#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:07:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179232 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/52/4315246.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_4315246
loop_
_publ_author_name
'Elena V. Mutseneck'
'Susanne Bieller'
'Michael Bolte'
'Hans-Wolfram Lerner'
'Matthias Wagner'
_publ_section_title
;
 Fourth Generation Scorpionates: Coordination Behavior of a New Class of
 Conformationally Flexible Mixed-Donor (Pyrazol-1-yl)borates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3540
_journal_page_last               3552
_journal_paper_doi               10.1021/ic100104t
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C31 H38 B2 Br N8 O2 Zn'
_chemical_formula_weight         721.59
_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                 101.466(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2759(8)
_cell_length_b                   23.382(2)
_cell_length_c                   18.0718(17)
_cell_measurement_reflns_used    9067
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      3.5
_cell_volume                     3427.2(6)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990) '
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_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  0.0900
_diffrn_reflns_av_sigmaI/netI    0.1253
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17627
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.44
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.923
_exptl_absorpt_correction_T_max  0.8460
_exptl_absorpt_correction_T_min  0.6770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         6026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0262P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                3587
_reflns_number_total             6026
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic100104t_si_002_06.cif
_cod_data_source_block           wa825
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_database_code               4315246
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 0.40723(8) 0.71872(2) 0.21699(3) 0.02387(15) Uani 1 1 d . . .
Br1 Br 0.32190(8) 0.79427(2) 0.12332(3) 0.03524(16) Uani 1 1 d . . .
O1 O 0.4712(4) 0.64676(12) 0.31065(16) 0.0222(7) Uani 1 1 d . . .
B1 B 0.4423(8) 0.6654(2) 0.3849(3) 0.0249(13) Uani 1 1 d . . .
B2 B 0.3985(8) 0.5909(2) 0.2851(3) 0.0254(13) Uani 1 1 d . . .
N11 N 0.3817(5) 0.72905(16) 0.3774(2) 0.0269(10) Uani 1 1 d . . .
N12 N 0.3439(5) 0.75498(15) 0.3086(2) 0.0236(9) Uani 1 1 d . . .
C13 C 0.2942(7) 0.8082(2) 0.3203(3) 0.0315(12) Uani 1 1 d . . .
H13 H 0.2628 0.8364 0.2822 0.038 Uiso 1 1 calc R . .
C14 C 0.2959(8) 0.8158(2) 0.3970(3) 0.0378(14) Uani 1 1 d . . .
H14 H 0.2640 0.8491 0.4206 0.045 Uiso 1 1 calc R . .
C15 C 0.3530(8) 0.7654(2) 0.4311(3) 0.0321(13) Uani 1 1 d . . .
H15 H 0.3695 0.7574 0.4836 0.039 Uiso 1 1 calc R . .
N21 N 0.2973(6) 0.59844(16) 0.2021(2) 0.0274(10) Uani 1 1 d . . .
N22 N 0.2811(5) 0.65034(16) 0.1674(2) 0.0264(9) Uani 1 1 d . . .
C23 C 0.1832(7) 0.6425(2) 0.1000(3) 0.0350(13) Uani 1 1 d . . .
H23 H 0.1512 0.6718 0.0635 0.042 Uiso 1 1 calc R . .
C24 C 0.1352(8) 0.5865(2) 0.0905(3) 0.0404(14) Uani 1 1 d . . .
H24 H 0.0659 0.5697 0.0478 0.048 Uiso 1 1 calc R . .
C25 C 0.2094(7) 0.5597(2) 0.1566(3) 0.0356(13) Uani 1 1 d . . .
H25 H 0.1997 0.5203 0.1679 0.043 Uiso 1 1 calc R . .
N31 N 0.2920(6) 0.62523(16) 0.3937(2) 0.0273(10) Uani 1 1 d . . .
N32 N 0.2691(5) 0.58407(16) 0.3391(2) 0.0275(10) Uani 1 1 d . . .
C33 C 0.1437(8) 0.5508(2) 0.3490(3) 0.0412(15) Uani 1 1 d . . .
