Pairwise H2/D2 Exchange and H2 Substitution at a Bimetallic Dinickel(II) Complex Featuring Two Terminal Hydrides.
Manz, Dennis-Helmut; Duan, Peng-Cheng; Dechert, Sebastian; Demeshko, Serhiy; Oswald, Rainer; John, Michael; Mata, Ricardo A.; Meyer, Franc; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b08629

data_4126705
_publ_section_title
;
 Pairwise H2/D2 Exchange and H2 Substitution at a Bimetallic Dinickel(II)
 Complex Featuring Two Terminal Hydrides.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b08629
_journal_year                    2017
_chemical_formula_moiety
'C39 H55 N6 Ni2 -, C28 H40.58 K O8 +, C4 H10 O'
_chemical_formula_sum            'C71 H105.58 K N6 Ni2 O9'
_chemical_formula_weight         1343.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
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_cell_angle_alpha                90
_cell_angle_beta                 94.7290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_b                   23.4343(3)
_cell_length_c                   23.2487(3)
_cell_measurement_reflns_used    82295
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.688
_cell_measurement_theta_min      1.159
_cell_volume                     14455.5(3)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2015)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2015)'
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_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'SHELXL-2016 (Sheldrick, 2016)'
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_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            82295
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.688
_diffrn_reflns_theta_min         1.159
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.9837
_exptl_absorpt_correction_T_min  0.8795
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2015)'
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       block
_exptl_crystal_F_000             5765
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     938
_refine_ls_number_reflns         13658
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+22.4791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11503
_reflns_number_total             13658
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08629_si_002.cif
_cod_data_source_block           2KDB18C6-pd184
_cod_database_code               4126705
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.746
_shelx_estimated_absorpt_t_max   0.878
_shelx_res_checksum              59972
_shelx_hkl_checksum              71228