#------------------------------------------------------------------------------
#$Date: 2024-11-15 14:46:36 +0200 (Fri, 15 Nov 2024) $
#$Revision: 295934 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/75/4327593.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4327593
loop_
_publ_author_name
'Michael Rombach'
'Heinrich Vahrenkamp'
_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/[σ²(Fo²)+(0.1441P)²+4.4513P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zn1 Zn 0.77931(4) 0.71425(3) 0.23870(2) 0.02530(19) Uani 1 1 d .
S1 S 0.86983(12) 0.75910(8) 0.13069(6) 0.0408(3) Uani 1 1 d .
H1 H 0.8325 0.7223 0.0728 0.061 Uiso 1 1 calc R
N1 N 0.5938(4) 0.7201(2) 0.24705(18) 0.0287(7) Uani 1 1 d .
N2 N 0.8100(3) 0.7617(2) 0.35204(17) 0.0282(7) Uani 1 1 d .
N3 N 0.7846(3) 0.5962(2) 0.28168(16) 0.0256(6) Uani 1 1 d .
N4 N 0.5544(3) 0.6965(2) 0.32116(17) 0.0274(7) Uani 1 1 d .
N5 N 0.7382(3) 0.7287(2) 0.40898(17) 0.0282(7) Uani 1 1 d .
N6 N 0.7146(3) 0.5875(2) 0.34781(17) 0.0280(7) Uani 1 1 d .
N7 N 0.5893(4) 0.7851(2) -0.0057(2) 0.0349(8) Uani 1 1 d .
N8 N 1.1295(5) 0.8839(3) 0.2604(2) 0.0460(10) Uani 1 1 d .
N9 N 1.0851(4) 0.5441(3) 0.1245(2) 0.0394(9) Uani 1 1 d .
B1 B 0.6465(4) 0.6608(3) 0.3845(2) 0.0289(9) Uani 1 1 d .
H1 H 0.6038 0.6426 0.4319 0.035 Uiso 1 1 d R
C1 C 0.4389(4) 0.7172(3) 0.3286(2) 0.0296(8) Uani 1 1 d .
C2 C 0.3996(4) 0.7540(3) 0.2575(2) 0.0340(9) Uani 1 1 d .
H2 H 0.3229 0.7740 0.2449 0.041 Uiso 1 1 d R
C3 C 0.4995(4) 0.7543(2) 0.2085(2) 0.0272(8) Uani 1 1 d .
C4 C 0.3705(5) 0.7035(3) 0.4039(3) 0.0400(10) Uani 1 1 d .
H4A H 0.4218 0.6769 0.4433 0.060 Uiso 1 1 d R
H4B H 0.3015 0.6697 0.3918 0.060 Uiso 1 1 d R
H4C H 0.3443 0.7550 0.4245 0.060 Uiso 1 1 d R
C5 C 0.5076(4) 0.7889(2) 0.1269(2) 0.0282(8) Uani 1 1 d .
C6 C 0.4435(4) 0.8579(3) 0.1058(2) 0.0340(9) Uani 1 1 d .
H6 H 0.3934 0.8823 0.1426 0.041 Uiso 1 1 d R
C7 C 0.4543(5) 0.8919(3) 0.0295(2) 0.0385(10) Uani 1 1 d .
H7 H 0.4111 0.9385 0.0148 0.046 Uiso 1 1 d R
C8 C 0.5294(4) 0.8541(3) -0.0239(2) 0.0326(9) Uani 1 1 d .
C9 C 0.5765(4) 0.7532(3) 0.0682(2) 0.0327(9) Uani 1 1 d .
H9 H 0.6160 0.7044 0.0803 0.039 Uiso 1 1 d R
C10 C 0.5476(5) 0.8894(4) -0.1059(2) 0.0456(12) Uani 1 1 d .
H10A H 0.6021 0.8555 -0.1347 0.068 Uiso 1 1 d R
H10B H 0.5808 0.9434 -0.1005 0.068 Uiso 1 1 d R
H10C H 0.4714 0.8921 -0.1348 0.068 Uiso 1 1 d R
C11 C 0.7483(4) 0.7731(3) 0.4781(2) 0.0284(8) Uani 1 1 d .
C12 C 0.8302(4) 0.8351(3) 0.4662(2) 0.0351(9) Uani 1 1 d .
H12 H 0.8541 0.8753 0.5028 0.042 Uiso 1 1 d R
C13 C 0.8693(4) 0.8257(3) 0.3870(2) 0.0308(8) Uani 1 1 d .
