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

data_4327591
_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_moiety         'C30 H29 B N6 S Zn'
_chemical_formula_sum            'C32 H32 B N7 S Zn'
_chemical_formula_weight         622.89
_chemical_melting_point          471
_chemical_name_common            TpPhe,MeZnSH
_chemical_name_systematic
; 
Hydrotris(5-methyl-3-phenyl-pyrazol-1-yl)borato-zinc-hydrogensulfide 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 112.22(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.828(3)
_cell_length_b                   23.793(5)
_cell_length_c                   10.912(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     3083.2(13)
_computing_cell_refinement       'CAD4 5.1'
_computing_data_collection       'CAD4 5.1'
_computing_data_reduction        'CADFOR und CADSEX'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997), Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  Nonius-Turbo-CAD4
_diffrn_measurement_method       Omega-2Theta
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6260
_diffrn_reflns_theta_full        25.89
_diffrn_reflns_theta_max         25.89
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        10%
_diffrn_standards_interval_count 'OCR every 200 refl.'
_diffrn_standards_interval_time  'ICR every 1800s'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  none
_exptl_absorpt_correction_T_min  none
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            coulourless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       isometric
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    Riding-Model
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0383P)^2^+9.3230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1395
_reflns_number_gt                3718
_reflns_number_total             5937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0105102B_1.cif
_cod_data_source_block           M1
_cod_original_cell_volume        3083.2(11)
_cod_database_code               4327591