Tetra-, hexa- and octanuclear copper hydride complexes supported by tridentate phosphine ligands.
Nakajima, Takayuki; Nakamae, Kanako; Hatano, Rika; Imai, Kaho; Harada, Masafumi; Ura, Yasuyuki; Tanase, Tomoaki; Dalton transactions (Cambridge, England : 2003) 48 (2019) 12050–12059; doi:10.1039/c9dt02467k

data_7700593
_publ_section_title
;
 Tetra-, hexa- and octanuclear copper hydride complexes supported by
 tridentate phosphine ligands.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12050
_journal_page_last               12059
_journal_paper_doi               10.1039/c9dt02467k
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C128 H120 B2 Cu8 F8 P12'
_chemical_formula_sum            'C128 H120 B2 Cu8 F8 P12'
_chemical_formula_weight         2712.02
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-07-11 deposited with the CCDC.    2019-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   26.0932(16)
_cell_length_b                   26.0932(16)
_cell_length_c                   28.933(3)
_cell_measurement_reflns_used    17317
_cell_measurement_temperature    153
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.20
_cell_volume                     19699(3)
_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    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      153
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1550
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            75046
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.111
_diffrn_reflns_theta_max         25.111
_diffrn_reflns_theta_min         3.154
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5528.00
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.77
_refine_ls_abs_structure_details
;
 Flack x determined using 2603 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     363
_refine_ls_number_reflns         8716
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1316P)^2^+4.1424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2006
_refine_ls_wR_factor_ref         0.2177
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                7051
_reflns_number_total             8716
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9dt02467k2.cif
_cod_data_source_block           '[Cu8H6(dpmp)4](PF6)2'
_cod_depositor_comments
'Adding full bibliography for 7700591--7700594.cif.'
_cod_database_code               7700593
_shelx_res_checksum              31307
_shelx_fab_checksum              66508