11B H 0.7527 0.5332 0.4161 0.044 Uiso 1 1 calc R U .
H11C H 0.7157 0.5943 0.3263 0.044 Uiso 1 1 calc R U .
H11D H 0.8720 0.5911 0.4031 0.044 Uiso 1 1 calc R U .
C112 C 0.90505(17) 0.55792(8) 0.19316(13) 0.0308(3) Uani 1 1 d . . .
H11E H 0.9437 0.5252 0.1446 0.046 Uiso 1 1 calc R U .
H11F H 0.9823 0.5893 0.2290 0.046 Uiso 1 1 calc R U .
H11G H 0.8274 0.5861 0.1501 0.046 Uiso 1 1 calc R U .
C201 C 0.96670(14) 0.33042(8) 0.04096(11) 0.0228(3) Uani 1 1 d . . .
H20E H 0.9625 0.3292 -0.0385 0.034 Uiso 1 1 calc R U .
H20F H 1.0679 0.3309 0.0785 0.034 Uiso 1 1 calc R U .
H20G H 0.9180 0.3730 0.0603 0.034 Uiso 1 1 calc R U .
C202 C 0.68887(17) 0.2500 -0.01372(14) 0.0138(3) Uani 1 2 d S T P
C203 C 0.45353(17) 0.2500 -0.06187(14) 0.0141(3) Uani 1 2 d S T P
C204 C 0.30433(18) 0.2500 -0.06367(15) 0.0182(3) Uani 1 2 d S T P
H20C H 0.2665 0.2500 0.0022 0.022 Uiso 1 2 calc R U P
C205 C 0.2144(2) 0.2500 -0.16519(17) 0.0229(4) Uani 1 2 d S T P
H20H H 0.1127 0.2500 -0.1691 0.027 Uiso 1 2 calc R U P
C206 C 0.2699(2) 0.2500 -0.26260(16) 0.0240(4) Uani 1 2 d S T P
H20D H 0.2045 0.2500 -0.3308 0.029 Uiso 1 2 calc R U P
C207 C 0.4169(2) 0.2500 -0.26218(15) 0.0206(4) Uani 1 2 d S T P
H20B H 0.4539 0.2500 -0.3284 0.025 Uiso 1 2 calc R U P
C208 C 0.50867(18) 0.2500 -0.15946(14) 0.0154(3) Uani 1 2 d S T P
C209 C 0.76427(19) 0.2500 -0.20065(14) 0.0181(3) Uani 1 2 d S T P
H20A H 0.8625 0.2500 -0.1532 0.022 Uiso 1 2 calc R U P
C210 C 0.75219(16) 0.31673(8) -0.26976(12) 0.0275(3) Uani 1 1 d . . .
H21A H 0.7649 0.3581 -0.2216 0.041 Uiso 1 1 calc R U .
H21B H 0.6567 0.3186 -0.3173 0.041 Uiso 1 1 calc R U .
H21C H 0.8272 0.3165 -0.3150 0.041 Uiso 1 1 calc R U .
C300 C 0.3959(2) 0.52309(12) 0.41565(16) 0.0490(5) Uani 1 1 d . . .
H30C H 0.3232 0.5392 0.3573 0.059 Uiso 1 1 calc R U .
C301 C 0.4431(2) 0.45479(11) 0.41687(14) 0.0430(4) Uani 1 1 d . . .
H30A H 0.4041 0.4235 0.3592 0.052 Uiso 1 1 calc R U .
C302 C 0.5471(2) 0.43182(10) 0.50190(19) 0.0465(5) Uani 1 1 d . . .
H30B H 0.5797 0.3843 0.5034 0.056 Uiso 1 1 calc R U .
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'
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
N21 Mg O2 100.42(6) . .
N21 Mg O1 161.97(6) . .
O2 Mg O1 61.55(5) . .
