#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:24:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179139 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/00/4310040.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_4310040
loop_
_publ_author_name
'Philip J. Bailey'
'Alice Dawson'
'Chiara McCormack'
'Stephen A. Moggach'
'Iain D. H. Oswald'
'Simon Parsons'
'David W. H. Rankin'
'Andrew Turner'
_publ_section_title
;
Barriers to Racemization in C3-Symmetric Complexes Containing the
Hydrotris(2-mercapto-1-ethylimidazolyl)borate (TmEt) Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8884
_journal_page_last               8898
_journal_paper_doi               10.1021/ic0505293
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C15 H22 B Cl N6 S3 Zn, C H2 Cl2'
_chemical_formula_sum            'C16 H24 B Cl3 N6 S3 Zn'
_chemical_formula_weight         579.12
_chemical_name_systematic
; 
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.361(3)
_cell_angle_beta                 91.097(3)
_cell_angle_gamma                111.863(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0230(18)
_cell_length_b                   10.277(2)
_cell_length_c                   14.641(3)
_cell_measurement_reflns_used    5459
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      26.65
_cell_measurement_theta_min      2.43
_cell_volume                     1259.6(4)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'φ & ω 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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11310
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         28.82
_diffrn_reflns_theta_min         1.39
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.558
_exptl_absorpt_correction_T_max  0.560
_exptl_absorpt_correction_T_min  0.496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         5892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0501P)²+0.4225P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                5129
_reflns_number_total             5892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0505293si20050817_061150_1.cif
_cod_data_source_block           cm4968
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' 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        1259.7(4)
_cod_database_code               4310040
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 0.67527(3) 0.67494(3) 0.190081(17) 0.02543(8) Uani 1 1 d . . .
Cl1 Cl 0.60670(8) 0.84423(6) 0.12762(4) 0.03789(15) Uani 1 1 d . . .
B1 B 0.8151(3) 0.4027(3) 0.27261(17) 0.0256(5) Uani 1 1 d . . .
S1 S 0.75231(7) 0.55832(6) 0.07197(4) 0.02712(13) Uani 1 1 d . . .
N11 N 0.9382(2) 0.49298(19) 0.20367(12) 0.0251(4) Uani 1 1 d . . .
C12 C 0.9229(3) 0.5576(2) 0.12616(15) 0.0247(4) Uani 1 1 d . . .
N13 N 1.0704(2) 0.6251(2) 0.09418(13) 0.0284(4) Uani 1 1 d . . .
C131 C 1.1087(3) 0.7167(3) 0.01468(17) 0.0370(6) Uani 1 1 d . . .
H13A H 1.0272 0.6765 -0.0335 0.044 Uiso 1 1 calc R . .
H13B H 1.2119 0.7229 -0.0091 0.044 Uiso 1 1 calc R . .
C132 C 1.1161(4) 0.8619(3) 0.0398(2) 0.0504(7) Uani 1 1 d . . .
H13C H 1.0111 0.8570 0.0575 0.076 Uiso 1 1 calc R . .
H13D H 1.1504 0.9227 -0.0124 0.076 Uiso 1 1 calc R . .
H13E H 1.1915 0.8992 0.0903 0.076 Uiso 1 1 calc R . .
C14 C 1.1812(3) 0.6042(3) 0.15205(18) 0.0348(5) Uani 1 1 d . . .
H14 H 1.2926 0.6402 0.1456 0.042 Uiso 1 1 calc R . .
C15 C 1.0999(3) 0.5232(3) 0.21904(17) 0.0327(5) Uani 1 1 d . . .
H15 H 1.1448 0.4916 0.2685 0.039 Uiso 1 1 calc R . .
S2 S 0.47682(6) 0.48873(6) 0.26430(4) 0.02676(13) Uani 1 1 d . . .
N21 N 0.6508(2) 0.32290(18) 0.22586(12) 0.0238(4) Uani 1 1 d . . .
C22 C 0.5176(3) 0.3526(2) 0.21614(14) 0.0238(4) Uani 1 1 d . . .
N23 N 0.4156(2) 0.25401(19) 0.15995(13) 0.0275(4) Uani 1 1 d . . .
C231 C 0.2553(3) 0.2446(3) 0.13180(17) 0.0361(5) Uani 1 1 d . . .
H23A H 0.2275 0.1973 0.0720 0.043 Uiso 1 1 calc R . .
H23B H 0.2551 0.3393 0.1254 0.043 Uiso 1 1 calc R . .
C232 C 0.1311(3) 0.1654(3) 0.1997(2) 0.0494(7) Uani 1 1 d . . .
H23C H 0.1310 0.0715 0.2063 0.074 Uiso 1 1 calc R . .
H23D H 0.0266 0.1598 0.1780 0.074 Uiso 1 1 calc R . .
H23E H 0.1559 0.2139 0.2583 0.074 Uiso 1 1 calc R . .
C24 C 0.4851(3) 0.1614(2) 0.13348(16) 0.0323(5) Uani 1 1 d . . .