H33 H 0.1024 0.5187 0.3188 0.049 Uiso 1 1 calc R . .
C34 C 0.0834(8) 0.5709(2) 0.4111(3) 0.0413(14) Uani 1 1 d . . .
H34 H -0.0051 0.5556 0.4312 0.050 Uiso 1 1 calc R . .
C35 C 0.1790(7) 0.6176(2) 0.4370(3) 0.0367(13) Uani 1 1 d . . .
H35 H 0.1672 0.6408 0.4788 0.044 Uiso 1 1 calc R . .
N41 N 0.6534(5) 0.71575(17) 0.2183(2) 0.0276(9) Uani 1 1 d . . .
N42 N 0.7613(6) 0.6819(2) 0.2649(3) 0.0386(12) Uani 1 1 d . . .
H42 H 0.726(9) 0.656(3) 0.295(4) 0.07(2) Uiso 1 1 d . . .
C43 C 0.9179(8) 0.6900(3) 0.2544(3) 0.0449(15) Uani 1 1 d . . .
H43 H 1.0144 0.6712 0.2804 0.054 Uiso 1 1 calc R . .
C44 C 0.9095(7) 0.7306(2) 0.1992(3) 0.0392(14) Uani 1 1 d . . .
H44 H 0.9986 0.7455 0.1791 0.047 Uiso 1 1 calc R . .
C45 C 0.7465(7) 0.7454(2) 0.1788(3) 0.0305(12) Uani 1 1 d . . .
H45 H 0.7047 0.7731 0.1415 0.037 Uiso 1 1 calc R . .
C51 C 0.5976(7) 0.65920(19) 0.4537(3) 0.0264(11) Uani 1 1 d . . .
C52 C 0.6189(8) 0.6134(2) 0.5052(3) 0.0353(13) Uani 1 1 d . . .
H52 H 0.5335 0.5859 0.5029 0.042 Uiso 1 1 calc R . .
C53 C 0.7638(8) 0.6075(2) 0.5597(3) 0.0442(15) Uani 1 1 d . . .
H53 H 0.7763 0.5759 0.5934 0.053 Uiso 1 1 calc R . .
C54 C 0.8874(8) 0.6469(2) 0.5649(3) 0.0375(13) Uani 1 1 d . . .
H54 H 0.9848 0.6431 0.6025 0.045 Uiso 1 1 calc R . .
C55 C 0.8699(7) 0.6922(2) 0.5151(3) 0.0367(13) Uani 1 1 d . . .
H55 H 0.9564 0.7193 0.5184 0.044 Uiso 1 1 calc R . .
C56 C 0.7296(7) 0.6985(2) 0.4610(3) 0.0312(12) Uani 1 1 d . . .
H56 H 0.7208 0.7302 0.4275 0.037 Uiso 1 1 calc R . .
C61 C 0.5265(7) 0.53974(19) 0.2921(3) 0.0265(11) Uani 1 1 d . . .
C62 C 0.6231(8) 0.5322(2) 0.2362(3) 0.0386(14) Uani 1 1 d . . .
H62 H 0.6021 0.5559 0.1926 0.046 Uiso 1 1 calc R . .
C63 C 0.7469(9) 0.4917(2) 0.2430(3) 0.0509(17) Uani 1 1 d . . .
H63 H 0.8108 0.4886 0.2050 0.061 Uiso 1 1 calc R . .
C64 C 0.7782(9) 0.4556(2) 0.3049(4) 0.0502(17) Uani 1 1 d . . .
H64 H 0.8623 0.4274 0.3093 0.060 Uiso 1 1 calc R . .
C65 C 0.6856(9) 0.4611(2) 0.3602(3) 0.0496(17) Uani 1 1 d . . .
H65 H 0.7055 0.4365 0.4029 0.059 Uiso 1 1 calc R . .
C66 C 0.5628(8) 0.5028(2) 0.3534(3) 0.0412(15) Uani 1 1 d . . .
H66 H 0.5014 0.5060 0.3924 0.049 Uiso 1 1 calc R . .
O71 O 0.1684(8) 0.4288(2) 0.2203(3) 0.0824(17) Uani 1 1 d . . .
