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_7708960
_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         'C50 H69 Mg N3 O Si'
_chemical_formula_sum            'C51.8 H73.2 Mg N3 O Si'
_chemical_formula_weight         806.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-14
_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                90
_cell_angle_beta                 106.0960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.70880(10)
_cell_length_b                   17.60950(10)
_cell_length_c                   21.7081(2)
_cell_measurement_reflns_used    22503
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.9430
_cell_measurement_theta_min      3.2920
_cell_volume                     5035.01(7)
_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 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  0.0402
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66427
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.070
_diffrn_reflns_theta_min         3.285
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       block
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         10019
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0587P)^2^+1.4413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8625
_reflns_number_total             10019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03775g2.cif
_cod_data_source_block           s20msh59-cpd8
_cod_depositor_comments
'Adding full bibliography for 7708958--7708960.cif.'
_cod_original_formula_sum        'C51.80 H73.20 Mg N3 O Si'
_cod_database_code               7708960
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si1-C45 \\sim Si1-C45A
 with sigma of 0.02
 C45-C46 \\sim C45A-C46A
 with sigma of 0.02
 C45-C50 \\sim C45A-C50A
 with sigma of 0.02
 C46-C47 \\sim C46A-C47A
 with sigma of 0.02
 C47-C48 \\sim C47A-C48A
 with sigma of 0.02
 C48-C49 \\sim C48A-C49A
 with sigma of 0.02
 C49-C50 \\sim C49A-C50A
 with sigma of 0.02
 Si1-C46 \\sim Si1-C46A
 with sigma of 0.04
 Si1-C50 \\sim Si1-C50A
 with sigma of 0.04
 C45-C47 \\sim C45A-C47A
 with sigma of 0.04
 C45-C49 \\sim C45A-C49A
 with sigma of 0.04
 C46-C48 \\sim C46A-C48A
 with sigma of 0.04
 C46-C50 \\sim C46A-C50A
 with sigma of 0.04
 C47-C49 \\sim C47A-C49A
 with sigma of 0.04
 C48-C50 \\sim C48A-C50A
 with sigma of 0.04
 Si1-C45A \\sim Si1-C45
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C45A \\sim C46A \\sim C47A \\sim C48A \\sim C49A \\sim C50A: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.01
C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C45(0.6) C46(0.6) H46(0.6) C47(0.6) H47(0.6) C48(0.6) H48(0.6)
 C49(0.6) H49(0.6) C50(0.6) H50(0.6) C45A(0.4) C46A(0.4) H46A(0.4) C47A(0.4)
 H47A(0.4) C48A(0.4) H48A(0.4) C49A(0.4) H49A(0.4) C50A(0.4) H50A(0.4)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C37(H37), C40(H40)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C33(H33),
 C34(H34), C35(H35), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
 C46A(H46A), C47A(H47A), C48A(H48A), C49A(H49A), C50A(H50A)
5.c 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), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C)
;