Octahedral Coordination of Halide Ions (I-, Br-, Cl-) Sandwich Bonded with Tridentate Mercuracarborand-3 Receptors
Hans Lee; Carolyn B. Knobler; M. Frederick Hawthorne; Journal of the American Chemical Society 123 (2001) 8543–8549; doi:10.1021/ja010755l

data_4115675
_publ_contact_author
;
Hawthorne, M. F.,
Department of Chemistry and Biochemistry,
University of California,
Los Angeles, CA 90095-1569.  USA
;
_publ_contact_author_email       hawthorne@chem.ucla.edu
_publ_contact_author_fax         310-825-5490
_publ_contact_author_phone       310-825-7378
_publ_section_title
;
 Octahedral Coordination of Halide Ions (I-, Br-, Cl-) Sandwich Bonded
 with Tridentate Mercuracarborand-3 Receptors
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8543
_journal_page_last               8549
_journal_paper_doi               10.1021/ja010755l
_journal_volume                  123
_journal_year                    2001
_chemical_formula_moiety
;
CH3P(C6H5)3 [((CH3)2C2B10H8Hg)3)2.Br] ((CH3)2CO)2  (H2O)2
;
_chemical_formula_sum            'C24.5 H56.5 B30 Br0.5 Hg3 O1.5 P0.5'
_chemical_formula_weight         1356.71
_chemical_name_common
;
triphenylmethylphosphonium [(B-hexamethyl 9-mercuracarborand-3)2.Br] 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 106.424(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.671(8)
_cell_length_b                   17.576(6)
_cell_length_c                   26.079(8)
_cell_measurement_reflns_used    1001
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.33
_cell_measurement_theta_min      6.91
_cell_volume                     10847(6)
_computing_cell_refinement       'Bruker software'
_computing_data_collection       'Bruker software'
_computing_data_reduction        'Bruker software'
_computing_molecular_graphics    'Bruker software'
_computing_publication_material  'Bruker software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker Smart 1000'
_diffrn_measurement_method       'phi and 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  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            34317
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    8.878
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_type   Sadabs
_exptl_absorpt_process_details
;
Bruker software
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             5044
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         4.112
_refine_diff_density_min         -2.748
_refine_diff_density_rms         0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         12824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          1.831
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+409.5086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1578
_reflns_number_gt                9787
_reflns_number_total             12824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja010755l_2.cif
_cod_data_source_block           MePPh3[12.Br].((CH3)2CO)2.(H2O)2
_cod_original_formula_sum        'C24.50 H56.50 B30 Br0.50 Hg3 O1.50 P0.50'
_cod_database_code               4115675