Benzannulated tris(2-mercapto-1-imidazolyl)hydroborato ligands: tetradentate κ4-S3H binding and access to monomeric monovalent thallium in an [S3] coordination environment.
Rong, Yi; Palmer, Joshua H.; Parkin, Gerard; Dalton transactions (Cambridge, England : 2003) 43 (2014) 1397–1407; doi:10.1039/c3dt52418c

data_7028633
_publ_section_title
;
 Benzannulated tris(2-mercapto-1-imidazolyl)hydroborato ligands:
 tetradentate \k4-S3H binding and access to monomeric monovalent thallium
 in an [S3] coordination environment.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1397
_journal_page_last               1407
_journal_paper_doi               10.1039/c3dt52418c
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C36 H46 B K N6 O4 S3'
_chemical_formula_weight         772.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :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                   15.7585(12)
_cell_length_b                   15.7585(12)
_cell_length_c                   52.744(4)
_cell_measurement_reflns_used    9646
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.32
_cell_volume                     11343.1(15)
_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      130(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       75
_diffrn_reflns_limit_l_min       -75
_diffrn_reflns_number            56765
_diffrn_reflns_theta_full        30.61
_diffrn_reflns_theta_max         30.61
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  0.7848
_exptl_absorpt_correction_T_min  0.7531
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.78
_exptl_crystal_size_min          0.72
_platon_squeeze_details
; 
The unit cell contains twelve acetone molecules which have been treated as a diffuse contribution to the overall 
scattering without specific atom positions by SQUEEZE/PLATON. 
;
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         7721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0689P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                5441
_reflns_number_total             7721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52418c.txt
_cod_data_source_block           tmks10(jhp-2-97-b)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7028633