#------------------------------------------------------------------------------
#$Date: 2024-11-15 14:46:36 +0200 (Fri, 15 Nov 2024) $
#$Revision: 295934 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/15/4311572.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_4311572
loop_
_publ_author_name
'Horst Brombacher'
'Heinrich Vahrenkamp'
_publ_section_title
;
 Pyrazolylborate-Zinc Alkoxide Complexes. 3. Acid-Base Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6054
_journal_page_last               6060
_journal_paper_doi               10.1021/ic049177a
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C39 H35 B N8 O3 S Zn'
_chemical_formula_weight         771.99
_chemical_melting_point          240
_chemical_name_common            Tp(Ph,Me)Zn-o-Benzoesäuresulfimid
_chemical_name_systematic
; 
 Hydrotris(3-phenyl-5-methylpyrazol-1-yl)borato-zink-o-Benzoesäuresulfimid 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.358(2)
_cell_angle_beta                 106.553(2)
_cell_angle_gamma                92.744(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6821(10)
_cell_length_b                   12.2344(11)
_cell_length_c                   13.2961(11)
_cell_measurement_temperature    210(2)
_cell_volume                     1816.5(3)
_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      210(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_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  0.0778
_diffrn_reflns_av_sigmaI/netI    0.1685
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17001
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.716
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         8663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.1794
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1207P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1813
_refine_ls_wR_factor_ref         0.2490
_reflns_number_gt                3471
_reflns_number_total             8663
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049177asi20040706_093708_5.cif
_cod_data_source_block           brombmm
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (95
times).

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (61 time).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4311572
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.53063(6) 0.80133(6) 0.71621(6) 0.0332(2) Uani 1 1 d . . .
N1 N 0.4565(4) 0.8192(4) 0.5602(4) 0.0330(12) Uani 1 1 d . . .
N2 N 0.3966(4) 0.6890(4) 0.7180(4) 0.0337(12) Uani 1 1 d . . .
N3 N 0.4590(4) 0.9374(4) 0.7547(4) 0.0328(12) Uani 1 1 d . . .
N4 N 0.3373(4) 0.8384(4) 0.5389(4) 0.0363(12) Uani 1 1 d . . .
N5 N 0.2857(4) 0.7317(4) 0.6803(4) 0.0324(12) Uani 1 1 d . . .
N6 N 0.3368(4) 0.9355(4) 0.7096(4) 0.0353(12) Uani 1 1 d . . .
N7 N 0.6852(4) 0.7666(4) 0.8102(4) 0.0308(12) Uani 1 1 d . . .
N8 N 0.9263(8) 0.4070(7) 0.6094(7) 0.091(3) Uani 1 1 d . . .
O1 O 0.5935(4) 0.7706(4) 0.9410(3) 0.0439(12) Uani 1 1 d . . .
O2 O 0.7995(4) 0.6478(4) 0.7166(4) 0.0463(12) Uani 1 1 d . . .
O3 O 0.8777(4) 0.8345(4) 0.7771(3) 0.0398(11) Uani 1 1 d . . .
S1 S 0.81393(13) 0.73744(13) 0.79330(13) 0.0350(4) Uani 1 1 d . . .
B1 B 0.2738(6) 0.8436(6) 0.6282(5) 0.0292(15) Uani 1 1 d . . .
H1 H 0.1883 0.8577 0.5984 0.035 Uiso 1 1 calc R . .
C1 C 0.2889(6) 0.8447(5) 0.4338(5) 0.0396(16) Uani 1 1 d . . .
C2 C 0.3783(6) 0.8297(5) 0.3878(5) 0.0403(16) Uani 1 1 d . . .
H2B H 0.3712 0.8295 0.3156 0.048 Uiso 1 1 calc R . .
C3 C 0.4811(5) 0.8149(5) 0.4678(5) 0.0344(14) Uani 1 1 d . . .
C4 C 0.1611(6) 0.8679(6) 0.3836(5) 0.0489(18) Uani 1 1 d . . .
H4A H 0.1198 0.8741 0.4372 0.073 Uiso 1 1 calc R . .
H4B H 0.1227 0.8085 0.3328 0.073 Uiso 1 1 calc R . .
H4C H 0.1581 0.9360 0.3484 0.073 Uiso 1 1 calc R . .
C5 C 0.6019(5) 0.7960(5) 0.4595(5) 0.0317(14) Uani 1 1 d . . .
C6 C 0.6141(6) 0.7314(6) 0.3748(5) 0.0433(17) Uani 1 1 d . . .
H6A H 0.5455 0.7018 0.3231 0.052 Uiso 1 1 calc R . .
