#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:50:54 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179818 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/14/7011442.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_7011442
loop_
_publ_author_name
'White, Jennifer L.'
'Tanski, Joseph M.'
'Rabinovich, Daniel'
_publ_section_title
;
 Bulky tris(mercaptoimidazolyl)borates: synthesis and molecular
 structures of the Group 12 metal complexes [TmtBu]MBr (M = Zn, Cd, Hg)
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2987
_journal_paper_doi               10.1039/b111558h
_journal_year                    2002
_chemical_formula_sum            'C23 H37 B Br N7 S3 Zn'
_chemical_formula_weight         663.87
_chemical_name_systematic
; 
? 
;
_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                 109.407(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6992(8)
_cell_length_b                   33.035(3)
_cell_length_c                   10.2817(8)
_cell_measurement_temperature    238(2)
_cell_volume                     3107.2(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      238(2)
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.901
_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  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            20156
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    2.303
_exptl_absorpt_correction_T_max  0.8024
_exptl_absorpt_correction_T_min  0.6559
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.735
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         6938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.735
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0400P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                6016
_reflns_number_total             6938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b111558h.txt
_cod_data_source_block           danzns20
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3107.2(4)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7011442
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
Zn Zn 0.17567(3) 0.126240(9) 0.42519(3) 0.03068(11) Uani 1 1 d . . .
Br Br 0.04004(3) 0.160209(10) 0.54623(4) 0.05098(12) Uani 1 1 d . . .
B B 0.4123(3) 0.07476(10) 0.2780(3) 0.0353(7) Uani 1 1 d . . .
S1 S 0.33217(7) 0.170745(19) 0.36253(7) 0.03059(15) Uani 1 1 d . . .
S2 S 0.33076(7) 0.07883(2) 0.57736(7) 0.03464(17) Uani 1 1 d . . .
S3 S 0.04404(7) 0.09211(2) 0.22009(8) 0.03790(17) Uani 1 1 d . . .
N11 N 0.3502(2) 0.11111(7) 0.1816(2) 0.0345(5) Uani 1 1 d . . .
N12 N 0.2543(3) 0.16801(7) 0.0790(2) 0.0347(5) Uani 1 1 d . . .
N21 N 0.5111(2) 0.08849(6) 0.4238(2) 0.0312(5) Uani 1 1 d . . .
N22 N 0.6060(2) 0.11170(7) 0.6349(2) 0.0337(5) Uani 1 1 d . . .
N31 N 0.2901(2) 0.04419(7) 0.2817(2) 0.0331(5) Uani 1 1 d . . .
N32 N 0.0907(2) 0.01012(7) 0.2672(2) 0.0327(5) Uani 1 1 d . . .
C11 C 0.3118(3) 0.14951(8) 0.2034(3) 0.0296(5) Uani 1 1 d . . .
C12 C 0.3145(3) 0.10595(10) 0.0413(3) 0.0432(7) Uani 1 1 d . . .
H12A H 0.3298 0.0823 -0.0027 0.052 Uiso 1 1 calc R . .
C13 C 0.2542(4) 0.14043(10) -0.0224(3) 0.0440(7) Uani 1 1 d . . .
H13A H 0.2186 0.1449 -0.1181 0.053 Uiso 1 1 calc R . .
C14 C 0.1932(3) 0.21038(8) 0.0514(3) 0.0377(6) Uani 1 1 d . . .
C15 C 0.1416(4) 0.21808(11) -0.1032(3) 0.0597(9) Uani 1 1 d . . .
H15A H 0.0644 0.1991 -0.1491 0.089 Uiso 1 1 calc R . .
H15B H 0.2228 0.2145 -0.1374 0.089 Uiso 1 1 calc R . .
H15C H 0.1048 0.2455 -0.1217 0.089 Uiso 1 1 calc R . .
C16 C 0.3140(3) 0.24082(9) 0.1218(4) 0.0476(8) Uani 1 1 d . . .
H16A H 0.3487 0.2361 0.2205 0.071 Uiso 1 1 calc R . .
H16B H 0.2755 0.2681 0.1033 0.071 Uiso 1 1 calc R . .
H16C H 0.3943 0.2376 0.0863 0.071 Uiso 1 1 calc R . .
C17 C 0.0630(3) 0.21407(10) 0.1022(3) 0.0464(7) Uani 1 1 d . . .
H17A H 0.0949 0.2095 0.2009 0.070 Uiso 1 1 calc R . .
H17B H -0.0103 0.1941 0.0560 0.070 Uiso 1 1 calc R . .
H17C H 0.0213 0.2410 0.0820 0.070 Uiso 1 1 calc R . .
