Electrocatalytic hydrogen evolution by robust square planar nickel complexes in an S2P2 coordination environment
Chen, Luo; Li, Tao; Xie, Bin; Lai, Chuan; Ji, Run-Wu; He, Jia-Yu; Cao, Jia-Xi; Liu, Meng-Nan; Li, Wei; Zhang, Dong-Liang; Catalysis Science & Technology 13 (2023) 3655–3666; doi:10.1039/D2CY02158G

data_1569186
_publ_section_title
;
 Electrocatalytic hydrogen evolution by robust square planar nickel
 complexes in an S2P2 coordination environment
;
_journal_issue                   12
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              3655
_journal_page_last               3666
_journal_paper_doi               10.1039/D2CY02158G
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C45 H35 Br2 N Ni O P2 S2, C H2 Cl2'
_chemical_formula_sum            'C46 H37 Br2 Cl2 N Ni O P2 S2'
_chemical_formula_weight         1035.25
_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     dual
_audit_creation_date             2020-09-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-30 deposited with the CCDC.	2023-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                118.128(4)
_cell_angle_beta                 102.945(4)
_cell_angle_gamma                94.354(6)
_cell_formula_units_Z            2
_cell_length_a                   8.874(17)
_cell_length_b                   16.683(12)
_cell_length_c                   16.979(12)
_cell_measurement_reflns_used    3946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.41
_cell_volume                     2112(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0955
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10613
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.409
_exptl_absorpt_coefficient_mu    2.691
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.3681
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1193 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.4938.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.199
_refine_diff_density_min         -1.783
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         7306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0666
_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^)+(0.1006P)^2^+11.6827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1860
_refine_ls_wR_factor_ref         0.1993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5557
_reflns_number_total             7306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cy02158g2.cif
_cod_data_source_block           ww
_cod_depositor_comments
'Adding full bibliography for 1569186--1569187.cif.'
_cod_database_code               1569186
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.756
_shelx_estimated_absorpt_t_min   0.643
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H46A(0.5) H46B(0.5) H46C(0.5) H46D(0.5) Cl1(0.5) Cl2(0.5)
 Cl1A(0.5) Cl2A(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C46(H46C,H46D)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C10(H10), C11(H11), C13(H13), C14(H14),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C43(H43),
  C44(H44)
3.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C)
;
_shelx_res_checksum              38425
_olex2_submission_special_instructions 'No special instructions were received'