A Polar Copper-Boron One-Electron σ-Bond
Marc-Etienne Moret; Limei Zhang; Jonas C. Peters; Journal of the American Chemical Society 135 (2013) 3792–3795; doi:10.1021/ja4006578

data_4119472
_publ_section_title
;
 A Polar Copper-Boron One-Electron \s-Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3792
_journal_page_last               3795
_journal_paper_doi               10.1021/ja4006578
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C64 H94 B Cu K O10 P3'
_chemical_formula_weight         1229.75
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.586(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3982(5)
_cell_length_b                   34.9481(15)
_cell_length_c                   16.0773(7)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.90
_cell_measurement_theta_min      2.33
_cell_volume                     6397.8(5)
_computing_cell_refinement       'SAINT V7.68A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 v2010.7-0 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V7.68A (Bruker-AXS, 2007)'
_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      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w and \f 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  0.0659
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       -59
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            242329
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         37.48
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.9634
_exptl_absorpt_correction_T_min  0.8470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker-AXS, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       plate
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         32108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+2.5089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                23615
_reflns_number_total             32108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4006578_si_002_3.cif
_cod_data_source_block           mem140_0m
_cod_database_code               4119472