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_4327091
_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            'C41 H56 B Cl4 I N6 S3 Zn'
_chemical_formula_weight         1073.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   15.1780(6)
_cell_length_b                   15.1780(6)
_cell_length_c                   69.100(3)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      31.73
_cell_measurement_theta_min      2.68
_cell_volume                     13786.0(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0806
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       102
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            66759
_diffrn_reflns_theta_full        31.88
_diffrn_reflns_theta_max         31.88
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_T_max  0.8554
_exptl_absorpt_correction_T_min  0.7711
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             6576
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_platon_squeeze_details
; The unit cell contains 24 methylene chloride molecules which have been
treated as a diffuse contribution to the overall scattering without
specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.288
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         5154
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                3356
_reflns_number_total             5154
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201504d_si_002_03.cif
_cod_data_source_block           novap
_cod_original_cell_volume        13785.9(10)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4327091