A phosphine-free molecularly-defined Ni(II) complex in catalytic hydrogenation of CO<sub>2</sub>.
Bhardwaj, Ritu; Choudhury, Joyanta; Chemical communications (Cambridge, England) 60 (2024) 10176–10179; doi:10.1039/d4cc03054k

data_7133541
_publ_section_title
;
 A phosphine-free molecularly-defined Ni(II) complex in catalytic
 hydrogenation of CO<sub>2</sub>.
;
_journal_issue                   74
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10176
_journal_page_last               10179
_journal_paper_doi               10.1039/d4cc03054k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '2(C30 H35 N6 Ni), 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C62 H73 F12 N13 Ni2 P2'
_chemical_formula_weight         1407.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-06-23 deposited with the CCDC.	2024-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.365(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7635(11)
_cell_length_b                   13.5055(7)
_cell_length_c                   22.7364(12)
_cell_measurement_reflns_used    1166
_cell_measurement_temperature    140.00
_cell_measurement_theta_max      22.39
_cell_measurement_theta_min      2.48
_cell_volume                     6342.5(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      140.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  D8-venture
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1326
_diffrn_reflns_av_unetI/netI     0.1053
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            104927
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.154
_diffrn_reflns_theta_min         2.173
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5570
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1173 before and 0.0740 after correction.
The Ratio of minimum to maximum transmission is 0.7466.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       needle
_exptl_crystal_F_000             2920
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         18689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0432P)^2^+4.2259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10497
_reflns_number_total             18689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03054k2.cif
_cod_data_source_block           f1
_cod_depositor_comments          'Adding full bibliography for 7133541.cif.'
_cod_database_code               7133541
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C51(H51), C49(H49), C14(H14), C31(H31), C34(H34), C38(H38), C32(H32), C9(H9),
 C40(H40), C23(H23), C11(H11), C6(H6), C5(H5), C16(H16), C35(H35), C3(H3)
2.b Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C59(H59A,H59B,H59C), C25(H25A,H25B,H25C), C55(H55A,H55B,
 H55C), C62(H62A,H62B,H62C), C61(H61A,H61B,H61C), C26(H26A,H26B,H26C), C29(H29A,
 H29B,H29C), C27(H27A,H27B,H27C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C),
 C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C54(H54A,H54B,H54C), C44(H44A,H44B,
 H44C), C43(H43A,H43B,H43C), C21(H21A,H21B,H21C), C45(H45A,H45B,H45C), C63(H63A,
 H63B,H63C)
;
_shelx_res_checksum              32767
_shelx_hkl_checksum              91382
_olex2_submission_special_instructions 'No special instructions were received'