C72 C 0.063(2) 0.3892(8) 0.1968(12) 0.040(6) Uiso 0.35(2) 1 d P A 1
H72A H -0.0460 0.4061 0.1756 0.048 Uiso 0.35(2) 1 calc PR A 1
H72B H 0.0511 0.3636 0.2390 0.048 Uiso 0.35(2) 1 calc PR A 1
C72' C 0.0561(16) 0.4083(5) 0.1536(9) 0.068(5) Uiso 0.65(2) 1 d P A 2
H72C H 0.0454 0.4367 0.1122 0.081 Uiso 0.65(2) 1 calc PR A 2
H72D H -0.0545 0.4010 0.1647 0.081 Uiso 0.65(2) 1 calc PR A 2
C73 C 0.1317(11) 0.3536(3) 0.1320(5) 0.081(3) Uani 1 1 d . . .
H73A H 0.0882 0.3140 0.1263 0.097 Uiso 0.35(2) 1 calc PR A 1
H73B H 0.1090 0.3733 0.0826 0.097 Uiso 0.35(2) 1 calc PR A 1
H73C H 0.0776 0.3200 0.1501 0.097 Uiso 0.65(2) 1 calc PR A 2
H73D H 0.1189 0.3509 0.0765 0.097 Uiso 0.65(2) 1 calc PR A 2
C74 C 0.3054(10) 0.3554(4) 0.1677(4) 0.076(2) Uani 1 1 d . A .
H74A H 0.3726 0.3690 0.1316 0.092 Uiso 1 1 calc R . .
H74B H 0.3448 0.3169 0.1860 0.092 Uiso 1 1 calc R . .
C75 C 0.3169(13) 0.3954(3) 0.2313(5) 0.091(3) Uani 1 1 d . A .
H75A H 0.3307 0.3740 0.2794 0.110 Uiso 1 1 calc R . .
H75B H 0.4135 0.4208 0.2336 0.110 Uiso 1 1 calc R . .
C81 C 0.6705(12) 0.6208(3) 0.0492(4) 0.083(3) Uani 1 1 d . . .
H81A H 0.7844 0.6347 0.0624 0.124 Uiso 1 1 calc R . .
H81B H 0.6156 0.6270 0.0918 0.124 Uiso 1 1 calc R . .
H81C H 0.6114 0.6417 0.0050 0.124 Uiso 1 1 calc R . .
C82 C 0.6708(10) 0.5576(3) 0.0312(4) 0.066(2) Uani 1 1 d . . .
H82A H 0.7271 0.5368 0.0769 0.079 Uiso 1 1 calc R . .
H82B H 0.7356 0.5515 -0.0086 0.079 Uiso 1 1 calc R . .
C83 C 0.5008(11) 0.5319(3) 0.0051(4) 0.071(2) Uani 1 1 d . . .
H83A H 0.4322 0.5416 0.0424 0.085 Uiso 1 1 calc R . .
H83B H 0.4491 0.5498 -0.0435 0.085 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'
Br Br -0.2901 2.4595 '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'
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
N12 Zn1 N22 120.08(17) . . ?
N12 Zn1 N41 115.32(17) . . ?
N22 Zn1 N41 113.96(17) . . ?
N12 Zn1 O1 76.72(12) . . ?
N22 Zn1 O1 77.15(13) . . ?
N41 Zn1 O1 83.50(14) . . ?
N12 Zn1 Br1 100.21(11) . . ?
N22 Zn1 Br1 102.20(11) . . ?
N41 Zn1 Br1 100.54(11) . . ?
O1 Zn1 Br1 175.75(9) . . ?
B2 O1 B1 114.7(4) . . ?
B2 O1 Zn1 112.7(3) . . ?
B1 O1 Zn1 112.7(3) . . ?
O1 B1 N11 108.0(4) . . ?
O1 B1 N31 100.8(4) . . ?
N11 B1 N31 109.1(4) . . ?
O1 B1 C51 115.3(4) . . ?
N11 B1 C51 110.2(4) . . ?
N31 B1 C51 112.9(4) . . ?
