Isocyanate deoxygenation by a molecular magnesium silanide.
Okokhere-Edeghoghon, Bibian; Neale, Samuel E.; Hill, Michael S.; Mahon, Mary F.; McMullin, Claire L.; Dalton transactions (Cambridge, England : 2003) 51 (2021) 136–144; doi:10.1039/d1dt03775g

data_7708959
_publ_section_title
;
 Isocyanate deoxygenation by a molecular magnesium silanide.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              136
_journal_page_last               144
_journal_paper_doi               10.1039/d1dt03775g
_journal_volume                  51
_journal_year                    2021
_chemical_formula_moiety         'C135 H198 Mg3 N12 O6 Si3'
_chemical_formula_sum            'C153 H240 Mg3 N12 O6 Si3'
_chemical_formula_weight         2500.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-02 deposited with the CCDC.	2021-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                61.681(2)
_cell_angle_beta                 85.617(2)
_cell_angle_gamma                86.756(2)
_cell_formula_units_Z            2
_cell_length_a                   16.2685(3)
_cell_length_b                   24.0536(4)
_cell_length_c                   24.3670(5)
_cell_measurement_reflns_used    17150
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.1630
_cell_measurement_theta_min      4.1340
_cell_volume                     8367.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            60767
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.972
_diffrn_reflns_theta_min         3.682
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.993
_exptl_crystal_description       block
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.183
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1741
_refine_ls_number_reflns         32598
_refine_ls_number_restraints     493
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0490
_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/[\s^2^(Fo^2^)+(0.0660P)^2^+0.1283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23665
_reflns_number_total             32598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03775g2.cif
_cod_data_source_block           s21msh42-cpd-14
_cod_depositor_comments
'Adding full bibliography for 7708958--7708960.cif.'
_cod_database_code               7708959
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si2-C49 \\sim Si2-C49A
 with sigma of 0.02
 C49-C54 \\sim C49A-C54A
 with sigma of 0.02
 C49-C50 \\sim C49A-C50A
 with sigma of 0.02
 C54-C53 \\sim C54A-C53A
 with sigma of 0.02
 C53-C52 \\sim C53A-C52A
 with sigma of 0.02
 C52-C51 \\sim C52A-C51A
 with sigma of 0.02
 C51-C50 \\sim C51A-C50A
 with sigma of 0.02
 Si2-C54 \\sim Si2-C54A
 with sigma of 0.04
 Si2-C50 \\sim Si2-C50A
 with sigma of 0.04
 C49-C53 \\sim C49A-C53A
 with sigma of 0.04
 C49-C51 \\sim C49A-C51A
 with sigma of 0.04
 C54-C52 \\sim C54A-C52A
 with sigma of 0.04
 C54-C50 \\sim C54A-C50A
 with sigma of 0.04
 C53-C51 \\sim C53A-C51A
 with sigma of 0.04
 C52-C50 \\sim C52A-C50A
 with sigma of 0.04
 Si1-C40 \\sim Si1-C40A
 with sigma of 0.02
 C40-C41 \\sim C40A-C41A
 with sigma of 0.02
 C40-C45 \\sim C40A-C45A
 with sigma of 0.02
 C41-C42 \\sim C41A-C42A
 with sigma of 0.02
 C44-C43 \\sim C44A-C43A
 with sigma of 0.02
 C44-C45 \\sim C44A-C45A
 with sigma of 0.02
 C43-C42 \\sim C43A-C42A
 with sigma of 0.02