C7 C 0.7262(6) 0.7106(6) 0.3663(6) 0.0472(18) Uani 1 1 d . . .
H7A H 0.7335 0.6659 0.3095 0.057 Uiso 1 1 calc R . .
C8 C 0.8272(6) 0.7551(6) 0.4404(6) 0.0456(17) Uani 1 1 d . . .
H8A H 0.9034 0.7404 0.4346 0.055 Uiso 1 1 calc R . .
C9 C 0.8162(6) 0.8217(6) 0.5237(6) 0.0504(19) Uani 1 1 d . . .
H9A H 0.8850 0.8529 0.5742 0.061 Uiso 1 1 calc R . .
C10 C 0.7046(6) 0.8421(5) 0.5321(5) 0.0409(16) Uani 1 1 d . . .
H10A H 0.6977 0.8882 0.5882 0.049 Uiso 1 1 calc R . .
C11 C 0.2024(5) 0.6651(5) 0.7028(5) 0.0354(15) Uani 1 1 d . . .
C12 C 0.2573(6) 0.5783(5) 0.7530(5) 0.0385(16) Uani 1 1 d . . .
H12A H 0.2205 0.5190 0.7772 0.046 Uiso 1 1 calc R . .
C13 C 0.3784(5) 0.5949(5) 0.7613(5) 0.0320(14) Uani 1 1 d . . .
C14 C 0.0722(5) 0.6859(6) 0.6704(6) 0.0474(18) Uani 1 1 d . . .
H14A H 0.0606 0.7543 0.6356 0.071 Uiso 1 1 calc R . .
H14B H 0.0436 0.6905 0.7321 0.071 Uiso 1 1 calc R . .
H14C H 0.0279 0.6264 0.6226 0.071 Uiso 1 1 calc R . .
C15 C 0.4747(5) 0.5214(5) 0.8010(5) 0.0341(14) Uani 1 1 d . . .
C16 C 0.5713(5) 0.5150(5) 0.7607(5) 0.0355(15) Uani 1 1 d . . .
H16A H 0.5774 0.5614 0.7075 0.043 Uiso 1 1 calc R . .
C17 C 0.6597(6) 0.4418(5) 0.7968(5) 0.0408(16) Uani 1 1 d . . .
H17A H 0.7260 0.4407 0.7701 0.049 Uiso 1 1 calc R . .
C18 C 0.6488(6) 0.3708(6) 0.8724(5) 0.0457(17) Uani 1 1 d . . .
H18A H 0.7069 0.3199 0.8962 0.055 Uiso 1 1 calc R . .
C19 C 0.5519(6) 0.3751(5) 0.9128(5) 0.0415(16) Uani 1 1 d . . .
H19A H 0.5444 0.3268 0.9641 0.050 Uiso 1 1 calc R . .
C20 C 0.4666(6) 0.4496(5) 0.8783(5) 0.0378(15) Uani 1 1 d . . .
H20A H 0.4020 0.4523 0.9071 0.045 Uiso 1 1 calc R . .
C21 C 0.2913(6) 1.0180(5) 0.7534(5) 0.0369(15) Uani 1 1 d . . .
C22 C 0.3841(6) 1.0765(5) 0.8259(5) 0.0398(16) Uani 1 1 d . . .
H22A H 0.3784 1.1389 0.8675 0.048 Uiso 1 1 calc R . .
C23 C 0.4886(5) 1.0250(5) 0.8259(5) 0.0330(14) Uani 1 1 d . . .
C24 C 0.1602(6) 1.0350(6) 0.7251(6) 0.0483(18) Uani 1 1 d . . .
H24A H 0.1173 0.9805 0.6707 0.073 Uiso 1 1 calc R . .
H24B H 0.1461 1.1077 0.6996 0.073 Uiso 1 1 calc R . .
H24C H 0.1323 1.0278 0.7868 0.073 Uiso 1 1 calc R . .
C25 C 0.6121(5) 1.0537(5) 0.8905(5) 0.0319(14) Uani 1 1 d . . .
C26 C 0.7106(6) 1.0284(5) 0.8567(5) 0.0367(15) Uani 1 1 d . . .
H26A H 0.6988 0.9945 0.7894 0.044 Uiso 1 1 calc R . .
C27 C 0.8253(6) 1.0525(5) 0.9208(6) 0.0442(17) Uani 1 1 d . . .
H27A H 0.8914 1.0335 0.8983 0.053 Uiso 1 1 calc R . .
C28 C 0.8426(7) 1.1050(6) 1.0187(6) 0.0496(19) Uani 1 1 d . . .
