#------------------------------------------------------------------------------
#$Date: 2024-11-15 14:46:36 +0200 (Fri, 15 Nov 2024) $
#$Revision: 295934 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/05/4320579.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_4320579
loop_
_publ_author_name
'Udo Brand'
'Michael Rombach'
'Jan Seebacher'
'Heinrich Vahrenkamp'
_publ_section_title
;
 Functional Modeling of Cobalamine-Independent Methionine Synthase with
 Pyrazolylborate-Zinc-Thiolate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6151
_journal_page_last               6157
_journal_paper_doi               10.1021/ic0105112
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C34 H37 B N6 S Zn'
_chemical_formula_weight         637.94
_chemical_name_common            TpZnS2Bu
_chemical_name_systematic
;
 Hydrotris(5-methyl-3-phenylpyrazol-1-yl)borato)-zink-2-butylthiolat
;
_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                 99.350(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1782(16)
_cell_length_b                   11.1262(17)
_cell_length_c                   28.835(5)
_cell_measurement_temperature    171(2)
_cell_volume                     3222.0(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      171(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            28215
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       UNREGULAR
_exptl_crystal_F_000             1336
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0716P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1408
_reflns_number_gt                4783
_reflns_number_total             7725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0105112_1.cif
_cod_data_source_block           seebcm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'y' was changed to '?' - the value is
undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3222.1(9)
_cod_database_code               4320579
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.21628(3) 0.57129(3) 0.129417(12) 0.02996(12) Uani 1 1 d . . .
N1 N -0.0622(2) 0.6266(2) 0.13030(9) 0.0318(6) Uani 1 1 d . . .
N2 N 0.0137(2) 0.5448(2) 0.11033(9) 0.0314(6) Uani 1 1 d . . .
N3 N 0.0945(2) 0.6852(2) 0.20350(9) 0.0325(6) Uani 1 1 d . . .
N4 N 0.2017(2) 0.6119(2) 0.19898(9) 0.0305(5) Uani 1 1 d . . .
N5 N 0.0907(2) 0.8049(2) 0.12963(8) 0.0298(5) Uani 1 1 d . . .
N6 N 0.1912(2) 0.7511(2) 0.11075(8) 0.0289(5) Uani 1 1 d . . .
S1 S 0.37555(8) 0.45602(7) 0.10813(3) 0.0365(2) Uani 1 1 d . . .
B1 B 0.0038(3) 0.7333(3) 0.15900(12) 0.0315(8) Uani 1 1 d . . .
H1 H -0.0662 0.7869 0.1684 0.038 Uiso 1 1 calc R . .
C1 C -0.0734(3) 0.4647(3) 0.08730(11) 0.0334(7) Uani 1 1 d . . .
C2 C -0.2026(3) 0.4950(3) 0.09354(12) 0.0397(8) Uani 1 1 d . . .
H2A H -0.2819 0.4529 0.0814 0.048 Uiso 1 1 calc R . .
C3 C -0.1931(3) 0.5968(3) 0.12035(11) 0.0344(7) Uani 1 1 d . . .
C4 C -0.3006(3) 0.6680(3) 0.13700(13) 0.0435(8) Uani 1 1 d . . .
H4A H -0.2612 0.7362 0.1558 0.065 Uiso 1 1 calc R . .
H4B H -0.3486 0.6167 0.1563 0.065 Uiso 1 1 calc R . .
H4C H -0.3627 0.6977 0.1099 0.065 Uiso 1 1 calc R . .
C5 C -0.0330(3) 0.3673(3) 0.05792(12) 0.0375(7) Uani 1 1 d . . .
C6 C -0.1006(3) 0.2587(3) 0.05474(13) 0.0459(8) Uani 1 1 d . . .
H6A H -0.1680 0.2452 0.0734 0.055 Uiso 1 1 calc R . .
C7 C -0.0704(4) 0.1699(3) 0.02448(15) 0.0589(11) Uani 1 1 d . . .
H7A H -0.1168 0.0955 0.0227 0.071 Uiso 1 1 calc R . .
