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

data_4327593
_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            'C30 H32 B N9 S Zn'
_chemical_formula_weight         626.89
_chemical_melting_point          557
_chemical_name_common            LPic,MeZnSH
_chemical_name_systematic
;
Hydrotris(5-methyl-3-3'(4-methyl)-pyridyl-pyrazol-1-
yl)borato-zink-hydrogensulfide'
;
_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                 91.86(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.090(2)
_cell_length_b                   16.370(3)
_cell_length_c                   16.660(3)
_cell_measurement_temperature    200(2)
_cell_volume                     3022.9(10)
_computing_cell_refinement       'Cell (STOE) '
_computing_data_collection       'Exposure (STOE) '
_computing_data_reduction        'Integrate (STOE)'
_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      200(2)
_diffrn_measured_fraction_theta_full 0.758
_diffrn_measured_fraction_theta_max 0.758
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Phi-Mode, Oscillation'
_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  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14223
_diffrn_reflns_theta_full        28.10
_diffrn_reflns_theta_max         28.10
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_min  none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_meas      ?
_exptl_crystal_description       isometric
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.627
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    Riding-Model
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1441P)^2^+4.4513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.2226
_reflns_number_gt                4736
_reflns_number_total             5586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0105102B_3.cif
_cod_data_source_block           M3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not-measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3022.9(9)
_cod_database_code               4327593