#------------------------------------------------------------------------------
#$Date: 2018-08-25 23:35:37 +0300 (Sat, 25 Aug 2018) $
#$Revision: 210140 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/84/4308436.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_4308436
loop_
_publ_author_name
'Matsunaga, Yuki'
'Fujisawa, Kiyoshi'
'Ibi, Naoko'
'Miyashita, Yoshitaro'
'Okamoto, Ken-ichi'
_publ_section_title
;
 Structural and Spectroscopic Characterization of First-Row
 Transition Metal(II) Substituted Blue Copper Model Complexes
 with Hydrotris(pyrazolyl)borate+
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              325
_journal_page_last               335
_journal_paper_doi               10.1021/ic049814x
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C33 H46 B F5 N6 S Zn '
_chemical_formula_sum            'C33 H46 B F5 N6 S Zn'
_chemical_formula_weight         730.01
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 114.020(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.983(10)
_cell_length_b                   16.105(11)
_cell_length_c                   18.54(1)
_cell_measurement_reflns_used    744
_cell_measurement_temperature    212.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      4.0
_cell_volume                     3814(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure Ver. 3.5.1'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.9655
_diffrn_measured_fraction_theta_max 0.9655
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.090
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30469
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998)  Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1528.00
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.65
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.646
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     470
_refine_ls_number_reflns         4640
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/σ²(Fo)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                4640
_reflns_number_total             8435
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic049814xsi20041011_033639_1.cif
_cod_data_source_block           '[ZnL(SC6F5)]'
_cod_original_cell_volume        3814.3(47)
_cod_original_formula_sum        'C33 H46 B F5 N6 S Zn '
_cod_database_code               4308436
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-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 0.67210(6) 0.44527(5) 0.87406(4) 0.0301(2) Uani 1.00 1 d . . .
S1 S 0.6398(2) 0.56415(13) 0.80467(13) 0.0616(6) Uani 1.00 1 d . . .
F41 F 0.5168(4) 0.4148(3) 0.7115(4) 0.090(2) Uani 1.00 1 d . . .
F42 F 0.3197(4) 0.4093(5) 0.6071(3) 0.112(2) Uani 1.00 1 d . . .
F43 F 0.2035(5) 0.5489(5) 0.5680(5) 0.174(3) Uani 1.00 1 d . . .
F44 F 0.2851(6) 0.6939(4) 0.6424(6) 0.188(4) Uani 1.00 1 d . . .
F45 F 0.4859(5) 0.7001(3) 0.7495(4) 0.100(2) Uani 1.00 1 d . . .
N21 N 0.7862(4) 0.4543(3) 0.9851(3) 0.032(2) Uani 1.00 1 d . . .
N22 N 0.8020(4) 0.3807(3) 1.0272(3) 0.032(2) Uani 1.00 1 d . . .
N31 N 0.7377(4) 0.3413(3) 0.8527(3) 0.029(2) Uani 1.00 1 d . . .
N32 N 0.7621(4) 0.2835(3) 0.9115(3) 0.030(2) Uani 1.00 1 d . . .
N11 N 0.5740(4) 0.3830(3) 0.9101(3) 0.033(2) Uani 1.00 1 d . . .
N12 N 0.6211(4) 0.3173(3) 0.9595(3) 0.033(2) Uani 1.00 1 d . . .
C21 C 0.813(2) 0.6576(7) 1.0357(11) 0.266(11) Uani 1.00 1 d . . .
C22 C 0.9585(11) 0.6204(7) 1.0109(12) 0.214(9) Uani 1.00 1 d . . .
C23 C 0.8533(6) 0.5964(5) 1.0025(5) 0.050(2) Uani 1.00 1 d . . .
C24 C 0.8487(5) 0.5103(5) 1.0326(4) 0.042(2) Uani 1.00 1 d . . .
C25 C 0.9060(6) 0.4758(4) 1.1066(4) 0.046(2) Uani 1.00 1 d . . .
C26 C 0.8742(5) 0.3932(4) 1.1022(4) 0.040(2) Uani 1.00 1 d . . .
C27 C 0.9122(7) 0.3271(5) 1.1644(4) 0.058(3) Uani 1.00 1 d . . .
C28 C 0.8391(9) 0.3186(7) 1.2052(6) 0.111(5) Uani 1.00 1 d . . .
C29 C 1.0223(7) 0.3400(7) 1.2208(6) 0.109(4) Uani 1.00 1 d . . .