 Si1-C41 \\sim Si1-C41A
 with sigma of 0.04
 Si1-C45 \\sim Si1-C45A
 with sigma of 0.04
 C40-C44 \\sim C40A-C44A
 with sigma of 0.04
 C40-C42 \\sim C40A-C42A
 with sigma of 0.04
 C41-C43 \\sim C41A-C43A
 with sigma of 0.04
 C41-C45 \\sim C41A-C45A
 with sigma of 0.04
 C44-C42 \\sim C44A-C42A
 with sigma of 0.04
 C43-C45 \\sim C43A-C45A
 with sigma of 0.04
 N8-C91 \\sim N8-C91A
 with sigma of 0.02
 C91-C92 \\sim C91A-C92A
 with sigma of 0.02
 C91-C96 \\sim C91A-C96A
 with sigma of 0.02
 C92-C100 \\sim C92A-C1A
 with sigma of 0.02
 C92-C93 \\sim C92A-C93A
 with sigma of 0.02
 C100-C102 \\sim C1A-C1B
 with sigma of 0.02
 C100-C101 \\sim C1A-C1C
 with sigma of 0.02
 C93-C94 \\sim C93A-C94A
 with sigma of 0.02
 C96-C97 \\sim C96A-C97A
 with sigma of 0.02
 C96-C95 \\sim C96A-C95A
 with sigma of 0.02
 C94-C95 \\sim C94A-C95A
 with sigma of 0.02
 C97-C99 \\sim C97A-C99A
 with sigma of 0.02
 C97-C98 \\sim C97A-C98A
 with sigma of 0.02
 N8-C92 \\sim N8-C92A
 with sigma of 0.04
 N8-C96 \\sim N8-C96A
 with sigma of 0.04
 C91-C100 \\sim C91A-C1A
 with sigma of 0.04
 C91-C93 \\sim C91A-C93A
 with sigma of 0.04
 C91-C97 \\sim C91A-C97A
 with sigma of 0.04
 C91-C95 \\sim C91A-C95A
 with sigma of 0.04
 C92-C96 \\sim C92A-C96A
 with sigma of 0.04
 C92-C94 \\sim C92A-C94A
 with sigma of 0.04
 C92-C102 \\sim C92A-C1B
 with sigma of 0.04
 C92-C101 \\sim C92A-C1C
 with sigma of 0.04
 C100-C93 \\sim C1A-C93A
 with sigma of 0.04
 C93-C95 \\sim C93A-C95A
 with sigma of 0.04
 C96-C94 \\sim C96A-C94A
 with sigma of 0.04
 C96-C99 \\sim C96A-C99A
 with sigma of 0.04
 C96-C98 \\sim C96A-C98A
 with sigma of 0.04
 C102-C101 \\sim C1B-C1C
 with sigma of 0.04
 C97-C95 \\sim C97A-C95A
 with sigma of 0.04
 C99-C98 \\sim C99A-C98A
 with sigma of 0.04
 C62-C63 \\sim C62A-C63A
 with sigma of 0.02
 C63-C64 \\sim C63A-C64A
 with sigma of 0.02
 C64-C65 \\sim C64A-C65A
 with sigma of 0.02
 C66-C65 \\sim C66A-C65A
 with sigma of 0.02
 Si3-C62 \\sim Si3-C62A
 with sigma of 0.04
 Si3-C66 \\sim Si3-C66A
 with sigma of 0.04
 C62-C64 \\sim C62A-C64A
 with sigma of 0.04
 C62-C66 \\sim C62A-C66A
 with sigma of 0.04
 C63-C65 \\sim C63A-C65A
 with sigma of 0.04
 C64-C66 \\sim C64A-C66A
 with sigma of 0.04
 C130-C132 \\sim C130-C1E
 with sigma of 0.02
 C130-C131 \\sim C130-C1D
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C49 \\sim C54: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
C49A \\sim C50A \\sim C51A \\sim C52A \\sim C53A \\sim C54A: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.01
C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.01
C40A \\sim C41A \\sim C42A \\sim C43A \\sim C44A \\sim C45A: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.01
C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97 \\sim C98 \\sim
C99 \\sim C100 \\sim C101 \\sim C102: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.01
C131 \\sim C132 \\sim C1D \\sim C1E: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.01
C62A \\sim C62 \\sim C61 \\sim C66A \\sim C65A \\sim C65 \\sim C63 \\sim C63A
\\sim C64A \\sim C64 \\sim C66: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.01
C1B \\sim C1A \\sim C1C \\sim C92A \\sim C93A \\sim C94A \\sim C91A \\sim C96A
\\sim C95A \\sim C97A \\sim C99A \\sim C98A: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: H130(0.65) H13D(0.35) C40(0.58) C41(0.58) H41(0.58) C42(0.58)
