Reductive Trimerization of CO to the Deltate Dianion Using Activated Magnesium(I) Compounds.
Yuvaraj, K.; Douair, Iskander; Paparo, Albert; Maron, Laurent; Jones, Cameron; Journal of the American Chemical Society 141 (2019) 8764–8768; doi:10.1021/jacs.9b04085

data_4127605
_publ_section_title
;
 Reductive Trimerization of CO to the Deltate Dianion Using Activated
 Magnesium(I) Compounds.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8764
_journal_page_last               8768
_journal_paper_doi               10.1021/jacs.9b04085
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C72 H100.2 Mg2 N6 O0.2'
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_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
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_cell_angle_alpha                90
_cell_angle_beta                 106.9570(10)
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_cell_length_a                   19.62320(10)
_cell_length_b                   16.95570(10)
_cell_length_c                   20.77040(10)
_cell_measurement_reflns_used    46603
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      77.3350
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_cell_volume                     6610.38(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)'
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_computing_publication_material  Ciftab
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65651
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
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_diffrn_reflns_theta_max         67.997
_diffrn_reflns_theta_min         6.336
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85921
_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            orange
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       block
_exptl_crystal_F_000             2399
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         12009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+4.3443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11195
_reflns_number_total             12009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04085_si_006.cif
_cod_data_source_block           Cj1351
_cod_original_formula_sum        'C72 H100.20 Mg2 N6 O0.20'
_cod_database_code               4127605
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_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.914
_shelx_res_checksum              13535
_shelx_hkl_checksum              18078