Pyrazolylborate-Zinc-Hydrosulfide Complexes and Their Reactions
Michael Rombach; Heinrich Vahrenkamp; Inorganic Chemistry 40 (2001) 6144–6150; doi:10.1021/ic010510+

data_4327594
_publ_section_title
;
 Pyrazolylborate-Zinc-Hydrosulfide Complexes and Their Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6144
_journal_page_last               6150
_journal_paper_doi               10.1021/ic010510+
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C74 H75 B2 F24 N19 O8 S2 Zn2'
_chemical_formula_weight         2031.01
_chemical_name_common            'TpPic,MeZnSH 2 CF3(C(OH)2)CF3 '
_chemical_name_systematic
; 
Hydrotris(5-methyl-3-3'-(4-methyl)-pyridyl-pyrazol-1-
yl)borato-zink-hydrogensulfide 2 Hexafluoro-2,2-propandiole' 
;
_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                 97.7880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6544(8)
_cell_length_b                   16.2385(7)
_cell_length_c                   28.2153(11)
_cell_measurement_temperature    180(2)
_cell_volume                     8922.1(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL '
_computing_publication_material  'Bruker SHELXTL '
_computing_structure_refinement  'Bruker SHELXTL '
_computing_structure_solution    'Bruker SHELXTL '
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean '8192 pixel/mm'
_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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            61360
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.19
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       isometric
_exptl_crystal_F_000             4136
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.6
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1220
_refine_ls_number_reflns         12862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0833P)^2^+0.4828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1331
_reflns_number_gt                9356
_reflns_number_total             12862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0105102B_4.cif
_cod_data_source_block           M18
_cod_database_code               4327594