Synthesis and Crystal Structure of a New Hexahydro-closo-hexaborate Copper(I) Complex Cu2[(C6H5)3P]4B6H6
Raifah M. Kabbani; Arnold L. Rheingold; Kin-Chung Lam; Yevgeniy Margulis; Max Vovchenko; Inorganic Chemistry 38 (1999) 3748–3750; doi:10.1021/ic990248t

data_4322186
_publ_contact_author
; 
     Dr. Raifah M. Kabbani 
     Department of Chemistry and Physical Sciences  
     Pace University
     New York, NY 10038
     USA 
;
_publ_contact_author_email       rkabbabi@pace.edu.
_publ_contact_author_fax         '+212 346 1256'
_publ_contact_author_phone       '+212 488 1200'
_publ_section_title
;
 Synthesis and Crystal Structure of a New Hexahydro-closo-hexaborate
 Copper(I) Complex Cu2[(C6H5)3P]4B6H6
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3748
_journal_page_last               3750
_journal_paper_doi               10.1021/ic990248t
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C76 H72 B6 Cu2 N2 P4'
_chemical_formula_weight         1329.18
_chemical_name_systematic
;
 Cu2[(C6H5)3P]4B6H6
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.216(13)
_cell_angle_beta                 83.631(15)
_cell_angle_gamma                84.642(17)
_cell_formula_units_Z            1
_cell_length_a                   9.6717(19)
_cell_length_b                   10.576(2)
_cell_length_c                   17.653(2)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    256(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     1763.3(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      256(2)
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'omega 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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0858
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6801
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        <1%
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blade
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         5598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                3617
_reflns_number_total             5598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990248t.cif
_cod_data_source_block           pace01
_cod_original_cell_volume        1763.4(5)
_cod_database_code               4322186