C14 C 0.6797(5) 0.7542(3) 0.5517(2) 0.0410(11) Uani 1 1 d .
H14A H 0.6293 0.7074 0.5416 0.062 Uiso 1 1 d R
H14B H 0.6304 0.8000 0.5655 0.062 Uiso 1 1 d R
H14C H 0.7357 0.7426 0.5954 0.062 Uiso 1 1 d R
C15 C 0.9556(4) 0.8766(3) 0.3442(2) 0.0295(8) Uani 1 1 d .
C16 C 0.9479(5) 0.9602(3) 0.3444(3) 0.0406(10) Uani 1 1 d .
H16 H 0.8873 0.9862 0.3721 0.049 Uiso 1 1 d R
C17 C 1.0306(5) 1.0058(3) 0.3025(3) 0.0451(11) Uani 1 1 d .
H17 H 1.0277 1.0626 0.3024 0.054 Uiso 1 1 d R
C18 C 1.1191(4) 0.9639(3) 0.2604(3) 0.0375(9) Uani 1 1 d .
C19 C 1.0470(4) 0.8411(3) 0.3012(3) 0.0374(9) Uani 1 1 d .
H19 H 1.0515 0.7844 0.3005 0.045 Uiso 1 1 d R
C20 C 1.2102(6) 1.0108(4) 0.2128(3) 0.0540(14) Uani 1 1 d .
H20A H 1.2640 0.9735 0.1875 0.081 Uiso 1 1 d R
H20B H 1.2557 1.0463 0.2482 0.081 Uiso 1 1 d R
H20C H 1.1682 1.0427 0.1725 0.081 Uiso 1 1 d R
C21 C 0.7128(4) 0.5081(3) 0.3706(2) 0.0311(8) Uani 1 1 d .
C22 C 0.7844(4) 0.4646(3) 0.3188(2) 0.0328(9) Uani 1 1 d .
H22 H 0.8008 0.4089 0.3200 0.039 Uiso 1 1 d R
C23 C 0.8273(4) 0.5222(2) 0.26473(19) 0.0265(7) Uani 1 1 d .
C24 C 0.6470(6) 0.4767(3) 0.4410(3) 0.0493(14) Uani 1 1 d .
H24A H 0.6042 0.5205 0.4657 0.074 Uiso 1 1 d R
H24B H 0.7047 0.4541 0.4790 0.074 Uiso 1 1 d R
H24C H 0.5910 0.4351 0.4238 0.074 Uiso 1 1 d R
C25 C 0.9123(4) 0.5058(3) 0.20024(19) 0.0285(8) Uani 1 1 d .
C26 C 0.9126(4) 0.4297(3) 0.1614(2) 0.0335(9) Uani 1 1 d .
H26 H 0.8544 0.3911 0.1734 0.040 Uiso 1 1 d R
C27 C 0.9969(5) 0.4122(3) 0.1055(2) 0.0370(10) Uani 1 1 d .
H27 H 0.9958 0.3620 0.0793 0.044 Uiso 1 1 d R
C28 C 1.0848(4) 0.4707(3) 0.0891(2) 0.0333(9) Uani 1 1 d .
C29 C 1.0013(4) 0.5608(3) 0.1783(2) 0.0321(8) Uani 1 1 d .
H29 H 1.0027 0.6123 0.2020 0.039 Uiso 1 1 d R
C30 C 1.1813(6) 0.4507(4) 0.0312(3) 0.0504(13) Uani 1 1 d .
