CO2 reduction or HCO2− oxidation? Solvent-dependent thermochemistry of a nickel hydride complex
Ceballos, Bianca M.; Tsay, Charlene; Yang, Jenny Y.; Chem. Commun.  (2017) –; doi:10.1039/C7CC02511D

data_7120285
_publ_section_title
;
 CO2 reduction or HCO2&#x2212; oxidation? Solvent-dependent
 thermochemistry of a nickel hydride complex
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02511D
_journal_year                    2017
_chemical_formula_sum            'C28 H64 B2 F8 Ni O8 P4'
_chemical_formula_weight         885.00
_chemical_name_systematic        Ni(tmepe)2(BF4)2
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-01 deposited with the CCDC.
2017-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.6513(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1558(19)
_cell_length_b                   12.2650(12)
_cell_length_c                   19.1620(19)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.92
_cell_measurement_theta_min      2.27
_cell_volume                     4212.8(7)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25493
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.013
_diffrn_reflns_theta_min         2.012
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       irregular
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_exptl_crystal_size_max          0.444
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_exptl_crystal_size_min          0.345
_refine_diff_density_max         1.189
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0822P)^2^+8.3673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4615
_reflns_number_total             5299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02511d2.cif
_cod_data_source_block           jyy104
_cod_original_cell_volume        4212.7(7)
_cod_database_code               7120285
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.750
_shelx_estimated_absorpt_t_max   0.797
_shelx_res_checksum              314