C21 C 0.4871(3) 0.09334(8) 0.5444(3) 0.0295(5) Uani 1 1 d . . .
C22 C 0.6474(3) 0.10425(9) 0.4383(3) 0.0391(7) Uani 1 1 d . . .
H22A H 0.6918 0.1048 0.3697 0.047 Uiso 1 1 calc R . .
C23 C 0.7053(3) 0.11853(8) 0.5669(3) 0.0399(7) Uani 1 1 d . . .
H23A H 0.7971 0.1310 0.6043 0.048 Uiso 1 1 calc R . .
C24 C 0.6230(3) 0.12780(10) 0.7770(3) 0.0437(7) Uani 1 1 d . . .
C25 C 0.5113(4) 0.16103(11) 0.7650(4) 0.0567(9) Uani 1 1 d . . .
H25A H 0.5256 0.1825 0.7064 0.085 Uiso 1 1 calc R . .
H25B H 0.5233 0.1718 0.8558 0.085 Uiso 1 1 calc R . .
H25C H 0.4136 0.1500 0.7251 0.085 Uiso 1 1 calc R . .
C26 C 0.7772(4) 0.14526(15) 0.8402(5) 0.0772(13) Uani 1 1 d . . .
H26A H 0.7902 0.1675 0.7836 0.116 Uiso 1 1 calc R . .
H26B H 0.8487 0.1243 0.8445 0.116 Uiso 1 1 calc R . .
H26C H 0.7904 0.1551 0.9325 0.116 Uiso 1 1 calc R . .
C27 C 0.6058(4) 0.09308(12) 0.8690(3) 0.0582(9) Uani 1 1 d . . .
H27A H 0.5085 0.0817 0.8309 0.087 Uiso 1 1 calc R . .
H27B H 0.6202 0.1033 0.9610 0.087 Uiso 1 1 calc R . .
H27C H 0.6779 0.0723 0.8732 0.087 Uiso 1 1 calc R . .
C31 C 0.1439(3) 0.04785(8) 0.2555(3) 0.0311(5) Uani 1 1 d . . .
C32 C 0.3280(3) 0.00427(8) 0.3133(3) 0.0407(7) Uani 1 1 d . . .
H32A H 0.4229 -0.0065 0.3369 0.049 Uiso 1 1 calc R . .
C33 C 0.2069(3) -0.01668(8) 0.3049(3) 0.0397(6) Uani 1 1 d . . .
H33A H 0.2019 -0.0445 0.3215 0.048 Uiso 1 1 calc R . .
C34 C -0.0676(3) -0.00207(9) 0.2356(3) 0.0360(6) Uani 1 1 d . . .
C35 C -0.1493(3) 0.00676(12) 0.0825(3) 0.0528(9) Uani 1 1 d . . .
H35A H -0.1043 -0.0083 0.0261 0.079 Uiso 1 1 calc R . .
H35B H -0.1445 0.0355 0.0652 0.079 Uiso 1 1 calc R . .
H35C H -0.2507 -0.0014 0.0595 0.079 Uiso 1 1 calc R . .
C36 C -0.1365(4) 0.02050(11) 0.3274(3) 0.0518(8) Uani 1 1 d . . .
H36A H -0.0831 0.0144 0.4233 0.078 Uiso 1 1 calc R . .
H36B H -0.2375 0.0121 0.3055 0.078 Uiso 1 1 calc R . .
H36C H -0.1328 0.0494 0.3120 0.078 Uiso 1 1 calc R . .
C37 C -0.0736(4) -0.04740(9) 0.2596(3) 0.0469(7) Uani 1 1 d . . .
H37A H -0.0225 -0.0534 0.3560 0.070 Uiso 1 1 calc R . .
H37B H -0.0274 -0.0618 0.2028 0.070 Uiso 1 1 calc R . .
H37C H -0.1747 -0.0559 0.2354 0.070 Uiso 1 1 calc R . .
H1 H 0.486(3) 0.0600(9) 0.227(3) 0.039(8) Uiso 1 1 d . . .
C2S C 0.7027(6) 0.22153(19) 0.3692(7) 0.1045(18) Uani 1 1 d . . .
C1S C 0.6944(8) 0.2055(4) 0.2424(11) 0.196(5) Uani 1 1 d . . .
N1S N 0.6865(12) 0.1918(7) 0.1398(11) 0.410(12) 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'
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'
Br Br -0.2901 2.4595 '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
S1 Zn S3 105.12(3) . . ?
S1 Zn S2 105.58(2) . . ?
S3 Zn S2 108.13(3) . . ?
