#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:33:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179188 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/32/4313256.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_4313256
loop_
_publ_author_name
'Heidi Boerzel'
'Margery Koeckert'
'Weiming Bu'
'Bernhard Spingler'
'Stephen J. Lippard'
_publ_section_title
;
 Zinc-Bound Thiolate-Disulfide Exchange: A Strategy for Inhibiting
 Metallo-β-lactamases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1604
_journal_page_last               1615
_journal_paper_doi               10.1021/ic025624f
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C37 H35 B N6 S Zn'
_chemical_formula_weight         671.95
_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                69.084(5)
_cell_angle_beta                 71.052(5)
_cell_angle_gamma                72.267(5)
_cell_formula_units_Z            2
_cell_length_a                   11.699(5)
_cell_length_b                   12.515(5)
_cell_length_c                   13.388(5)
_cell_measurement_temperature    188(2)
_cell_volume                     1691.8(12)
_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      188(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0948
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10677
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamond
_exptl_crystal_F_000             700
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .15
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0022(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.748
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.748
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          4.548
_refine_ls_shift/su_mean         0.103
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                4700
_reflns_number_total             7449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025624f_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1691.9(12)
_cod_database_code               4313256
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 0.28065(3) 0.18607(3) 0.72940(3) 0.02568(13) Uani 1 1 d . . .
S1 S 0.26692(8) 0.35992(7) 0.60360(6) 0.0337(2) Uani 1 1 d . . .
N11 N 0.1670(2) 0.0698(2) 0.76981(19) 0.0265(6) Uani 1 1 d . . .
N12 N 0.1809(2) -0.0199(2) 0.86535(19) 0.0256(6) Uani 1 1 d . . .
N21 N 0.2571(2) 0.1669(2) 0.89397(19) 0.0272(6) Uani 1 1 d . . .
N22 N 0.2907(2) 0.0526(2) 0.95395(19) 0.0268(6) Uani 1 1 d . . .
N31 N 0.4346(2) 0.0494(2) 0.73004(19) 0.0262(6) Uani 1 1 d . . .
N32 N 0.4127(2) -0.0531(2) 0.81025(19) 0.0266(6) Uani 1 1 d . . .
C11 C 0.0675(3) 0.0630(3) 0.7451(2) 0.0284(7) Uani 1 1 d . . .
C12 C 0.0172(3) -0.0299(3) 0.8234(3) 0.0310(7) Uani 1 1 d . . .
H12A H -0.0515 -0.0535 0.8248 0.037 Uiso 1 1 calc R . .
C13 C 0.0893(3) -0.0795(2) 0.8984(2) 0.0269(7) Uani 1 1 d . . .
C14 C 0.0727(3) -0.1762(3) 1.0043(3) 0.0347(8) Uani 1 1 d . . .
H14A H 0.1479 -0.2351 1.0048 0.052 Uiso 1 1 calc R . .
H14B H 0.0066 -0.2102 1.0104 0.052 Uiso 1 1 calc R . .
H14C H 0.0532 -0.1452 1.0653 0.052 Uiso 1 1 calc R . .
C15 C 0.0231(3) 0.1474(3) 0.6480(3) 0.0339(7) Uani 1 1 d . . .
C16 C -0.0107(3) 0.2659(3) 0.6358(3) 0.0435(9) Uani 1 1 d . . .
H16A H -0.0033 0.2943 0.6884 0.052 Uiso 1 1 calc R . .
C17 C -0.0559(3) 0.3442(3) 0.5459(3) 0.0474(9) Uani 1 1 d . . .
H17A H -0.0781 0.4240 0.5388 0.057 Uiso 1 1 calc R . .
C18 C -0.0674(4) 0.3046(4) 0.4697(4) 0.0599(12) Uani 1 1 d . . .
H18A H -0.1000 0.3567 0.4110 0.072 Uiso 1 1 calc R . .
C19 C -0.0318(7) 0.1886(5) 0.4779(5) 0.118(3) Uani 1 1 d . . .
H19A H -0.0365 0.1619 0.4231 0.142 Uiso 1 1 calc R . .
C20 C 0.0118(6) 0.1092(4) 0.5685(4) 0.097(2) Uani 1 1 d . . .
