Cross-coupling of CO and an isocyanide mediated by a tetrameric magnesium hydride cluster.
Yang, Wenbang; White, Andrew J. P.; Crimmin, Mark R.; Chemical science 15 (2024) 11807–11813; doi:10.1039/d4sc02638a

data_1571986
_publ_section_title
;
 Cross-coupling of CO and an isocyanide mediated by a tetrameric magnesium
 hydride cluster.
;
_journal_issue                   30
_journal_name_full               'Chemical science'
_journal_page_first              11807
_journal_page_last               11813
_journal_paper_doi               10.1039/d4sc02638a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C86 H118 Mg4 N10, 1.5(C4 H10 O)'
_chemical_formula_sum            'C92 H133 Mg4 N10 O1.5'
_chemical_formula_weight         1500.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-01-26 deposited with the CCDC.	2024-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.6657(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0772(2)
_cell_length_b                   15.05708(15)
_cell_length_c                   30.2204(3)
_cell_measurement_reflns_used    11649
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.4680
_cell_measurement_theta_min      3.9120
_cell_volume                     9117.06(16)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4115
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            30683
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.681
_diffrn_reflns_theta_min         3.281
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3260
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.273
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         17484
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0644P)^2^+0.7242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13517
_reflns_number_total             17484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02638a3.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 1571986--1571991.cif.'
_cod_original_cell_volume        9117.04(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C92 H133 Mg4 N10 O1.50'
_cod_database_code               1571986
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              24319
_shelx_hkl_checksum              16219