Synthesis and Structural Characterization of Tris(2-mercapto-1-adamantylimidazolyl)hydroborato Complexes: A Sterically Demanding Tripodal [S3] Donor Ligand
Kevin Yurkerwich; Michael Yurkerwich; Gerard Parkin; Inorganic Chemistry 50 (2011) 12284–12295; doi:10.1021/ic201504d

data_4327096
_publ_section_title
;
 Synthesis and Structural Characterization of
 Tris(2-mercapto-1-adamantylimidazolyl)hydroborato Complexes: A Sterically
 Demanding Tripodal [S3] Donor Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12284
_journal_page_last               12295
_journal_paper_doi               10.1021/ic201504d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C40 H54 B Cl2 Ga2 I5 N6 S3'
_chemical_formula_weight         1570.72
_chemical_name_systematic
; 
 ? 
;
_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                 110.4300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   43.038(3)
_cell_length_b                   10.4807(6)
_cell_length_c                   24.4546(15)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.73
_cell_measurement_theta_min      2.27
_cell_volume                     10336.9(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      170(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0789
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            82091
_diffrn_reflns_theta_full        30.54
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    4.289
_exptl_absorpt_correction_T_max  0.8821
_exptl_absorpt_correction_T_min  0.5850
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.019
_exptl_crystal_description       plate
_exptl_crystal_F_000             6000
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.308
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         15789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0390P)^2^+26.7832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                9649
_reflns_number_total             15789
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201504d_si_002_08.cif
_cod_data_source_block           15s10
_cod_original_cell_volume        10336.8(11)
_cod_database_code               4327096