H20A H 0.0334 0.0296 0.5748 0.116 Uiso 1 1 calc R . .
C21 C 0.2514(3) 0.2343(3) 0.9548(2) 0.0282(7) Uani 1 1 d . . .
C22 C 0.2852(3) 0.1622(3) 1.0529(2) 0.0333(7) Uani 1 1 d . . .
H22A H 0.2907 0.1864 1.1089 0.040 Uiso 1 1 calc R . .
C23 C 0.3085(3) 0.0485(3) 1.0499(2) 0.0305(7) Uani 1 1 d . . .
C24 C 0.3464(4) -0.0632(3) 1.1334(3) 0.0429(9) Uani 1 1 d . . .
H24A H 0.4211 -0.1089 1.0993 0.064 Uiso 1 1 calc R . .
H24B H 0.2820 -0.1066 1.1623 0.064 Uiso 1 1 calc R . .
H24C H 0.3604 -0.0460 1.1923 0.064 Uiso 1 1 calc R . .
C25 C 0.2086(3) 0.3629(3) 0.9202(2) 0.0286(7) Uani 1 1 d . . .
C26 C 0.1164(3) 0.4147(3) 0.8625(3) 0.0336(7) Uani 1 1 d . . .
H26A H 0.0864 0.3686 0.8399 0.040 Uiso 1 1 calc R . .
C27 C 0.0691(3) 0.5344(3) 0.8384(3) 0.0397(8) Uani 1 1 d . . .
H27A H 0.0066 0.5682 0.8008 0.048 Uiso 1 1 calc R . .
C28 C 0.1148(3) 0.6038(3) 0.8702(3) 0.0411(9) Uani 1 1 d . . .
H28A H 0.0828 0.6841 0.8547 0.049 Uiso 1 1 calc R . .
C29 C 0.2076(4) 0.5531(3) 0.9247(3) 0.0453(9) Uani 1 1 d . . .
H29A H 0.2394 0.6000 0.9448 0.054 Uiso 1 1 calc R . .
C30 C 0.2547(3) 0.4342(3) 0.9503(3) 0.0385(8) Uani 1 1 d . . .
H30A H 0.3173 0.4014 0.9878 0.046 Uiso 1 1 calc R . .
C31 C 0.5399(3) 0.0190(3) 0.6563(2) 0.0273(7) Uani 1 1 d . . .
C32 C 0.5832(3) -0.1019(3) 0.6889(3) 0.0333(7) Uani 1 1 d . . .
H32A H 0.6537 -0.1451 0.6526 0.040 Uiso 1 1 calc R . .
C33 C 0.5012(3) -0.1447(3) 0.7856(2) 0.0282(7) Uani 1 1 d . . .
C34 C 0.4996(3) -0.2688(3) 0.8557(3) 0.0422(9) Uani 1 1 d . . .
H34A H 0.4948 -0.2748 0.9304 0.063 Uiso 1 1 calc R . .
H34B H 0.5739 -0.3199 0.8282 0.063 Uiso 1 1 calc R . .
H34C H 0.4291 -0.2909 0.8533 0.063 Uiso 1 1 calc R . .
C35 C 0.5920(3) 0.1095(3) 0.5612(2) 0.0310(7) Uani 1 1 d . . .
C36 C 0.5892(3) 0.2167(3) 0.5718(3) 0.0346(7) Uani 1 1 d . . .
H36A H 0.5567 0.2304 0.6405 0.041 Uiso 1 1 calc R . .
C37 C 0.6344(3) 0.3035(3) 0.4814(3) 0.0467(9) Uani 1 1 d . . .
H37A H 0.6309 0.3755 0.4890 0.056 Uiso 1 1 calc R . .
C38 C 0.6847(3) 0.2820(4) 0.3799(3) 0.0544(11) Uani 1 1 d . . .
H38A H 0.7147 0.3401 0.3188 0.065 Uiso 1 1 calc R . .
C39 C 0.6908(3) 0.1746(4) 0.3685(3) 0.0495(10) Uani 1 1 d . . .
H39A H 0.7256 0.1609 0.3000 0.059 Uiso 1 1 calc R . .