O1 B2 N21 107.8(4) . . ?
O1 B2 C61 114.8(5) . . ?
N21 B2 C61 112.3(4) . . ?
O1 B2 N32 100.4(4) . . ?
N21 B2 N32 107.4(4) . . ?
C61 B2 N32 113.2(4) . . ?
C15 N11 N12 109.6(4) . . ?
C15 N11 B1 129.5(4) . . ?
N12 N11 B1 120.8(4) . . ?
C13 N12 N11 106.9(4) . . ?
C13 N12 Zn1 131.0(3) . . ?
N11 N12 Zn1 120.7(3) . . ?
N12 C13 C14 109.4(4) . . ?
N12 C13 H13 125.3 . . ?
C14 C13 H13 125.3 . . ?
C15 C14 C13 105.8(4) . . ?
C15 C14 H14 127.1 . . ?
C13 C14 H14 127.1 . . ?
N11 C15 C14 108.3(4) . . ?
N11 C15 H15 125.9 . . ?
C14 C15 H15 125.9 . . ?
C25 N21 N22 109.1(4) . . ?
C25 N21 B2 129.2(4) . . ?
N22 N21 B2 121.6(4) . . ?
C23 N22 N21 106.6(4) . . ?
C23 N22 Zn1 132.9(3) . . ?
N21 N22 Zn1 120.4(3) . . ?
N22 C23 C24 110.7(5) . . ?
N22 C23 H23 124.6 . . ?
C24 C23 H23 124.6 . . ?
C23 C24 C25 104.9(5) . . ?
C23 C24 H24 127.5 . . ?
C25 C24 H24 127.5 . . ?
N21 C25 C24 108.6(4) . . ?
N21 C25 H25 125.7 . . ?
C24 C25 H25 125.7 . . ?
C35 N31 N32 108.3(4) . . ?
C35 N31 B1 141.6(4) . . ?
N32 N31 B1 110.1(4) . . ?
C33 N32 N31 108.3(4) . . ?
C33 N32 B2 140.7(4) . . ?
N31 N32 B2 111.0(4) . . ?
N32 C33 C34 108.8(5) . . ?
N32 C33 H33 125.6 . . ?
C34 C33 H33 125.6 . . ?
C35 C34 C33 105.5(5) . . ?
C35 C34 H34 127.2 . . ?
C33 C34 H34 127.2 . . ?
N31 C35 C34 109.0(5) . . ?
N31 C35 H35 125.5 . . ?
C34 C35 H35 125.5 . . ?
C45 N41 N42 104.8(4) . . ?
C45 N41 Zn1 131.0(4) . . ?
N42 N41 Zn1 124.2(3) . . ?
N41 N42 C43 111.2(5) . . ?
N41 N42 H42 121(5) . . ?
C43 N42 H42 127(5) . . ?
N42 C43 C44 106.6(5) . . ?
N42 C43 H43 126.7 . . ?
C44 C43 H43 126.7 . . ?
C43 C44 C45 106.0(5) . . ?
C43 C44 H44 127.0 . . ?
C45 C44 H44 127.0 . . ?
N41 C45 C44 111.4(5) . . ?
N41 C45 H45 124.3 . . ?
C44 C45 H45 124.3 . . ?
C52 C51 C56 116.1(5) . . ?
C52 C51 B1 123.8(5) . . ?
C56 C51 B1 119.8(4) . . ?
C53 C52 C51 121.2(5) . . ?
C53 C52 H52 119.4 . . ?
C51 C52 H52 119.4 . . ?
C54 C53 C52 120.5(5) . . ?
C54 C53 H53 119.8 . . ?
C52 C53 H53 119.8 . . ?
C53 C54 C55 119.6(5) . . ?
C53 C54 H54 120.2 . . ?
C55 C54 H54 120.2 . . ?
C56 C55 C54 120.9(5) . . ?
C56 C55 H55 119.5 . . ?
C54 C55 H55 119.5 . . ?
C55 C56 C51 121.7(5) . . ?
C55 C56 H56 119.1 . . ?
