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_4327098
_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            'C59 H56 B2 Cl4 F15 Ga N6 S3'
_chemical_formula_weight         1463.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.7140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7614(9)
_cell_length_b                   22.6171(16)
_cell_length_c                   20.7143(15)
_cell_measurement_reflns_used    9590
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      32.13
_cell_measurement_theta_min      2.17
_cell_volume                     5958.5(7)
_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      125(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            101812
_diffrn_reflns_theta_full        32.67
_diffrn_reflns_theta_max         32.67
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  0.8842
_exptl_absorpt_correction_T_min  0.7035
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;The unit cell contains 4 molecules of methylene chloride which have been
modeled as a diffuse contribution to the overall scattering.
;
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         20824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.1462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1016
_reflns_number_gt                15725
_reflns_number_total             20824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201504d_si_002_10.cif
_cod_data_source_block           sqp
_cod_database_code               4327098