H28A H 0.9207 1.1212 1.0627 0.059 Uiso 1 1 calc R . .
C29 C 0.7467(7) 1.1336(6) 1.0519(6) 0.0495(19) Uani 1 1 d . . .
H29A H 0.7593 1.1712 1.1176 0.059 Uiso 1 1 calc R . .
C30 C 0.6307(6) 1.1072(5) 0.9885(5) 0.0376(15) Uani 1 1 d . . .
H30A H 0.5650 1.1254 1.0121 0.045 Uiso 1 1 calc R . .
C31 C 0.8748(5) 0.6958(5) 0.9221(6) 0.0406(16) Uani 1 1 d . . .
C32 C 0.9850(6) 0.6569(6) 0.9670(7) 0.056(2) Uani 1 1 d . . .
H32A H 1.0402 0.6459 0.9286 0.068 Uiso 1 1 calc R . .
C33 C 1.0101(7) 0.6346(7) 1.0729(7) 0.068(3) Uani 1 1 d . . .
H33A H 1.0841 0.6064 1.1061 0.081 Uiso 1 1 calc R . .
C34 C 0.9319(7) 0.6520(7) 1.1307(7) 0.067(2) Uani 1 1 d . . .
H34A H 0.9528 0.6365 1.2021 0.080 Uiso 1 1 calc R . .
C35 C 0.8225(7) 0.6921(6) 1.0840(6) 0.0523(19) Uani 1 1 d . . .
H35A H 0.7681 0.7048 1.1228 0.063 Uiso 1 1 calc R . .
C36 C 0.7943(5) 0.7134(5) 0.9784(5) 0.0403(16) Uani 1 1 d . . .
C37 C 0.6815(5) 0.7541(5) 0.9122(5) 0.0330(14) Uani 1 1 d . . .
C38 C 0.7129(8) 0.4681(7) 0.5227(6) 0.072(3) Uani 1 1 d . . .
H38A H 0.7095 0.4949 0.4543 0.108 Uiso 1 1 calc R . .
H38B H 0.6942 0.5259 0.5664 0.108 Uiso 1 1 calc R . .
H38C H 0.6553 0.4061 0.5143 0.108 Uiso 1 1 calc R . .
C39 C 0.8321(9) 0.4341(7) 0.5721(6) 0.060(2) Uani 1 1 d . . .
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'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 Zn1 N3 116.9(2) . . y
N7 Zn1 N1 138.0(2) . . y
N3 Zn1 N1 91.8(2) . . y
N7 Zn1 N2 112.2(2) . . y
N3 Zn1 N2 98.9(2) . . y
N1 Zn1 N2 91.0(2) . . y
C3 N1 N4 106.5(5) . . y
C3 N1 Zn1 142.4(4) . . y
N4 N1 Zn1 111.0(4) . . y
C13 N2 N5 106.7(5) . . y
C13 N2 Zn1 140.7(4) . . y
N5 N2 Zn1 110.9(4) . . y
C23 N3 N6 106.7(5) . . y
C23 N3 Zn1 139.4(4) . . y
N6 N3 Zn1 112.7(4) . . y
C1 N4 N1 109.7(5) . . y
C1 N4 B1 128.8(5) . . y
N1 N4 B1 121.4(5) . . y
C11 N5 N2 109.0(5) . . y
C11 N5 B1 130.2(5) . . y
N2 N5 B1 120.7(5) . . y
C21 N6 N3 109.6(5) . . y
C21 N6 B1 130.3(5) . . y
N3 N6 B1 119.9(5) . . y
C37 N7 S1 112.6(4) . . y
C37 N7 Zn1 112.7(4) . . y
S1 N7 Zn1 134.4(3) . . y
O3 S1 O2 116.5(3) . . y
O3 S1 N7 110.5(3) . . y
O2 S1 N7 111.1(3) . . y
O3 S1 C31 110.3(3) . . y
O2 S1 C31 111.5(3) . . y
N7 S1 C31 94.9(3) . . y
N6 B1 N5 109.8(5) . . y
N6 B1 N4 108.7(5) . . y
N5 B1 N4 107.8(5) . . y
N4 C1 C2 107.2(5) . . y
N4 C1 C4 123.7(6) . . y
C2 C1 C4 129.0(6) . . y
C1 C2 C3 107.0(6) . . y
N1 C3 C2 109.6(6) . . y
N1 C3 C5 122.1(5) . . y
C2 C3 C5 128.3(6) . . y
C10 C5 C6 118.4(6) . . y
C10 C5 C3 122.3(6) . . y
C6 C5 C3 119.3(6) . . y
C7 C6 C5 120.5(6) . . y
C8 C7 C6 120.3(7) . . y
C7 C8 C9 119.8(6) . . y
