Triphosphine-Ligated Copper Hydrides for CO2 Hydrogenation: Structure, Reactivity, and Thermodynamic Studies.
Zall, Christopher M.; Linehan, John C.; Appel, Aaron M.; Journal of the American Chemical Society 138 (2016) 9968–9977; doi:10.1021/jacs.6b05349

data_4130627
_publ_section_title
;
 Triphosphine-Ligated Copper Hydrides for CO2 Hydrogenation: Structure,
 Reactivity, and Thermodynamic Studies.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9968
_journal_page_last               9977
_journal_paper_doi               10.1021/jacs.6b05349
_journal_volume                  138
_journal_year                    2016
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C82 H79 Cu2 P6'
_chemical_formula_sum            'C82 H79 Cu2 P6'
_chemical_formula_weight         1377.35
_chemical_name_common            '[(p3Cu)2H]PF6'
_space_group_crystal_system      trigonal
_space_group_IT_number           149
_space_group_name_Hall           'P 3 2'
_space_group_name_H-M_alt        'P 3 1 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.6406(13)
_cell_length_b                   21.6406(13)
_cell_length_c                   16.2448(11)
_cell_measurement_reflns_used    9557
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      21.69
_cell_measurement_theta_min      2.26
_cell_volume                     6588.5(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker 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  0.0738
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            65812
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.121
_diffrn_reflns_theta_max         25.121
_diffrn_reflns_theta_min         1.086
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.041
_exptl_crystal_description       Block
_exptl_crystal_F_000             2157
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.312
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7844
_refine_ls_number_restraints     700
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1216P)^2^+7.2468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1805
_refine_ls_wR_factor_ref         0.2230
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                4930
_reflns_number_total             7844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05349_si_002.cif
_cod_data_source_block           Zall016_sad_sq
_cod_original_cell_volume        6588.5(9)
_cod_database_code               4130627
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              53462
_shelx_hkl_checksum              68053
_shelx_fab_checksum              13892