C51 C56 H56 119.1 . . ?
C66 C61 C62 115.3(5) . . ?
C66 C61 B2 124.5(5) . . ?
C62 C61 B2 119.9(4) . . ?
C63 C62 C61 122.3(5) . . ?
C63 C62 H62 118.9 . . ?
C61 C62 H62 118.9 . . ?
C64 C63 C62 120.4(6) . . ?
C64 C63 H63 119.8 . . ?
C62 C63 H63 119.8 . . ?
C65 C64 C63 119.1(6) . . ?
C65 C64 H64 120.4 . . ?
C63 C64 H64 120.4 . . ?
C64 C65 C66 120.0(5) . . ?
C64 C65 H65 120.0 . . ?
C66 C65 H65 120.0 . . ?
C61 C66 C65 122.8(5) . . ?
C61 C66 H66 118.6 . . ?
C65 C66 H66 118.6 . . ?
C72 O71 C75 99.3(9) . . ?
C72 O71 C72' 37.5(8) . . ?
C75 O71 C72' 109.0(7) . . ?
O71 C72 C73 107.1(13) . . ?
O71 C72 H72A 110.3 . . ?
C73 C72 H72A 110.3 . . ?
O71 C72 H72B 110.3 . . ?
C73 C72 H72B 110.3 . . ?
H72A C72 H72B 108.5 . . ?
O71 C72' C73 105.3(10) . . ?
O71 C72' H72C 110.7 . . ?
C73 C72' H72C 110.7 . . ?
O71 C72' H72D 110.7 . . ?
C73 C72' H72D 110.7 . . ?
H72C C72' H72D 108.8 . . ?
C74 C73 C72' 106.6(8) . . ?
C74 C73 C72 97.0(9) . . ?
C72' C73 C72 32.8(6) . . ?
C74 C73 H73A 112.4 . . ?
C72' C73 H73A 131.1 . . ?
C72 C73 H73A 112.4 . . ?
C74 C73 H73B 112.4 . . ?
C72' C73 H73B 79.9 . . ?
C72 C73 H73B 112.4 . . ?
H73A C73 H73B 109.9 . . ?
C74 C73 H73C 110.4 . . ?
C72' C73 H73C 110.4 . . ?
C72 C73 H73C 85.6 . . ?
H73A C73 H73C 27.8 . . ?
H73B C73 H73C 130.5 . . ?
C74 C73 H73D 110.4 . . ?
C72' C73 H73D 110.4 . . ?
C72 C73 H73D 141.2 . . ?
H73A C73 H73D 82.6 . . ?
H73B C73 H73D 31.9 . . ?
H73C C73 H73D 108.6 . . ?
C73 C74 C75 105.7(7) . . ?
C73 C74 H74A 110.6 . . ?
C75 C74 H74A 110.6 . . ?
C73 C74 H74B 110.6 . . ?
C75 C74 H74B 110.6 . . ?
H74A C74 H74B 108.7 . . ?
O71 C75 C74 108.5(7) . . ?
O71 C75 H75A 110.0 . . ?
C74 C75 H75A 110.0 . . ?
O71 C75 H75B 110.0 . . ?
C74 C75 H75B 110.0 . . ?
H75A C75 H75B 108.4 . . ?
C82 C81 H81A 109.5 . . ?
C82 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C82 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C81 C82 C83 114.4(7) . . ?
C81 C82 H82A 108.7 . . ?
C83 C82 H82A 108.7 . . ?
C81 C82 H82B 108.7 . . ?
C83 C82 H82B 108.7 . . ?
H82A C82 H82B 107.6 . . ?
C83 C83 C82 114.6(9) 3_665 . ?
C83 C83 H83A 108.6 3_665 . ?
C82 C83 H83A 108.6 . . ?
C83 C83 H83B 108.6 3_665 . ?
C82 C83 H83B 108.6 . . ?
H83A C83 H83B 107.6 . . ?
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 N12 2.019(4) . ?
Zn1 N22 2.019(4) . ?
Zn1 N41 2.034(4) . ?
Zn1 O1 2.371(3) . ?