C10 C9 C8 119.8(7) . . y
C9 C10 C5 121.2(6) . . y
N5 C11 C12 108.5(5) . . y
N5 C11 C14 122.7(6) . . y
C12 C11 C14 128.7(6) . . y
C11 C12 C13 106.6(6) . . y
N2 C13 C12 109.2(5) . . y
N2 C13 C15 122.2(5) . . y
C12 C13 C15 128.5(6) . . y
C16 C15 C20 117.8(6) . . y
C16 C15 C13 122.6(6) . . y
C20 C15 C13 119.6(6) . . y
C15 C16 C17 121.8(6) . . y
C18 C17 C16 119.3(6) . . y
C17 C18 C19 119.8(6) . . y
C20 C19 C18 120.4(7) . . y
C19 C20 C15 121.0(6) . . y
N6 C21 C22 108.3(5) . . y
N6 C21 C24 122.7(6) . . y
C22 C21 C24 128.9(6) . . y
C21 C22 C23 106.7(6) . . y
N3 C23 C22 108.6(5) . . y
N3 C23 C25 122.7(5) . . y
C22 C23 C25 128.7(6) . . y
C30 C25 C26 119.2(6) . . y
C30 C25 C23 118.7(6) . . y
C26 C25 C23 122.1(6) . . y
C27 C26 C25 120.6(6) . . y
C26 C27 C28 119.6(7) . . y
C29 C28 C27 120.5(7) . . y
C28 C29 C30 120.2(7) . . y
C25 C30 C29 119.9(6) . . y
C32 C31 C36 122.2(7) . . y
C32 C31 S1 129.0(6) . . y
C36 C31 S1 108.7(4) . . y
C31 C32 C33 116.0(7) . . y
C34 C33 C32 122.9(7) . . y
C33 C34 C35 119.8(7) . . y
C34 C35 C36 118.5(8) . . y
C31 C36 C35 120.6(6) . . y
C31 C36 C37 111.9(6) . . y
C35 C36 C37 127.5(7) . . y
O1 C37 N7 123.1(6) . . y
O1 C37 C36 125.2(6) . . y
N7 C37 C36 111.7(6) . . y
N8 C39 C38 178.9(10) . . y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N7 1.958(5) . y
Zn1 N3 2.010(5) . y
Zn1 N1 2.032(5) . y
Zn1 N2 2.040(5) . y
N1 C3 1.339(7) . y
N1 N4 1.374(6) . y
N2 C13 1.343(7) . y
N2 N5 1.386(6) . y
N3 C23 1.365(7) . y
N3 N6 1.380(6) . y
N4 C1 1.357(8) . y
N4 B1 1.570(8) . y
N5 C11 1.345(7) . y
N5 B1 1.554(8) . y
N6 C21 1.350(8) . y
N6 B1 1.530(8) . y
N7 C37 1.383(7) . y
N7 S1 1.637(5) . y
N8 C39 1.142(11) . y
O1 C37 1.218(7) . y
O2 S1 1.437(4) . y
O3 S1 1.428(4) . y
S1 C31 1.764(7) . y
C1 C2 1.368(9) . y
C1 C4 1.497(9) . y
C2 C3 1.384(8) . y
C3 C5 1.475(8) . y
C5 C10 1.386(8) . y
C5 C6 1.394(8) . y
C6 C7 1.381(9) . y
C7 C8 1.375(9) . y
C8 C9 1.388(10) . y
C9 C10 1.374(9) . y
C11 C12 1.365(8) . y
C11 C14 1.496(8) . y
C12 C13 1.392(8) . y
C13 C15 1.466(8) . y
C15 C16 1.385(8) . y
C15 C20 1.399(8) . y
C16 C17 1.393(8) . y
C17 C18 1.384(9) . y
C18 C19 1.388(9) . y
C19 C20 1.377(8) . y
C21 C22 1.374(9) . y
C21 C24 1.496(8) . y
C22 C23 1.401(8) . y
C23 C25 1.470(8) . y
C25 C30 1.388(8) . y
C25 C26 1.393(8) . y
C26 C27 1.378(9) . y
C27 C28 1.383(10) . y
C28 C29 1.371(10) . y
C29 C30 1.391(9) . y
C31 C32 1.372(9) . y
C31 C36 1.378(9) . y
C32 C33 1.396(11) . y
C33 C34 1.370(12) . y
C34 C35 1.376(10) . y
C35 C36 1.386(9) . y
C36 C37 1.483(8) . y
C38 C39 1.448(12) . 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.
;