C8 C 0.0260(4) 0.1883(4) -0.00302(14) 0.0590(11) Uani 1 1 d . . .
H8A H 0.0456 0.1274 -0.0239 0.071 Uiso 1 1 calc R . .
C9 C 0.0936(4) 0.2952(4) -0.00006(13) 0.0549(10) Uani 1 1 d . . .
H9A H 0.1604 0.3082 -0.0190 0.066 Uiso 1 1 calc R . .
C10 C 0.0655(3) 0.3848(3) 0.03037(12) 0.0434(8) Uani 1 1 d . . .
H10A H 0.1137 0.4582 0.0324 0.052 Uiso 1 1 calc R . .
C11 C 0.2626(3) 0.5872(3) 0.24281(11) 0.0352(7) Uani 1 1 d . . .
C12 C 0.1940(3) 0.6432(3) 0.27510(12) 0.0459(9) Uani 1 1 d . . .
H12A H 0.2156 0.6396 0.3084 0.055 Uiso 1 1 calc R . .
C13 C 0.0894(3) 0.7046(3) 0.24952(12) 0.0421(8) Uani 1 1 d . . .
C14 C -0.0118(4) 0.7843(5) 0.26556(14) 0.0702(13) Uani 1 1 d . . .
H14A H -0.0723 0.8149 0.2382 0.105 Uiso 1 1 calc R . .
H14B H 0.0330 0.8519 0.2834 0.105 Uiso 1 1 calc R . .
H14C H -0.0626 0.7386 0.2857 0.105 Uiso 1 1 calc R . .
C15 C 0.3869(3) 0.5182(3) 0.25395(11) 0.0361(7) Uani 1 1 d . . .
C16 C 0.4014(4) 0.4355(3) 0.29058(12) 0.0454(8) Uani 1 1 d . . .
H16A H 0.3294 0.4210 0.3071 0.054 Uiso 1 1 calc R . .
C17 C 0.5195(4) 0.3745(3) 0.30302(14) 0.0540(10) Uani 1 1 d . . .
H17A H 0.5285 0.3183 0.3281 0.065 Uiso 1 1 calc R . .
C18 C 0.6242(4) 0.3942(3) 0.27948(14) 0.0541(10) Uani 1 1 d . . .
H18A H 0.7053 0.3515 0.2881 0.065 Uiso 1 1 calc R . .
C19 C 0.6112(4) 0.4761(4) 0.24335(14) 0.0549(10) Uani 1 1 d . . .
H19A H 0.6840 0.4904 0.2272 0.066 Uiso 1 1 calc R . .
C20 C 0.4931(3) 0.5377(3) 0.23038(13) 0.0454(9) Uani 1 1 d . . .
H20A H 0.4847 0.5937 0.2052 0.054 Uiso 1 1 calc R . .
C21 C 0.2524(3) 0.8373(3) 0.09012(10) 0.0323(7) Uani 1 1 d . . .
C22 C 0.1922(3) 0.9477(3) 0.09610(12) 0.0384(8) Uani 1 1 d . . .
H22A H 0.2161 1.0237 0.0850 0.046 Uiso 1 1 calc R . .
C23 C 0.0911(3) 0.9243(3) 0.12132(11) 0.0341(7) Uani 1 1 d . . .
C24 C -0.0055(4) 1.0086(3) 0.13806(14) 0.0505(9) Uani 1 1 d . . .
H24A H -0.0654 0.9633 0.1550 0.076 Uiso 1 1 calc R . .
H24B H -0.0577 1.0493 0.1110 0.076 Uiso 1 1 calc R . .
H24C H 0.0432 1.0685 0.1591 0.076 Uiso 1 1 calc R . .
C25 C 0.3627(3) 0.8130(3) 0.06432(11) 0.0397(8) Uani 1 1 d . . .
C26 C 0.4600(4) 0.9009(4) 0.06351(15) 0.0582(11) Uani 1 1 d . . .