Zn1 Br1 2.4514(8) . ?
O1 B2 1.472(6) . ?
O1 B1 1.475(6) . ?
B1 N11 1.567(7) . ?
B1 N31 1.592(7) . ?
B1 C51 1.607(8) . ?
B2 N21 1.575(7) . ?
B2 C61 1.587(8) . ?
B2 N32 1.594(7) . ?
N11 C15 1.346(6) . ?
N11 N12 1.363(5) . ?
N12 C13 1.341(6) . ?
C13 C14 1.395(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.371(7) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
N21 C25 1.338(6) . ?
N21 N22 1.361(5) . ?
N22 C23 1.335(6) . ?
C23 C24 1.369(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.380(8) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
N31 C35 1.345(7) . ?
N31 N32 1.364(5) . ?
N32 C33 1.338(7) . ?
C33 C34 1.397(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.375(8) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
N41 C45 1.341(6) . ?
N41 N42 1.354(6) . ?
N42 C43 1.360(8) . ?
N42 H42 0.90(7) . ?
C43 C44 1.369(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.371(8) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C51 C52 1.407(6) . ?
C51 C56 1.414(7) . ?
C52 C53 1.400(8) . ?
C52 H52 0.9500 . ?
C53 C54 1.366(8) . ?
C53 H53 0.9500 . ?
C54 C55 1.378(7) . ?
C54 H54 0.9500 . ?
C55 C56 1.369(8) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C61 C66 1.390(7) . ?
C61 C62 1.418(7) . ?
C62 C63 1.383(8) . ?
C62 H62 0.9500 . ?
C63 C64 1.383(8) . ?
C63 H63 0.9500 . ?
C64 C65 1.381(9) . ?
C64 H64 0.9500 . ?
C65 C66 1.396(8) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
O71 C72 1.284(17) . ?
O71 C75 1.436(10) . ?
O71 C72' 1.449(14) . ?
C72 C73 1.629(18) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C72' C73 1.510(13) . ?
C72' H72C 0.9900 . ?
C72' H72D 0.9900 . ?
C73 C74 1.454(11) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C73 H73C 0.9900 . ?
C73 H73D 0.9900 . ?
C74 C75 1.470(11) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C81 C82 1.514(10) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 C83 1.516(11) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C83 C83 1.504(14) 3_665 ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N42 H42 O1 0.90(7) 2.20(8) 2.813(6) 125(6) .
C25 H25 O71 0.95 2.38 3.312(7) 168.4 .
C15 H15 Br1 0.95 2.90 3.799(5) 159.3 4_576
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N12 Zn1 O1 B2 128.7(3) . . . . ?
N22 Zn1 O1 B2 3.1(3) . . . . ?
N41 Zn1 O1 B2 -113.3(3) . . . . ?
Br1 Zn1 O1 B2 84.7(11) . . . . ?
N12 Zn1 O1 B1 -3.0(3) . . . . ?
N22 Zn1 O1 B1 -128.6(3) . . . . ?
N41 Zn1 O1 B1 115.0(3) . . . . ?
Br1 Zn1 O1 B1 -47.0(12) . . . . ?
B2 O1 B1 N11 -132.3(4) . . . . ?
Zn1 O1 B1 N11 -1.6(5) . . . . ?
B2 O1 B1 N31 -18.0(5) . . . . ?
Zn1 O1 B1 N31 112.7(3) . . . . ?
B2 O1 B1 C51 103.9(5) . . . . ?
Zn1 O1 B1 C51 -125.3(3) . . . . ?
B1 O1 B2 N21 129.8(4) . . . . ?
Zn1 O1 B2 N21 -1.0(5) . . . . ?
B1 O1 B2 C61 -104.2(5) . . . . ?
Zn1 O1 B2 C61 125.0(3) . . . . ?
B1 O1 B2 N32 17.5(5) . . . . ?
Zn1 O1 B2 N32 -113.2(3) . . . . ?
O1 B1 N11 C15 -174.0(5) . . . . ?
N31 B1 N11 C15 77.3(6) . . . . ?
C51 B1 N11 C15 -47.2(7) . . . . ?