C40 C 0.6456(3) 0.0877(3) 0.4583(3) 0.0399(8) Uani 1 1 d . . .
H40A H 0.6508 0.0153 0.4506 0.048 Uiso 1 1 calc R . .
C41 C 0.3038(3) 0.3104(3) 0.4801(2) 0.0360(8) Uani 1 1 d . . .
H41A H 0.3842 0.2573 0.4736 0.043 Uiso 1 1 calc R . .
H41B H 0.2429 0.2678 0.4884 0.043 Uiso 1 1 calc R . .
C42 C 0.3050(3) 0.4127(3) 0.3759(2) 0.0339(8) Uani 1 1 d . . .
C43 C 0.2233(3) 0.4355(3) 0.3118(3) 0.0404(8) Uani 1 1 d . . .
H43A H 0.1656 0.3892 0.3338 0.049 Uiso 1 1 calc R . .
C44 C 0.2270(4) 0.5274(3) 0.2145(3) 0.0503(10) Uani 1 1 d . . .
H44A H 0.1714 0.5424 0.1724 0.060 Uiso 1 1 calc R . .
C45 C 0.3117(4) 0.5955(4) 0.1809(3) 0.0562(11) Uani 1 1 d . . .
H45A H 0.3145 0.6561 0.1155 0.067 Uiso 1 1 calc R . .
C46 C 0.3932(4) 0.5744(4) 0.2441(3) 0.0562(11) Uani 1 1 d . . .
H46A H 0.4505 0.6212 0.2214 0.067 Uiso 1 1 calc R . .
C47 C 0.3898(3) 0.4832(3) 0.3417(3) 0.0446(9) Uani 1 1 d . . .
H47A H 0.4447 0.4695 0.3841 0.053 Uiso 1 1 calc R . .
B1 B 0.2979(3) -0.0475(3) 0.9082(3) 0.0270(8) Uani 1 1 d . . .
H1 H 0.303(3) -0.129(2) 0.973(2) 0.020(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'
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'
B B 0.0013 0.0007 '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
N21 Zn1 N31 91.53(9) . . ?
N21 Zn1 N11 90.86(10) . . ?
N31 Zn1 N11 90.39(10) . . ?
N21 Zn1 S1 122.54(7) . . ?
N31 Zn1 S1 125.85(7) . . ?
N11 Zn1 S1 125.41(7) . . ?
C41 S1 Zn1 98.71(10) . . ?
C11 N11 N12 106.6(2) . . ?
C11 N11 Zn1 139.9(2) . . ?
N12 N11 Zn1 112.14(18) . . ?
C13 N12 N11 109.1(2) . . ?
C13 N12 B1 130.4(2) . . ?
N11 N12 B1 119.9(2) . . ?
C21 N21 N22 106.9(2) . . ?
C21 N21 Zn1 136.8(2) . . ?
N22 N21 Zn1 113.05(18) . . ?
C23 N22 N21 110.2(2) . . ?
C23 N22 B1 130.4(2) . . ?
N21 N22 B1 119.4(2) . . ?
C31 N31 N32 106.2(2) . . ?
C31 N31 Zn1 136.7(2) . . ?
N32 N31 Zn1 113.49(17) . . ?
C33 N32 N31 110.0(2) . . ?
C33 N32 B1 131.1(2) . . ?
N31 N32 B1 118.9(2) . . ?
N11 C11 C12 109.9(3) . . ?
N11 C11 C15 121.7(3) . . ?
C12 C11 C15 128.4(3) . . ?
C13 C12 C11 106.3(3) . . ?
N12 C13 C12 108.1(3) . . ?
N12 C13 C14 122.2(3) . . ?
C12 C13 C14 129.6(3) . . ?
C20 C15 C16 117.7(3) . . ?
C20 C15 C11 120.7(3) . . ?
C16 C15 C11 121.6(3) . . ?
C15 C16 C17 121.0(4) . . ?
C18 C17 C16 120.1(4) . . ?
C17 C18 C19 120.2(4) . . ?
C18 C19 C20 120.1(4) . . ?
C15 C20 C19 120.7(4) . . ?
N21 C21 C22 108.9(3) . . ?
N21 C21 C25 122.3(3) . . ?