N21 Mg N11 88.66(3) . 4_565
O2 Mg N11 94.79(3) . 4_565
O1 Mg N11 92.71(3) . 4_565
N21 Mg N11 88.66(3) . .
O2 Mg N11 94.79(3) . .
O1 Mg N11 92.71(3) . .
N11 Mg N11 170.36(6) 4_565 .
N21 Mg C1 93.63(6) . .
O2 Mg C1 165.95(6) . .
O1 Mg C1 104.40(6) . .
N11 Mg C1 85.47(3) 4_565 .
N11 Mg C1 85.47(3) . .
N21 Mg C2 131.32(7) . .
O2 Mg C2 30.90(6) . .
O1 Mg C2 30.65(6) . .
N11 Mg C2 94.36(3) 4_565 .
N11 Mg C2 94.36(3) . .
C1 Mg C2 135.05(7) . .
N21 Mg Si2 59.73(4) . .
O2 Mg Si2 160.15(5) . .
O1 Mg Si2 138.30(4) . .
N11 Mg Si2 85.33(3) 4_565 .
N11 Mg Si2 85.33(3) . .
C1 Mg Si2 33.90(4) . .
C2 Mg Si2 168.95(5) . .
N21 Mg Si1 108.48(4) . 4_565
O2 Mg Si1 138.27(3) . 4_565
O1 Mg Si1 87.22(4) . 4_565
N11 Mg Si1 57.44(3) 4_565 4_565
N11 Mg Si1 114.92(3) . 4_565
C1 Mg Si1 33.33(2) . 4_565
C2 Mg Si1 113.85(4) . 4_565
Si2 Mg Si1 56.913(13) . 4_565
N21 Mg Si1 108.49(4) . .
O2 Mg Si1 138.27(3) . .
O1 Mg Si1 87.22(4) . .
N11 Mg Si1 114.92(3) 4_565 .
N11 Mg Si1 57.44(3) . .
C1 Mg Si1 33.33(2) . .
C2 Mg Si1 113.85(4) . .
Si2 Mg Si1 56.913(13) . .
Si1 Mg Si1 57.562(15) 4_565 .
C2 O1 Mg 86.93(11) . .
C2 O2 Mg 88.18(11) . .
C1 Si1 C102 117.13(7) . .
C1 Si1 C101 117.31(7) . .
C102 Si1 C101 104.43(6) . .
C1 Si1 C103 103.85(6) . .
C102 Si1 C103 101.71(6) . .
C101 Si1 C103 111.42(6) . .
C1 Si1 Mg 45.60(5) . .
C102 Si1 Mg 99.25(4) . .
C101 Si1 Mg 156.02(5) . .
C103 Si1 Mg 66.63(4) . .
C1 Si2 C201 115.03(5) . 4_565
C1 Si2 C201 115.03(5) . .
C201 Si2 C201 108.00(9) 4_565 .
C1 Si2 C202 110.68(7) . .
C201 Si2 C202 103.43(5) 4_565 .
C201 Si2 C202 103.43(5) . .
C1 Si2 Mg 46.29(5) . .
C201 Si2 Mg 125.96(5) 4_565 .
C201 Si2 Mg 125.96(5) . .
C202 Si2 Mg 64.39(5) . .
C103 N11 C104 106.42(10) . .
C103 N11 Mg 118.84(8) . .
C104 N11 Mg 134.75(8) . .
C103 N12 C109 107.64(10) . .
C103 N12 C110 124.86(11) . .
C109 N12 C110 126.83(10) . .
C202 N21 C203 106.87(14) . .
C202 N21 Mg 115.87(11) . .
C203 N21 Mg 137.27(11) . .
C202 N22 C208 107.95(14) . .
C202 N22 C209 126.08(14) . .
C208 N22 C209 125.97(14) . .
Si1 C1 Si1 118.63(9) 4_565 .
Si1 C1 Si2 115.67(5) 4_565 .
Si1 C1 Si2 115.67(5) . .