O1 B1 N11 N12 8.5(6) . . . . ?
N31 B1 N11 N12 -100.2(5) . . . . ?
C51 B1 N11 N12 135.3(4) . . . . ?
C15 N11 N12 C13 1.1(6) . . . . ?
B1 N11 N12 C13 179.1(5) . . . . ?
C15 N11 N12 Zn1 169.5(4) . . . . ?
B1 N11 N12 Zn1 -12.5(6) . . . . ?
N22 Zn1 N12 C13 -120.2(5) . . . . ?
N41 Zn1 N12 C13 97.3(5) . . . . ?
O1 Zn1 N12 C13 173.4(5) . . . . ?
Br1 Zn1 N12 C13 -9.6(5) . . . . ?
N22 Zn1 N12 N11 74.5(4) . . . . ?
N41 Zn1 N12 N11 -67.9(4) . . . . ?
O1 Zn1 N12 N11 8.2(3) . . . . ?
Br1 Zn1 N12 N11 -174.8(3) . . . . ?
N11 N12 C13 C14 -1.7(6) . . . . ?
Zn1 N12 C13 C14 -168.5(4) . . . . ?
N12 C13 C14 C15 1.6(7) . . . . ?
N12 N11 C15 C14 -0.1(6) . . . . ?
B1 N11 C15 C14 -177.9(5) . . . . ?
C13 C14 C15 N11 -0.9(7) . . . . ?
O1 B2 N21 C25 -179.3(5) . . . . ?
C61 B2 N21 C25 53.3(7) . . . . ?
N32 B2 N21 C25 -71.9(6) . . . . ?
O1 B2 N21 N22 -3.2(6) . . . . ?
C61 B2 N21 N22 -130.6(5) . . . . ?
N32 B2 N21 N22 104.2(5) . . . . ?
C25 N21 N22 C23 -0.4(6) . . . . ?
B2 N21 N22 C23 -177.2(4) . . . . ?
C25 N21 N22 Zn1 -176.6(3) . . . . ?
B2 N21 N22 Zn1 6.6(6) . . . . ?
N12 Zn1 N22 C23 113.7(5) . . . . ?
N41 Zn1 N22 C23 -103.3(5) . . . . ?
O1 Zn1 N22 C23 179.9(5) . . . . ?
Br1 Zn1 N22 C23 4.2(5) . . . . ?
N12 Zn1 N22 N21 -71.2(4) . . . . ?
N41 Zn1 N22 N21 71.7(4) . . . . ?
O1 Zn1 N22 N21 -5.1(3) . . . . ?
Br1 Zn1 N22 N21 179.2(3) . . . . ?
N21 N22 C23 C24 0.2(6) . . . . ?
Zn1 N22 C23 C24 175.7(4) . . . . ?
N22 C23 C24 C25 0.1(7) . . . . ?
N22 N21 C25 C24 0.5(6) . . . . ?
B2 N21 C25 C24 177.0(5) . . . . ?
C23 C24 C25 N21 -0.3(7) . . . . ?
O1 B1 N31 C35 -169.6(6) . . . . ?
N11 B1 N31 C35 -56.1(8) . . . . ?
C51 B1 N31 C35 66.8(8) . . . . ?
O1 B1 N31 N32 10.7(5) . . . . ?
N11 B1 N31 N32 124.2(4) . . . . ?
C51 B1 N31 N32 -112.9(4) . . . . ?
C35 N31 N32 C33 -0.6(6) . . . . ?
B1 N31 N32 C33 179.2(4) . . . . ?
C35 N31 N32 B2 179.5(4) . . . . ?
B1 N31 N32 B2 -0.7(5) . . . . ?
O1 B2 N32 C33 170.6(6) . . . . ?
N21 B2 N32 C33 58.0(8) . . . . ?
C61 B2 N32 C33 -66.6(9) . . . . ?
O1 B2 N32 N31 -9.6(5) . . . . ?
N21 B2 N32 N31 -122.1(4) . . . . ?
C61 B2 N32 N31 113.3(4) . . . . ?
N31 N32 C33 C34 0.3(6) . . . . ?
