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_1550153
_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         '2(B F4), C41 H48 Co N Ni P2 S2, 4(C2 H3 N)'
_chemical_formula_sum            'C49 H60 B2 Co F8 N5 Ni P2 S2'
_chemical_formula_weight         1136.34
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-01-31
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9622(9)
_cell_length_b                   11.6996(4)
_cell_length_c                   20.9046(7)
_cell_measurement_reflns_used    9637
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      30.4020
_cell_measurement_theta_min      3.4420
_cell_volume                     5371.4(3)
_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)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.996
_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      6.00  52.00   1.00   32.00    --    5.65  11.00  15.00   46
  2  \w    -15.00  26.00   1.00   32.00    --   -4.48 -99.00-180.00   41
  3  \w     29.00  54.00   1.00   32.00    --    5.65-162.00 -78.00   25
  4  \w    -74.00  -1.00   1.00   32.00    --   -4.48 -37.00 120.00   73
;
_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      0.0292849000
_diffrn_orient_matrix_UB_12      0.0255447000
_diffrn_orient_matrix_UB_13      0.0016256000
_diffrn_orient_matrix_UB_21      0.0136453000
_diffrn_orient_matrix_UB_22      -0.0542544000
_diffrn_orient_matrix_UB_23      -0.0047340000
_diffrn_orient_matrix_UB_31      -0.0005505000
_diffrn_orient_matrix_UB_32      0.0088843000
_diffrn_orient_matrix_UB_33      -0.0335411000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27156
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.421
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98787
_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    1.405
_exptl_crystal_description       solid
_exptl_crystal_F_000             2352
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 3338 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.007(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         8897
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+1.9290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_full    0.856
_reflns_Friedel_fraction_max     0.875
_reflns_number_gt                8027
_reflns_number_total             8897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04346a2.cif
_cod_data_source_block           171209cxx-1
_cod_database_code               1550153
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         CoNiPSCN
_reflns_odcompleteness_completeness 99.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {HI,HJ,HK} of C49, All C(H,H) groups
 At 1.5 times of:
  {H5A,H5B,H5C} of C5, {H39A,H39B,H39C} of C39, {H40A,H40B,H40C} of C40,
  {H37A,H37B,H37C} of C37, {H38A,H38B,H38C} of C38, {HF,HG,HH} of C47, {HC,HD,
  HE} of C4, {H,HA,HB} of C43, {H41A,H41B,H41C} of C41
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1AA(H1AA,H1AB), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26),
  C28(H28), C29(H29), C30(H30), C31(H31)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H,HA,HB), C4(HC,HD,HE),
 C47(HF,HG,HH), C49(HI,HJ,HK)
;
_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 1.059
_oxdiff_exptl_absorpt_empirical_full_min 0.848