H26A H 0.4579 0.9734 0.0808 0.070 Uiso 1 1 calc R . .
C27 C 0.5611(4) 0.8799(6) 0.03671(19) 0.0832(17) Uani 1 1 d . . .
H27A H 0.6271 0.9397 0.0355 0.100 Uiso 1 1 calc R . .
C28 C 0.5666(5) 0.7763(6) 0.01249(18) 0.0873(19) Uani 1 1 d . . .
H28A H 0.6363 0.7637 -0.0053 0.105 Uiso 1 1 calc R . .
C29 C 0.4716(5) 0.6898(5) 0.01364(14) 0.0746(15) Uani 1 1 d . . .
H29A H 0.4757 0.6172 -0.0034 0.090 Uiso 1 1 calc R . .
C30 C 0.3692(4) 0.7070(3) 0.03946(12) 0.0474(9) Uani 1 1 d . . .
H30A H 0.3038 0.6464 0.0401 0.057 Uiso 1 1 calc R . .
C31 C 0.2456(4) 0.2867(3) 0.15671(17) 0.0641(12) Uani 1 1 d . . .
H31A H 0.2567 0.2142 0.1762 0.096 Uiso 1 1 calc R . .
H31B H 0.1803 0.2712 0.1284 0.096 Uiso 1 1 calc R . .
H31C H 0.2142 0.3528 0.1745 0.096 Uiso 1 1 calc R . .
C32 C 0.3737(5) 0.3195(4) 0.1431(2) 0.0861(17) Uani 1 1 d . . .
H32A H 0.4269 0.3443 0.1739 0.103 Uiso 1 1 calc R . .
C33 C 0.4500(5) 0.2210(4) 0.1300(2) 0.100(2) Uani 1 1 d . . .
H33A H 0.4667 0.1678 0.1578 0.120 Uiso 1 1 calc R . .
H33B H 0.3896 0.1762 0.1056 0.120 Uiso 1 1 calc R . .
C34 C 0.5703(5) 0.2293(4) 0.11354(19) 0.0820(14) Uani 1 1 d . . .
H34A H 0.5985 0.1491 0.1052 0.123 Uiso 1 1 calc R . .
H34B H 0.6378 0.2636 0.1381 0.123 Uiso 1 1 calc R . .
H34C H 0.5597 0.2812 0.0857 0.123 Uiso 1 1 calc 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Zn1 N6 89.60(9) . . y
N2 Zn1 N4 93.61(10) . . y
N6 Zn1 N4 90.90(10) . . y
N2 Zn1 S1 125.67(7) . . y
N6 Zn1 S1 123.16(7) . . y
N4 Zn1 S1 123.92(7) . . y
C3 N1 N2 110.4(2) . . y
C3 N1 B1 129.1(3) . . y
N2 N1 B1 120.5(2) . . y
C1 N2 N1 105.8(2) . . y
C1 N2 Zn1 140.4(2) . . y
N1 N2 Zn1 113.41(17) . . y
C13 N3 N4 110.0(2) . . y
C13 N3 B1 130.1(3) . . y
N4 N3 B1 119.8(2) . . y
C11 N4 N3 106.4(2) . . y
C11 N4 Zn1 140.1(2) . . y
N3 N4 Zn1 113.49(17) . . y
C23 N5 N6 109.6(2) . . y
C23 N5 B1 128.7(3) . . y
N6 N5 B1 121.6(2) . . y
C21 N6 N5 107.2(2) . . y
C21 N6 Zn1 139.5(2) . . y
N5 N6 Zn1 112.70(17) . . y
C32 S1 Zn1 104.67(13) . . y
N1 B1 N5 110.1(3) . . y
N1 B1 N3 109.2(2) . . y
N5 B1 N3 108.4(2) . . y
N2 C1 C2 109.5(3) . . y
N2 C1 C5 123.0(3) . . y
C2 C1 C5 127.4(3) . . y
C3 C2 C1 107.0(3) . . y
N1 C3 C2 107.4(3) . . y
N1 C3 C4 123.3(3) . . y
C2 C3 C4 129.4(3) . . y