 H42(0.58) C43(0.58) H43(0.58) C44(0.58) H44(0.58) C45(0.58) H45(0.58)
 C49(0.58) C54(0.58) H54(0.58) C53(0.58) H53(0.58) C52(0.58) H52(0.58)
 C51(0.58) H51(0.58) C50(0.58) H50(0.58) C62(0.55) H62(0.55) C63(0.55)
 H63(0.55) C64(0.55) H64(0.55) C65(0.55) H65(0.55) C66(0.55) H66(0.55)
 C91(0.58) C92(0.58) C93(0.58) H93(0.58) C94(0.58) H94(0.58) C95(0.58)
 H95(0.58) C96(0.58) C97(0.58) H97(0.58) C98(0.58) H98A(0.58) H98B(0.58)
 H98C(0.58) C99(0.58) H99A(0.58) H99B(0.58) H99C(0.58) C100(0.58) H100(0.58)
 C101(0.58) H10J(0.58) H10K(0.58) H10L(0.58) C102(0.58) H10M(0.58) H10N(0.58)
 H10O(0.58) C131(0.65) H13K(0.65) H13L(0.65) H13M(0.65) C132(0.65) H13N(0.65)
 H13O(0.65) H13P(0.65) C1A(0.42) H1AA(0.42) C1B(0.42) H1BA(0.42) H1BB(0.42)
 H1BC(0.42) C1C(0.42) H1CA(0.42) H1CB(0.42) H1CC(0.42) C1D(0.35) H1DA(0.35)
 H1DB(0.35) H1DC(0.35) C1E(0.35) H1EA(0.35) H1EB(0.35) H1EC(0.35) C40A(0.42)
 C41A(0.42) H41A(0.42) C42A(0.42) H42A(0.42) C43A(0.42) H43A(0.42) C44A(0.42)
 H44A(0.42) C45A(0.42) H45A(0.42) C49A(0.42) C50A(0.42) H50A(0.42) C51A(0.42)
 H51A(0.42) C52A(0.42) H52A(0.42) C53A(0.42) H53A(0.42) C54A(0.42) H54A(0.42)
 C62A(0.45) H62A(0.45) C63A(0.45) H63A(0.45) C64A(0.45) H64A(0.45) C65A(0.45)
 H65A(0.45) C66A(0.45) H66A(0.45) C91A(0.42) C92A(0.42) C93A(0.42) H93A(0.42)
 C94A(0.42) H94A(0.42) C95A(0.42) H95A(0.42) C96A(0.42) C97A(0.42) H97A(0.42)
 C98A(0.42) H98D(0.42) H98E(0.42) H98F(0.42) C99A(0.42) H99D(0.42) H99E(0.42)
 H99F(0.42)
5.a Ternary CH refined with riding coordinates:
 C3(H3), C12(H12), C15(H15), C24(H24), C27(H27), C31(H31), C35(H35), C55(H55),
 C67(H67), C71(H71), C76(H76), C85(H85), C88(H88), C104(H104), C109(H109),
 C118(H118), C121(H121), C130(H130), C130(H13D), C133(H133), C97(H97),
 C100(H100), C1A(H1AA), C97A(H97A)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C81(H81), C82(H82),
 C83(H83), C114(H114), C115(H115), C116(H116), C126(H126), C127(H127),
 C128(H128), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C54(H54),
 C53(H53), C52(H52), C51(H51), C50(H50), C62(H62), C63(H63), C64(H64), C65(H65),
  C66(H66), C93(H93), C94(H94), C95(H95), C41A(H41A), C42A(H42A), C43A(H43A),
 C44A(H44A), C45A(H45A), C50A(H50A), C51A(H51A), C52A(H52A), C53A(H53A),
 C54A(H54A), C62A(H62A), C63A(H63A), C64A(H64A), C65A(H65A), C66A(H66A),
 C93A(H93A), C94A(H94A), C95A(H95A)
5.c Fitted hexagon refined as free rotating group:
 C49(C54,C53,C52,C51,C50), C91A(C92A,C93A,C94A,C95A,C96A)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C39(H39A,H39B,H39C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C68(H68A,
 H68B,H68C), C69(H69A,H69B,H69C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C),
 C74(H74A,H74B,H74C), C78(H78A,H78B,H78C), C86(H86A,H86B,H86C), C87(H87A,H87B,
 H87C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C105(H10A,H10B,H10C),
 C106(H10D,H10E,H10F), C107(H10G,H10H,H10I), C111(H11A,H11B,H11C), C119(H11D,
 H11E,H11F), C120(H12A,H12B,H12C), C122(H12D,H12E,H12F), C123(H12G,H12H,H12I),
 C134(H13E,H13F,H13G), C135(H13H,H13I,H13J), C98(H98A,H98B,H98C), C99(H99A,H99B,
 H99C), C101(H10J,H10K,H10L), C102(H10M,H10N,H10O), C131(H13K,H13L,H13M),
 C132(H13N,H13O,H13P), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1D(H1DA,H1DB,
 H1DC), C1E(H1EA,H1EB,H1EC), C98A(H98D,H98E,H98F), C99A(H99D,H99E,H99F)
;