Electron Transfer from Hexameric Copper Hydrides
Michael S. Eberhart; Jack R. Norton; Ashley Zuzek; Wesley Sattler; Serge Ruccolo; Journal of the American Chemical Society 135 (2013) 17262–17265; doi:10.1021/ja408925m

data_4121163
_publ_section_title
;
 Electron Transfer from Hexameric Copper Hydrides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17262
_journal_page_last               17265
_journal_paper_doi               10.1021/ja408925m
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C90 H75 Cu3 P6'
_chemical_formula_weight         1532.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.054(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.758(13)
_cell_length_b                   15.190(9)
_cell_length_c                   26.251(16)
_cell_measurement_reflns_used    9342
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.83
_cell_measurement_theta_min      2.30
_cell_volume                     8041(8)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_sigmaI/netI    0.0707
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            128437
_diffrn_reflns_theta_full        30.82
_diffrn_reflns_theta_max         30.82
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.8553
_exptl_absorpt_correction_T_min  0.6233
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       block
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
The unit cell contains 4 toluene molecules which have been treated as a diffuse
contribution to the overall scattering without atom position by SQUEEZE/PLATON 
;
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     904
_refine_ls_number_reflns         24937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                15874
_reflns_number_total             24937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408925m_si_002.cif
_cod_data_source_block           mic2s10
_cod_database_code               4121163