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_1550151
_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         'B F4, C39 H45 Co Ni P2 S2, C H2 Cl2'
_chemical_formula_sum            'C40 H47 B Cl2 Co F4 Ni P2 S2'
_chemical_formula_weight         929.18
_chemical_name_systematic
;
 ?
;
_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             2017-11-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-08 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.543(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9111(2)
_cell_length_b                   20.1158(4)
_cell_length_c                   16.5430(3)
_cell_measurement_reflns_used    10353
_cell_measurement_temperature    192.99(10)
_cell_measurement_theta_max      76.9420
_cell_measurement_theta_min      4.0190
_cell_volume                     4237.04(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      192.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     99.00 178.00   1.00    0.71    --  107.75  57.00 -30.00   79
  2  \w     93.00 178.00   1.00    0.71    --  107.75  57.00   0.00   85
  3  \w     89.00 130.00   1.00    0.71    --  107.75  71.00  49.00   41
  4  \w    150.00 176.00   1.00    0.71    --  107.75  71.00  49.00   26
  5  \w     96.00 166.00   1.00    0.71    --  107.75  37.00 120.00   70
  6  \w     31.00  59.00   1.00    0.10    --   48.45  71.00  49.00   28
  7  \w     72.00  99.00   1.00    0.10    --   48.45  71.00  49.00   27
  8  \w    -68.00  12.00   1.00    0.10    --  -48.45  71.00  49.00   80
  9  \w    -77.00 -25.00   1.00    0.71    --  -86.25  71.00  49.00   52
 10  \w   -117.00 -71.00   1.00    0.10    --  -48.45-125.00  60.00   46
 11  \w   -120.00 -28.00   1.00    0.10    --  -48.45 -71.00 -80.00   92
 12  \w      9.00  69.00   1.00    0.10    --   48.45 -71.00 -80.00   60
 13  \w     41.00  94.00   1.00    0.71    --  107.75 -99.00-180.00   53
 14  \w     36.00 110.00   1.00    0.71    --  107.75 -99.00-120.00   74
 15  \w     46.00 128.00   1.00    0.71    --  107.75 -71.00 -80.00   82
 16  \w   -158.00 -66.00   1.00    0.71    --  -86.25 -71.00 -80.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0659272000
_diffrn_orient_matrix_UB_12      0.0589796000
_diffrn_orient_matrix_UB_13      0.0223746000
_diffrn_orient_matrix_UB_21      -0.0863482000
_diffrn_orient_matrix_UB_22      -0.0166241000
_diffrn_orient_matrix_UB_23      -0.0732143000
_diffrn_orient_matrix_UB_31      -0.0534023000
_diffrn_orient_matrix_UB_32      -0.0458903000
_diffrn_orient_matrix_UB_33      0.0552661000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29630
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.494
_diffrn_reflns_theta_min         4.035
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.797
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       solid
_exptl_crystal_F_000             1916
_refine_diff_density_max         1.404
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.118
_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     483
_refine_ls_number_reflns         8423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0673
_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^)+(0.0910P)^2^+13.6910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7034
_reflns_number_total             8423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04346a2.cif
_cod_data_source_block           171019cxx-1
_cod_database_code               1550151
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CoNiPSCH
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C0AA(H0AA,
 H0AB)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C29(H29)
2.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              24670
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.610
_oxdiff_exptl_absorpt_empirical_full_min 0.774