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_4115676
_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
;
[(C6H5)3PNP(C6H5)3] [((CH3)2-C2B10H8Hg)3]2 Cl
;
_chemical_formula_sum            'C60 H114 B60 Cl Hg6 N P2'
_chemical_formula_weight         2799.05
_chemical_name_common
;
PPN [B-hexamethyl 9-mercuracarborand-3]2.Cl
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 100.659(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   37.267(15)
_cell_length_b                   29.254(12)
_cell_length_c                   10.990(4)
_cell_measurement_reflns_used    1016
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      56.48
_cell_measurement_theta_min      6.68
_cell_volume                     11775(8)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_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  0.1046
_diffrn_reflns_av_sigmaI/netI    0.0965
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37707
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.11
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    7.877
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_type   Sadabs
_exptl_absorpt_process_details
;
Bruker Smart software
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       needle
_exptl_crystal_F_000             5232
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.35
_refine_diff_density_max         4.161
_refine_diff_density_min         -5.470
_refine_diff_density_rms         0.324
_refine_ls_extinction_coef       0.000035(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         14315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.0900
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1037P)^2^+688.1655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2206
_refine_ls_wR_factor_ref         0.2545
_reflns_number_gt                8031
_reflns_number_total             14315
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja010755l_3.cif
_cod_data_source_block           PPN[12.Cl]
_cod_original_cell_volume        11774(8)
_cod_database_code               4115676