Si1 C1 Mg 101.08(5) 4_565 .
Si1 C1 Mg 101.08(5) . .
Si2 C1 Mg 99.81(7) . .
O1 C2 O2 123.34(17) . .
O1 C2 Mg 62.43(10) . .
O2 C2 Mg 60.91(9) . .
N11 C103 N12 111.02(10) . .
N11 C103 Si1 117.04(9) . .
N12 C103 Si1 131.89(9) . .
N11 C104 C109 109.55(10) . .
N11 C104 C105 129.71(11) . .
C109 C104 C105 120.73(11) . .
C106 C105 C104 117.42(12) . .
C105 C106 C107 121.37(12) . .
C108 C107 C106 121.88(12) . .
C107 C108 C109 116.74(12) . .
N12 C109 C108 132.88(12) . .
N12 C109 C104 105.35(10) . .
C108 C109 C104 121.74(12) . .
N12 C110 C112 111.21(11) . .
N12 C110 C111 110.58(11) . .
C112 C110 C111 113.24(12) . .
N21 C202 N22 110.40(14) . .
N21 C202 Si2 120.01(12) . .
N22 C202 Si2 129.59(12) . .
N21 C203 C204 129.53(16) . .
N21 C203 C208 109.37(14) . .
C204 C203 C208 121.09(16) . .
C205 C204 C203 117.25(17) . .
C204 C205 C206 121.52(17) . .
C207 C206 C205 121.91(17) . .
C206 C207 C208 116.83(17) . .
N22 C208 C207 133.20(16) . .
N22 C208 C203 105.41(14) . .
C207 C208 C203 121.39(16) . .
N22 C209 C210 111.14(10) . 4_565
N22 C209 C210 111.14(10) . .
C210 C209 C210 112.54(16) 4_565 .
C302 C300 C301 120.14(17) 3_666 .
C300 C301 C302 119.57(17) . .
C300 C302 C301 120.28(17) 3_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg N21 2.1351(15) .
Mg O2 2.1418(14) .
Mg O1 2.1746(14) .
Mg N11 2.1858(10) 4_565
Mg N11 2.1858(10) .
Mg C1 2.3785(17) .
Mg C2 2.4497(19) .
Mg Si2 3.2422(7) .
Mg Si1 3.2671(6) 4_565
Mg Si1 3.2671(6) .
O1 C2 1.250(2) .
O2 C2 1.259(2) .
Si1 C1 1.8291(9) .
Si1 C102 1.8776(13) .
Si1 C101 1.8873(13) .
Si1 C103 1.9130(12) .
Si2 C1 1.8350(17) .
Si2 C201 1.8831(13) 4_565
Si2 C201 1.8831(13) .
Si2 C202 1.9314(17) .
N11 C103 1.3352(15) .
N11 C104 1.3862(15) .
N12 C103 1.3735(15) .
N12 C109 1.3921(16) .
N12 C110 1.4739(16) .
N21 C202 1.335(2) .
N21 C203 1.386(2) .
N22 C202 1.382(2) .
N22 C208 1.386(2) .
N22 C209 1.477(2) .
C1 Si1 1.8291(9) 4_565
C104 C109 1.3997(17) .
C104 C105 1.4009(17) .
C105 C106 1.3834(18) .
C106 C107 1.401(2) .
C107 C108 1.384(2) .
C108 C109 1.3983(17) .
C110 C112 1.5221(19) .
C110 C111 1.524(2) .
C203 C204 1.401(2) .
C203 C208 1.403(2) .
C204 C205 1.382(3) .
C205 C206 1.403(3) .
C206 C207 1.384(3) .
C207 C208 1.401(2) .
C209 C210 1.5200(17) 4_565
C209 C210 1.5201(17) .
C300 C302 1.364(3) 3_666
C300 C301 1.367(3) .
C301 C302 1.371(3) .
C302 C300 1.364(3) 3_666
