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_4127601
_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            'C61 H86 Mg2 N6'
_chemical_formula_weight         951.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 105.161(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1084(2)
_cell_length_b                   23.7535(3)
_cell_length_c                   20.6189(3)
_cell_measurement_reflns_used    29668
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      77.8480
_cell_measurement_theta_min      3.6980
_cell_volume                     5723.94(16)
_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    xseed
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58257
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.000
_diffrn_reflns_theta_min         6.554
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75868
_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            red
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 7548 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1279
_refine_ls_number_reflns         19672
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0715P)^2^+0.5601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    0.888
_reflns_Friedel_fraction_max     0.886
_reflns_number_gt                18128
_reflns_number_total             19672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04085_si_004.cif
_cod_data_source_block           Cj1350
_cod_original_cell_volume        5723.94(15)
_cod_database_code               4127601
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.887
_shelx_res_checksum              6779
_shelx_hkl_checksum              28411