H24 H 0.4400 0.0836 0.0939 0.039 Uiso 1 1 calc R . .
C25 C 0.6288(3) 0.2033(2) 0.17472(16) 0.0298(5) Uani 1 1 d . . .
H25 H 0.7025 0.1589 0.1698 0.036 Uiso 1 1 calc R . .
S3 S 0.89154(7) 0.76157(6) 0.29615(4) 0.03030(13) Uani 1 1 d . . .
N31 N 0.8016(2) 0.4880(2) 0.35750(12) 0.0270(4) Uani 1 1 d . . .
C32 C 0.8281(3) 0.6247(2) 0.37150(15) 0.0280(5) Uani 1 1 d . . .
N33 N 0.7917(3) 0.6398(2) 0.45918(14) 0.0354(5) Uani 1 1 d . . .
C331 C 0.8143(4) 0.7714(3) 0.50637(18) 0.0436(6) Uani 1 1 d . . .
H33A H 0.7352 0.7540 0.5544 0.052 Uiso 1 1 calc R . .
H33B H 0.7967 0.8367 0.4629 0.052 Uiso 1 1 calc R . .
C332 C 0.9792(4) 0.8371(3) 0.5483(2) 0.0543(8) Uani 1 1 d . . .
H33C H 0.9977 0.7720 0.5905 0.081 Uiso 1 1 calc R . .
H33D H 0.9889 0.9224 0.5809 0.081 Uiso 1 1 calc R . .
H33E H 1.0575 0.8591 0.5006 0.081 Uiso 1 1 calc R . .
C34 C 0.7418(4) 0.5118(3) 0.50036(17) 0.0431(6) Uani 1 1 d . . .
H34 H 0.7098 0.4933 0.5612 0.052 Uiso 1 1 calc R . .
C35 C 0.7472(3) 0.4179(3) 0.43775(16) 0.0373(6) Uani 1 1 d . . .
H35 H 0.7189 0.3213 0.4469 0.045 Uiso 1 1 calc R . .
C1S C 1.3726(5) 0.8952(3) 0.3160(2) 0.0581(8) Uani 1 1 d . . .
H1S1 H 1.4270 0.9203 0.2577 0.070 Uiso 1 1 calc R . .
H1S2 H 1.2588 0.8434 0.3025 0.070 Uiso 1 1 calc R . .
Cl1S Cl 1.39522(15) 1.04692(10) 0.37638(7) 0.0818(3) Uani 1 1 d . . .
Cl2S Cl 1.45013(14) 0.78636(9) 0.37611(6) 0.0726(3) Uani 1 1 d . . .
H1 H 0.861(3) 0.319(3) 0.2988(17) 0.032(7) Uiso 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'
Cl Cl 0.1484 0.1585 '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
Cl1 Zn1 S1 108.24(3) . . ?
Cl1 Zn1 S3 113.27(3) . . ?
S1 Zn1 S3 107.67(3) . . ?
Cl1 Zn1 S2 118.52(3) . . ?
S1 Zn1 S2 102.64(2) . . ?
S3 Zn1 S2 105.57(2) . . ?
N21 B1 N31 112.07(18) . . ?
N21 B1 N11 111.59(18) . . ?
N31 B1 N11 112.74(18) . . ?
N21 B1 H1 106.6(12) . . ?
N31 B1 H1 106.5(13) . . ?
N11 B1 H1 106.8(13) . . ?
C12 S1 Zn1 96.25(7) . . ?
C12 N11 C15 107.49(19) . . ?
C12 N11 B1 132.54(18) . . ?
C15 N11 B1 119.95(19) . . ?
N13 C12 N11 107.58(19) . . ?
N13 C12 S1 123.21(17) . . ?
N11 C12 S1 129.20(16) . . ?
C12 N13 C14 109.4(2) . . ?
C12 N13 C131 125.4(2) . . ?
C14 N13 C131 125.0(2) . . ?
N13 C131 C132 111.0(2) . . ?
N13 C131 H13A 109.4 . . ?
C132 C131 H13A 109.4 . . ?
N13 C131 H13B 109.4 . . ?
C132 C131 H13B 109.4 . . ?
H13A C131 H13B 108.0 . . ?
C131 C132 H13C 109.5 . . ?
C131 C132 H13D 109.5 . . ?
H13C C132 H13D 109.5 . . ?
C131 C132 H13E 109.5 . . ?
H13C C132 H13E 109.5 . . ?
H13D C132 H13E 109.5 . . ?
C15 C14 N13 106.7(2) . . ?
C15 C14 H14 126.6 . . ?
N13 C14 H14 126.6 . . ?
C14 C15 N11 108.8(2) . . ?
C14 C15 H15 125.6 . . ?
N11 C15 H15 125.6 . . ?
C22 S2 Zn1 97.76(7) . . ?
C22 N21 C25 107.90(18) . . ?
C22 N21 B1 132.52(18) . . ?
C25 N21 B1 119.26(18) . . ?
N23 C22 N21 107.44(18) . . ?
N23 C22 S2 123.98(17) . . ?