C22 C21 C25 128.7(3) . . ?
C23 C22 C21 106.5(3) . . ?
N22 C23 C22 107.4(3) . . ?
N22 C23 C24 123.3(3) . . ?
C22 C23 C24 129.3(3) . . ?
C26 C25 C30 118.7(3) . . ?
C26 C25 C21 120.7(3) . . ?
C30 C25 C21 120.5(3) . . ?
C27 C26 C25 120.5(3) . . ?
C28 C27 C26 120.0(3) . . ?
C29 C28 C27 119.4(3) . . ?
C28 C29 C30 121.2(3) . . ?
C29 C30 C25 120.1(3) . . ?
N31 C31 C32 109.5(3) . . ?
N31 C31 C35 120.2(3) . . ?
C32 C31 C35 130.3(3) . . ?
C33 C32 C31 106.4(3) . . ?
N32 C33 C32 107.9(3) . . ?
N32 C33 C34 122.4(3) . . ?
C32 C33 C34 129.8(3) . . ?
C36 C35 C40 119.3(3) . . ?
C36 C35 C31 120.8(3) . . ?
C40 C35 C31 119.9(3) . . ?
C37 C36 C35 120.9(3) . . ?
C38 C37 C36 119.4(4) . . ?
C37 C38 C39 120.4(3) . . ?
C40 C39 C38 120.5(3) . . ?
C39 C40 C35 119.5(4) . . ?
C42 C41 S1 111.6(2) . . ?
C47 C42 C43 118.8(3) . . ?
C47 C42 C41 120.6(3) . . ?
C43 C42 C41 120.6(3) . . ?
C42 C43 C44 120.5(4) . . ?
C45 C44 C43 120.3(4) . . ?
C44 C45 C46 119.9(3) . . ?
C45 C46 C47 120.1(4) . . ?
C42 C47 C46 120.3(4) . . ?
N32 B1 N22 109.1(2) . . ?
N32 B1 N12 108.3(2) . . ?
N22 B1 N12 108.8(2) . . ?
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 N21 2.063(3) . ?
Zn1 N31 2.072(3) . ?
Zn1 N11 2.080(3) . ?
Zn1 S1 2.2232(11) . ?
S1 C41 1.846(3) . ?
N11 C11 1.343(4) . ?
N11 N12 1.386(3) . ?
N12 C13 1.358(4) . ?
N12 B1 1.549(4) . ?
N21 C21 1.341(4) . ?
N21 N22 1.374(3) . ?
N22 C23 1.347(4) . ?
N22 B1 1.551(4) . ?
N31 C31 1.352(4) . ?
N31 N32 1.379(3) . ?
N32 C33 1.349(4) . ?
N32 B1 1.548(4) . ?
C11 C12 1.394(4) . ?
C11 C15 1.482(4) . ?
C12 C13 1.374(4) . ?
C13 C14 1.501(4) . ?
C15 C20 1.369(5) . ?
C15 C16 1.377(5) . ?
C16 C17 1.394(5) . ?
C17 C18 1.341(6) . ?
C18 C19 1.356(6) . ?
C19 C20 1.397(6) . ?
C21 C22 1.403(4) . ?
C21 C25 1.478(4) . ?
C22 C23 1.378(5) . ?
C23 C24 1.493(4) . ?
C25 C26 1.392(4) . ?
C25 C30 1.393(5) . ?
C26 C27 1.386(5) . ?
C27 C28 1.384(5) . ?
C28 C29 1.372(5) . ?
C29 C30 1.377(5) . ?
C31 C32 1.393(4) . ?
C31 C35 1.470(4) . ?
C32 C33 1.376(4) . ?
C33 C34 1.503(4) . ?
C35 C36 1.389(5) . ?
C35 C40 1.403(4) . ?
C36 C37 1.385(5) . ?
C37 C38 1.383(5) . ?
C38 C39 1.383(6) . ?
C39 C40 1.384(5) . ?
C41 C42 1.519(4) . ?
C42 C47 1.386(5) . ?
C42 C43 1.387(5) . ?
C43 C44 1.395(5) . ?
C44 C45 1.365(6) . ?
C45 C46 1.380(6) . ?
C46 C47 1.394(5) . ?
