Bimetallic Nickel-Cobalt Hydride in H2 Activation and Catalytic Proton Reduction
Wang, Wenguang; Chu, Xiaoxiao; Jin, Jihao; Ming, Bangrong; Pang, Maofu; Yu, Xin; Tung, Chen-Ho; Chemical Science  (2019) –; doi:10.1039/C8SC04346A

data_1550149
_publ_section_title
;
 Bimetallic Nickel-Cobalt Hydride in H2 Activation and Catalytic Proton
 Reduction
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04346A
_journal_year                    2019
_chemical_formula_moiety         'C H2 Cl2, C39 H45 Cl Co Ni P2 S2, F6 P'
_chemical_formula_sum            'C40 H47 Cl3 Co F6 Ni P3 S2'
_chemical_formula_weight         1022.79
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-02-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.02.02 svn.r3481 for OlexSys, GUI svn.r5470)
;
_audit_update_record
;
2018-05-08 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.789(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1464(3)
_cell_length_b                   13.3562(4)
_cell_length_c                   25.4313(7)
_cell_measurement_reflns_used    8312
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.5850
_cell_measurement_theta_min      3.7450
_cell_volume                     4666.6(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            28729
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.172
_diffrn_reflns_theta_min         3.579
_exptl_absorpt_coefficient_mu    7.121
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       solid
_exptl_crystal_F_000             2096
_refine_diff_density_max         1.181
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         9191
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1301
_refine_ls_R_factor_gt           0.0956
_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^)+(0.0702P)^2^+33.7617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2144
_refine_ls_wR_factor_ref         0.2377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6565
_reflns_number_total             9191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04346a2.cif
_cod_data_source_block           180226cxx-2_sq
_cod_database_code               1550149
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12
\\sim C13: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
3.a Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C14(H14A,H14B),
 C15(H15A,H15B)
3.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
  C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C)
;
_shelx_res_checksum              608
_shelx_fab_checksum              15458
_olex2_submission_special_instructions 'No special instructions were received'