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_1566334
_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_sum            'C34.67 H59 B N2 Ni P2'
_chemical_formula_weight         635.30
_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   geom
_atom_sites_solution_primary     SHELXT
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-09-03 deposited with the CCDC.	2022-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.639(5)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   23.1838(12)
_cell_length_b                   26.0619(11)
_cell_length_c                   17.5360(7)
_cell_measurement_reflns_used    11558
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      24.9800
_cell_measurement_theta_min      3.2350
_cell_volume                     10377.6(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31a (Rigaku OD, 2017)'
_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 5.8
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Dectris Pilatus 3R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1014
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36095
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.204
_diffrn_reflns_theta_max         25.204
_diffrn_reflns_theta_min         2.952
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.31a (Rigaku Oxford Diffraction, 2017) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       Block
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.476
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1105
_refine_ls_number_reflns         36095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1464
_refine_ls_R_factor_gt           0.0945
_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^)+(0.1826P)^2^+55.8112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2577
_refine_ls_wR_factor_ref         0.3333
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23932
_reflns_number_total             36095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06346d3.cif
_cod_data_source_block           007c-18066
_cod_depositor_comments
'Adding full bibliography for 1566334--1566339.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1566334
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.822
_shelx_estimated_absorpt_t_max   0.935
_shelx_res_checksum              42625
_shelx_hkl_checksum              32936