B2 N32 C33 C34 -179.9(6) . . . . ?
N32 C33 C34 C35 0.1(7) . . . . ?
N32 N31 C35 C34 0.7(6) . . . . ?
B1 N31 C35 C34 -179.0(6) . . . . ?
C33 C34 C35 N31 -0.5(7) . . . . ?
N12 Zn1 N41 C45 -107.8(4) . . . . ?
N22 Zn1 N41 C45 107.5(4) . . . . ?
O1 Zn1 N41 C45 -179.7(4) . . . . ?
Br1 Zn1 N41 C45 -1.1(4) . . . . ?
N12 Zn1 N41 N42 69.8(4) . . . . ?
N22 Zn1 N41 N42 -75.0(4) . . . . ?
O1 Zn1 N41 N42 -2.2(4) . . . . ?
Br1 Zn1 N41 N42 176.5(3) . . . . ?
C45 N41 N42 C43 -0.3(6) . . . . ?
Zn1 N41 N42 C43 -178.4(4) . . . . ?
N41 N42 C43 C44 0.1(6) . . . . ?
N42 C43 C44 C45 0.2(6) . . . . ?
N42 N41 C45 C44 0.4(6) . . . . ?
Zn1 N41 C45 C44 178.4(4) . . . . ?
C43 C44 C45 N41 -0.4(6) . . . . ?
O1 B1 C51 C52 -98.9(6) . . . . ?
N11 B1 C51 C52 138.5(5) . . . . ?
N31 B1 C51 C52 16.3(6) . . . . ?
O1 B1 C51 C56 75.4(6) . . . . ?
N11 B1 C51 C56 -47.2(6) . . . . ?
N31 B1 C51 C56 -169.4(4) . . . . ?
C56 C51 C52 C53 -0.4(7) . . . . ?
B1 C51 C52 C53 174.1(5) . . . . ?
C51 C52 C53 C54 1.0(9) . . . . ?
C52 C53 C54 C55 -1.1(9) . . . . ?
C53 C54 C55 C56 0.6(8) . . . . ?
C54 C55 C56 C51 -0.1(8) . . . . ?
C52 C51 C56 C55 0.0(7) . . . . ?
B1 C51 C56 C55 -174.7(5) . . . . ?
O1 B2 C61 C66 94.1(6) . . . . ?
N21 B2 C61 C66 -142.2(5) . . . . ?
N32 B2 C61 C66 -20.3(7) . . . . ?
O1 B2 C61 C62 -80.5(6) . . . . ?
N21 B2 C61 C62 43.1(7) . . . . ?
N32 B2 C61 C62 165.0(5) . . . . ?
C66 C61 C62 C63 -1.2(9) . . . . ?
B2 C61 C62 C63 173.9(6) . . . . ?
C61 C62 C63 C64 1.6(10) . . . . ?
C62 C63 C64 C65 -0.8(10) . . . . ?
C63 C64 C65 C66 -0.3(10) . . . . ?
C62 C61 C66 C65 0.1(8) . . . . ?
B2 C61 C66 C65 -174.8(6) . . . . ?
C64 C65 C66 C61 0.6(10) . . . . ?
C75 O71 C72 C73 -47.5(14) . . . . ?
C72' O71 C72 C73 61.8(14) . . . . ?
C72 O71 C72' C73 -70.4(16) . . . . ?
C75 O71 C72' C73 9.9(12) . . . . ?
O71 C72' C73 C74 -20.2(13) . . . . ?
O71 C72' C73 C72 56.6(14) . . . . ?
O71 C72 C73 C74 37.8(15) . . . . ?
O71 C72 C73 C72' -72.1(16) . . . . ?
C72' C73 C74 C75 22.5(11) . . . . ?
C72 C73 C74 C75 -9.5(11) . . . . ?
C72 O71 C75 C74 41.4(12) . . . . ?
C72' O71 C75 C74 3.9(11) . . . . ?
C73 C74 C75 O71 -16.7(10) . . . . ?
C81 C82 C83 C83 -174.0(8) . . . 3_665 ?