S1 Zn Br 111.65(2) . . ?
S3 Zn Br 117.75(2) . . ?
S2 Zn Br 107.93(2) . . ?
N11 B N21 112.1(2) . . ?
N11 B N31 112.3(2) . . ?
N21 B N31 113.2(2) . . ?
C11 S1 Zn 97.13(9) . . ?
C21 S2 Zn 95.36(9) . . ?
C31 S3 Zn 96.74(9) . . ?
C11 N11 C12 107.5(2) . . ?
C11 N11 B 133.4(2) . . ?
C12 N11 B 118.9(2) . . ?
C11 N12 C13 108.1(2) . . ?
C11 N12 C14 127.4(2) . . ?
C13 N12 C14 124.5(2) . . ?
C21 N21 C22 107.9(2) . . ?
C21 N21 B 133.1(2) . . ?
C22 N21 B 118.4(2) . . ?
C21 N22 C23 107.6(2) . . ?
C21 N22 C24 127.8(2) . . ?
C23 N22 C24 124.1(2) . . ?
C31 N31 C32 108.1(2) . . ?
C31 N31 B 133.3(2) . . ?
C32 N31 B 118.5(2) . . ?
C31 N32 C33 108.1(2) . . ?
C31 N32 C34 127.4(2) . . ?
C33 N32 C34 124.3(2) . . ?
N12 C11 N11 108.2(2) . . ?
N12 C11 S1 126.2(2) . . ?
N11 C11 S1 125.6(2) . . ?
C13 C12 N11 108.8(3) . . ?
C12 C13 N12 107.4(3) . . ?
N12 C14 C15 108.9(2) . . ?
N12 C14 C17 109.2(2) . . ?
C15 C14 C17 108.8(3) . . ?
N12 C14 C16 109.2(2) . . ?
C15 C14 C16 108.6(3) . . ?
C17 C14 C16 112.1(3) . . ?
N21 C21 N22 108.4(2) . . ?
N21 C21 S2 125.41(19) . . ?
N22 C21 S2 126.1(2) . . ?
C23 C22 N21 108.1(2) . . ?
C22 C23 N22 107.9(2) . . ?
N22 C24 C25 109.3(3) . . ?
N22 C24 C27 109.5(3) . . ?
C25 C24 C27 111.7(3) . . ?
N22 C24 C26 108.7(3) . . ?
C25 C24 C26 109.4(3) . . ?
C27 C24 C26 108.1(3) . . ?
N31 C31 N32 107.5(2) . . ?
N31 C31 S3 126.4(2) . . ?
N32 C31 S3 126.1(2) . . ?
C33 C32 N31 108.6(2) . . ?
C32 C33 N32 107.6(2) . . ?
N32 C34 C36 111.1(2) . . ?
N32 C34 C37 108.5(2) . . ?
C36 C34 C37 109.5(3) . . ?
N32 C34 C35 108.1(2) . . ?
C36 C34 C35 111.1(3) . . ?
C37 C34 C35 108.6(2) . . ?
N1S C1S C2S 178.7(19) . . ?
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
Zn S1 2.3517(7) . ?
Zn S3 2.3578(8) . ?
Zn S2 2.3663(8) . ?
Zn Br 2.3720(4) . ?
B N11 1.546(4) . ?
B N21 1.554(4) . ?
B N31 1.567(4) . ?
S1 C11 1.730(3) . ?
S2 C21 1.728(2) . ?
S3 C31 1.724(3) . ?
N11 C11 1.362(3) . ?
N11 C12 1.377(3) . ?
N12 C11 1.359(3) . ?
N12 C13 1.384(4) . ?
N12 C14 1.510(4) . ?
N21 C21 1.345(3) . ?
N21 C22 1.382(3) . ?
N22 C21 1.360(3) . ?
N22 C23 1.384(3) . ?
N22 C24 1.511(4) . ?
N31 C31 1.358(3) . ?
N31 C32 1.379(3) . ?
N32 C31 1.370(3) . ?
N32 C33 1.383(3) . ?
N32 C34 1.515(3) . ?
C12 C13 1.347(4) . ?
C14 C15 1.520(4) . ?
C14 C17 1.524(4) . ?
C14 C16 1.531(4) . ?
C22 C23 1.339(4) . ?
C24 C25 1.518(4) . ?
C24 C27 1.531(5) . ?
C24 C26 1.532(5) . ?
C32 C33 1.341(4) . ?
C34 C36 1.520(4) . ?
C34 C37 1.522(4) . ?
C34 C35 1.537(4) . ?
C2S C1S 1.384(12) . ?
C1S N1S 1.127(14) . ?
