Synergistic Cu<sub>2</sub> Catalysts for Formic Acid Dehydrogenation.
Nakajima, Takayuki; Kamiryo, Yoshia; Kishimoto, Masayo; Imai, Kaho; Nakamae, Kanako; Ura, Yasuyuki; Tanase, Tomoaki; Journal of the American Chemical Society 141 (2019) 8732–8736; doi:10.1021/jacs.9b03532

data_4127509
_publ_section_title
;
 Synergistic Cu<sub>2</sub> Catalysts for Formic Acid Dehydrogenation.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8732
_journal_page_last               8736
_journal_paper_doi               10.1021/jacs.9b03532
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C49 H52 Cu2 F12 N4 P6'
_chemical_formula_sum            'C49 H52 Cu2 F12 N4 P6'
_chemical_formula_weight         1237.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 102.508(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.870(3)
_cell_length_b                   16.613(3)
_cell_length_c                   21.508(4)
_cell_measurement_reflns_used    9544
_cell_measurement_temperature    153
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.20
_cell_volume                     5536.0(18)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_molecular_graphics    'CrystalStructure 4.2.5'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      153
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33352
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         3.170
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  0.816
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2520.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.34
_refine_ls_abs_structure_details
;
 Flack x determined using 5105 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     658
_refine_ls_number_reflns         12260
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0218P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0631
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                11127
_reflns_number_total             12260
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja9b03532_si_002.cif
_cod_data_source_block           8
_cod_database_code               4127509
_shelx_res_checksum              96735
_shelx_hkl_checksum              10816