H30A H 1.2337 0.4971 0.0267 0.076 Uiso 1 1 d R
H30B H 1.1449 0.4385 -0.0205 0.076 Uiso 1 1 d R
H30C H 1.2272 0.4045 0.0501 0.076 Uiso 1 1 d R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N2 Zn1 N3 91.91(13) y
N2 Zn1 N1 93.22(14) y
N3 Zn1 N1 92.15(14) y
N2 Zn1 S1 123.63(11) y
N3 Zn1 S1 125.79(9) y
N1 Zn1 S1 121.16(9) y
C3 N1 N4 106.4(3) y
C3 N1 Zn1 138.9(3) y
N4 N1 Zn1 113.1(3) y
C13 N2 N5 107.0(3) y
C13 N2 Zn1 138.4(3) y
N5 N2 Zn1 113.8(3) y
C23 N3 N6 106.8(3) y
C23 N3 Zn1 141.6(2) y
N6 N3 Zn1 111.4(2) y
C1 N4 N1 110.2(3) y
C1 N4 B1 129.9(3) y
N1 N4 B1 119.5(3) y
N2 N5 C11 109.9(4) y
N2 N5 B1 119.4(3) y
C11 N5 B1 129.7(3) y
C21 N6 N3 109.8(3) y
C21 N6 B1 128.2(3) y
N3 N6 B1 121.9(3) y
C8 N7 C9 117.8(4) y
C18 N8 C19 117.1(4) y
C28 N9 C29 119.0(4) y
N5 B1 N6 109.5(3) y
N5 B1 N4 108.6(3) y
N6 B1 N4 109.9(3) y
N4 C1 C2 107.9(3) y
N4 C1 C4 123.5(4) y
C2 C1 C4 128.6(4) y
C1 C2 C3 105.5(4) y
N1 C3 C2 110.0(3) y
N1 C3 C5 122.2(4) y
C2 C3 C5 127.7(4) y
C6 C5 C9 117.2(4) y
C6 C5 C3 120.2(4) y
C9 C5 C3 122.5(4) y
C5 C6 C7 120.0(4) y
C8 C7 C6 118.6(4) y
N7 C8 C7 122.4(4) y
N7 C8 C10 116.7(4) y
C7 C8 C10 120.9(4) y
N7 C9 C5 123.8(4) y
N5 C11 C12 107.8(3) y
N5 C11 C14 123.5(4) y
C12 C11 C14 128.7(4) y
C11 C12 C13 106.2(4) y
N2 C13 C12 109.0(4) y
N2 C13 C15 122.9(3) y
C12 C13 C15 128.0(4) y
C16 C15 C19 117.8(4) y
C16 C15 C13 121.5(4) y
C19 C15 C13 120.7(4) y
C15 C16 C17 119.5(5) y
C16 C17 C18 118.2(5) y
N8 C18 C17 123.3(4) y
N8 C18 C20 116.4(5) y
C17 C18 C20 120.3(5) y
N8 C19 C15 124.0(5) y
N6 C21 C22 107.7(3) y
N6 C21 C24 124.2(4) y
C22 C21 C24 128.1(4) y
C21 C22 C23 105.6(4) y
N3 C23 C22 110.2(3) y
N3 C23 C25 124.0(3) y
C22 C23 C25 125.7(4) y
C29 C25 C26 116.1(4) y
C29 C25 C23 123.1(4) y
C26 C25 C23 120.6(4) y
C27 C26 C25 120.7(4) y
C26 C27 C28 119.0(4) y
N9 C28 C27 121.3(4) y
N9 C28 C30 119.1(5) y
C27 C28 C30 119.6(4) y
N9 C29 C25 123.8(4) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 N2 2.060(3) y
Zn1 N3 2.061(3) y
Zn1 N1 2.069(4) y
Zn1 S1 2.2141(11) y
N1 C3 1.332(6) y
N1 N4 1.378(4) y
N2 C13 1.357(6) y
N2 N5 1.370(4) y
N3 C23 1.334(5) y
N3 N6 1.376(4) y
N4 C1 1.335(6) y
N4 B1 1.558(6) y
N5 C11 1.364(5) y
N5 B1 1.552(6) y
N6 C21 1.355(5) y
N6 B1 1.554(6) y
N7 C8 1.340(6) y
N7 C9 1.349(5) y
N8 C18 1.315(7) y
N8 C19 1.352(6) y
N9 C28 1.339(6) y
N9 C29 1.341(6) y
C1 C2 1.386(6) y
C1 C4 1.504(5) y
C2 C3 1.397(6) y
C3 C5 1.479(5) y
C5 C6 1.375(6) y
C5 C9 1.389(6) y
C6 C7 1.397(6) y
C7 C8 1.384(7) y
C8 C10 1.503(5) y
C11 C12 1.381(6) y
C11 C14 1.496(5) y
C12 C13 1.411(5) y
C13 C15 1.471(6) y
C15 C16 1.371(7) y
C15 C19 1.386(6) y
C16 C17 1.388(7) y
C17 C18 1.403(7) y
C18 C20 1.513(7) y
C21 C22 1.388(6) y
C21 C24 1.492(5) y
C22 C23 1.398(5) y
C23 C25 1.477(5) y
C25 C29 1.394(6) y
C25 C26 1.403(6) y
C26 C27 1.371(6) y
C27 C28 1.399(7) y
C28 C30 1.501(6) y
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2024-11-15T14:40:08+02:00
;
 Removed multiple data items that had the 'y' placeholder value.
;
