Ligand and solvent effects on CO2 insertion into group 10 metal alkyl bonds
Deziel, Anthony P.; Espinosa, Matthew R.; Pavlovic, Ljiljana; Charboneau, David J.; Hazari, Nilay; Hopmann, Kathrin H.; Mercado, Brandon Q.; Chemical Science 13 (2022) 2391–2404; doi:10.1039/D1SC06346D

data_1566336
_publ_section_title
;
 Ligand and solvent effects on CO2 insertion into group 10 metal alkyl
 bonds
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2391
_journal_page_last               2404
_journal_paper_doi               10.1039/D1SC06346D
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C50 H94 B2 N6 Ni2 P4'
_chemical_formula_sum            'C50 H94 B2 N6 Ni2 P4'
_chemical_formula_weight         1042.23
_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     SHELXT
_atom_sites_solution_secondary   difmap
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_audit_update_record
;
2021-09-03 deposited with the CCDC.	2022-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                103.985(7)
_cell_angle_beta                 111.062(7)
_cell_angle_gamma                90.654(5)
_cell_formula_units_Z            1
_cell_length_a                   10.5516(6)
_cell_length_b                   11.9228(9)
_cell_length_c                   13.7755(12)
_cell_measurement_reflns_used    6672
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      65.8380
_cell_measurement_theta_min      3.5420
_cell_volume                     1560.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB-2014/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1493
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            37353
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.564
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       Plate
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         5403
_refine_ls_number_restraints     565
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0794
_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^)+(0.1152P)^2^+1.7063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2006
_refine_ls_wR_factor_ref         0.2239
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3561
_reflns_number_total             5403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06346d3.cif
_cod_data_source_block           007a-19019
_cod_depositor_comments
'Adding full bibliography for 1566334--1566339.cif.'
_cod_database_code               1566336
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.694
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              23646
_shelx_hkl_checksum              36621
_shelx_fab_checksum              42383