C6 C5 C10 118.8(3) . . y
C6 C5 C1 119.8(3) . . y
C10 C5 C1 121.3(3) . . y
C5 C6 C7 120.3(4) . . y
C8 C7 C6 120.7(4) . . y
C7 C8 C9 119.5(4) . . y
C8 C9 C10 120.6(4) . . y
C9 C10 C5 120.2(3) . . y
N4 C11 C12 109.4(3) . . y
N4 C11 C15 124.2(3) . . y
C12 C11 C15 126.3(3) . . y
C13 C12 C11 106.9(3) . . y
N3 C13 C12 107.3(3) . . y
N3 C13 C14 122.6(3) . . y
C12 C13 C14 130.1(3) . . y
C20 C15 C16 118.8(3) . . y
C20 C15 C11 121.6(3) . . y
C16 C15 C11 119.5(3) . . y
C17 C16 C15 120.3(4) . . y
C18 C17 C16 120.6(3) . . y
C17 C18 C19 119.7(3) . . y
C18 C19 C20 120.4(4) . . y
C19 C20 C15 120.3(3) . . y
N6 C21 C22 109.3(3) . . y
N6 C21 C25 122.9(3) . . y
C22 C21 C25 127.7(3) . . y
C23 C22 C21 106.2(3) . . y
N5 C23 C22 107.7(3) . . y
N5 C23 C24 122.6(3) . . y
C22 C23 C24 129.7(3) . . y
C30 C25 C26 119.6(3) . . y
C30 C25 C21 121.5(3) . . y
C26 C25 C21 118.8(3) . . y
C25 C26 C27 118.6(5) . . y
C28 C27 C26 121.4(5) . . y
C27 C28 C29 119.9(4) . . y
C28 C29 C30 120.7(5) . . y
C25 C30 C29 119.8(4) . . y
C33 C32 C31 115.2(4) . . y
C33 C32 S1 115.9(3) . . y
C31 C32 S1 116.4(3) . . y
C34 C33 C32 126.0(5) . . 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 N2 2.067(2) . y
Zn1 N6 2.077(2) . y
Zn1 N4 2.085(3) . y
Zn1 S1 2.2300(9) . y
N1 C3 1.358(4) . y
N1 N2 1.379(3) . y
N1 B1 1.538(4) . y
N2 C1 1.353(4) . y
N3 C13 1.354(4) . y
N3 N4 1.385(3) . y
N3 B1 1.549(4) . y
N4 C11 1.343(4) . y
N5 C23 1.350(4) . y
N5 N6 1.371(3) . y
N5 B1 1.542(4) . y
N6 C21 1.335(4) . y
S1 C32 1.826(4) . y
C1 C2 1.397(4) . y
C1 C5 1.475(4) . y
C2 C3 1.366(4) . y
C3 C4 1.492(4) . y
C5 C6 1.386(4) . y
C5 C10 1.390(5) . y
C6 C7 1.386(5) . y
C7 C8 1.373(6) . y
C8 C9 1.370(6) . y
C9 C10 1.388(5) . y
C11 C12 1.398(5) . y
C11 C15 1.470(4) . y
C12 C13 1.374(5) . y
C13 C14 1.489(5) . y
C15 C20 1.384(5) . y
C15 C16 1.391(4) . y
C16 C17 1.376(5) . y
C17 C18 1.371(5) . y
C18 C19 1.374(5) . y
C19 C20 1.382(5) . y
C21 C22 1.396(4) . y
C21 C25 1.469(4) . y
C22 C23 1.378(4) . y
C23 C24 1.495(4) . y
C25 C30 1.387(5) . y
C25 C26 1.395(5) . y
C26 C27 1.403(6) . y
C27 C28 1.353(7) . y
C28 C29 1.369(7) . y
C29 C30 1.389(5) . y
C31 C32 1.467(5) . y
C32 C33 1.429(6) . y
C33 C34 1.386(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.
;