N21 C22 S2 128.58(17) . . ?
C22 N23 C24 109.20(19) . . ?
C22 N23 C231 125.9(2) . . ?
C24 N23 C231 124.9(2) . . ?
N23 C231 C232 112.0(2) . . ?
N23 C231 H23A 109.2 . . ?
C232 C231 H23A 109.2 . . ?
N23 C231 H23B 109.2 . . ?
C232 C231 H23B 109.2 . . ?
H23A C231 H23B 107.9 . . ?
C231 C232 H23C 109.5 . . ?
C231 C232 H23D 109.5 . . ?
H23C C232 H23D 109.5 . . ?
C231 C232 H23E 109.5 . . ?
H23C C232 H23E 109.5 . . ?
H23D C232 H23E 109.5 . . ?
C25 C24 N23 106.9(2) . . ?
C25 C24 H24 126.5 . . ?
N23 C24 H24 126.5 . . ?
C24 C25 N21 108.5(2) . . ?
C24 C25 H25 125.7 . . ?
N21 C25 H25 125.7 . . ?
C32 S3 Zn1 97.60(8) . . ?
C32 N31 C35 108.15(19) . . ?
C32 N31 B1 133.06(19) . . ?
C35 N31 B1 118.74(19) . . ?
N31 C32 N33 107.4(2) . . ?
N31 C32 S3 129.35(17) . . ?
N33 C32 S3 123.28(18) . . ?
C32 N33 C34 109.2(2) . . ?
C32 N33 C331 126.4(2) . . ?
C34 N33 C331 124.2(2) . . ?
N33 C331 C332 111.7(2) . . ?
N33 C331 H33A 109.3 . . ?
C332 C331 H33A 109.3 . . ?
N33 C331 H33B 109.3 . . ?
C332 C331 H33B 109.3 . . ?
H33A C331 H33B 107.9 . . ?
C331 C332 H33C 109.5 . . ?
C331 C332 H33D 109.5 . . ?
H33C C332 H33D 109.5 . . ?
C331 C332 H33E 109.5 . . ?
H33C C332 H33E 109.5 . . ?
H33D C332 H33E 109.5 . . ?
C35 C34 N33 107.2(2) . . ?
C35 C34 H34 126.4 . . ?
N33 C34 H34 126.4 . . ?
C34 C35 N31 108.1(2) . . ?
C34 C35 H35 126.0 . . ?
N31 C35 H35 126.0 . . ?
Cl1S C1S Cl2S 112.47(19) . . ?
Cl1S C1S H1S1 109.1 . . ?
Cl2S C1S H1S1 109.1 . . ?
Cl1S C1S H1S2 109.1 . . ?
Cl2S C1S H1S2 109.1 . . ?
H1S1 C1S H1S2 107.8 . . ?
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 Cl1 2.2464(7) . ?
Zn1 S1 2.3560(7) . ?
Zn1 S3 2.3633(7) . ?
Zn1 S2 2.3660(7) . ?
B1 N21 1.545(3) . ?
B1 N31 1.549(3) . ?
B1 N11 1.549(3) . ?
B1 H1 1.15(2) . ?
S1 C12 1.720(2) . ?
N11 C12 1.349(3) . ?
N11 C15 1.388(3) . ?
C12 N13 1.346(3) . ?
N13 C14 1.376(3) . ?
N13 C131 1.466(3) . ?
C131 C132 1.511(4) . ?
C131 H13A 0.9800 . ?
C131 H13B 0.9800 . ?
C132 H13C 0.9700 . ?
C132 H13D 0.9700 . ?
C132 H13E 0.9700 . ?
C14 C15 1.333(4) . ?
C14 H14 0.9400 . ?
C15 H15 0.9400 . ?
S2 C22 1.724(2) . ?
N21 C22 1.351(3) . ?
N21 C25 1.383(3) . ?
C22 N23 1.348(3) . ?
N23 C24 1.378(3) . ?
N23 C231 1.464(3) . ?
C231 C232 1.510(4) . ?
C231 H23A 0.9800 . ?
C231 H23B 0.9800 . ?
C232 H23C 0.9700 . ?
C232 H23D 0.9700 . ?
C232 H23E 0.9700 . ?
C24 C25 1.335(3) . ?
C24 H24 0.9400 . ?
C25 H25 0.9400 . ?
S3 C32 1.722(2) . ?
N31 C32 1.348(3) . ?
N31 C35 1.382(3) . ?
C32 N33 1.353(3) . ?
N33 C34 1.369(3) . ?
N33 C331 1.458(3) . ?
C331 C332 1.503(4) . ?
C331 H33A 0.9800 . ?
C331 H33B 0.9800 . ?
C332 H33C 0.9700 . ?
C332 H33D 0.9700 . ?
C332 H33E 0.9700 . ?
C34 C35 1.342(4) . ?
C34 H34 0.9400 . ?
C35 H35 0.9400 . ?
C1S Cl1S 1.730(3) . ?
C1S Cl2S 1.757(3) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
