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_4126704
_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         'C47 H71 N6 Na Ni2 O2'
_chemical_formula_sum            'C47 H71 N6 Na Ni2 O2'
_chemical_formula_weight         892.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                110.631(4)
_cell_angle_beta                 94.584(4)
_cell_angle_gamma                98.545(4)
_cell_formula_units_Z            2
_cell_length_a                   11.1496(5)
_cell_length_b                   13.0401(7)
_cell_length_c                   17.3856(8)
_cell_measurement_reflns_used    30911
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.830
_cell_measurement_theta_min      1.699
_cell_volume                     2315.3(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
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_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30911
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.830
_diffrn_reflns_theta_min         1.699
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.7971
_exptl_absorpt_correction_T_min  0.6473
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.320
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         9822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0585P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7866
_reflns_number_total             9822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08629_si_002.cif
_cod_data_source_block           Na2-pd127b
_cod_database_code               4126704
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.671
_shelx_estimated_absorpt_t_max   0.769
_shelx_res_checksum              78971
_shelx_hkl_checksum              61316