C31 C 0.7157(8) 0.3079(6) 0.6529(5) 0.092(4) Uani 1.00 1 d . . .
C32 C 0.8589(7) 0.3994(6) 0.7362(5) 0.084(4) Uani 1.00 1 d . . .
C33 C 0.7552(5) 0.3590(4) 0.7250(4) 0.036(2) Uani 1.00 1 d . . .
C34 C 0.7673(5) 0.3108(4) 0.7980(4) 0.032(2) Uani 1.00 1 d . . .
C35 C 0.8099(5) 0.2329(4) 0.8214(4) 0.041(2) Uani 1.00 1 d . . .
C36 C 0.8070(5) 0.2168(4) 0.8931(4) 0.034(2) Uani 1.00 1 d . . .
C37 C 0.8428(6) 0.1412(4) 0.9436(4) 0.047(2) Uani 1.00 1 d . . .
C39 C 0.7981(9) 0.0639(5) 0.8982(6) 0.106(4) Uani 1.00 1 d . . .
C38 C 0.9611(7) 0.1355(6) 0.9806(7) 0.116(4) Uani 1.00 1 d . . .
C11 C 0.2958(6) 0.4140(6) 0.7946(5) 0.080(3) Uani 1.00 1 d . . .
C12 C 0.3831(8) 0.5150(6) 0.9033(6) 0.104(4) Uani 1.00 1 d . . .
C13 C 0.3997(5) 0.4489(5) 0.8505(4) 0.048(2) Uani 1.00 1 d . . .
C14 C 0.4732(5) 0.3824(4) 0.8991(4) 0.037(2) Uani 1.00 1 d . . .
C15 C 0.4555(6) 0.3175(5) 0.9398(4) 0.050(3) Uani 1.00 1 d . . .
C16 C 0.5487(5) 0.2764(4) 0.9770(4) 0.041(2) Uani 1.00 1 d . . .
C17 C 0.5711(7) 0.1995(5) 1.0263(6) 0.066(3) Uani 1.00 1 d . . .
C18 C 0.5516(9) 0.1224(6) 0.9723(7) 0.114(5) Uani 1.00 1 d . . .
C19 C 0.5094(10) 0.1945(8) 1.0761(7) 0.142(6) Uani 1.00 1 d . . .
C40 C 0.5117(5) 0.5594(5) 0.7339(4) 0.042(2) Uani 1.00 1 d . . .
C41 C 0.4647(6) 0.4865(5) 0.6940(5) 0.050(3) Uani 1.00 1 d . . .
C42 C 0.3611(8) 0.4834(8) 0.6393(5) 0.075(4) Uani 1.00 1 d . . .
C43 C 0.3015(7) 0.5511(9) 0.6195(7) 0.096(4) Uani 1.00 1 d . . .
C44 C 0.3413(9) 0.6246(7) 0.6562(7) 0.088(4) Uani 1.00 1 d . . .
C45 C 0.4490(9) 0.6281(6) 0.7143(6) 0.070(4) Uani 1.00 1 d . . .
B1 B 0.7394(6) 0.3016(4) 0.9857(4) 0.029(2) Uani 1.00 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn 0.284 1.430
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.125 0.123
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.017 0.010
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.006 0.003
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
B B 0.001 0.001
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 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_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
S1 Zn1 N21 114.3(2) yes . . .
S1 Zn1 N31 126.4(2) yes . . .
S1 Zn1 N11 127.4(2) yes . . .
N21 Zn1 N31 91.5(2) yes . . .
N21 Zn1 N11 93.4(2) yes . . .
N31 Zn1 N11 94.4(2) yes . . .
C40 S1 Zn1 107.4(3) yes . . .
N22 N21 C24 107.4(5) yes . . .
N22 N21 Zn1 112.9(3) yes . . .
C24 N21 Zn1 139.6(5) yes . . .
C26 N22 B1 131.3(5) yes . . .
C26 N22 N21 109.3(5) yes . . .
B1 N22 N21 119.4(4) yes . . .
N32 N31 C34 107.5(5) yes . . .
N32 N31 Zn1 113.1(4) yes . . .
C34 N31 Zn1 139.3(4) yes . . .
C36 N32 B1 130.7(5) yes . . .
C36 N32 N31 109.2(6) yes . . .
B1 N32 N31 120.1(5) yes . . .
N12 N11 C14 106.4(6) yes . . .
N12 N11 Zn1 113.4(4) yes . . .
C14 N11 Zn1 140.2(4) yes . . .
C16 N12 B1 131.0(5) yes . . .
C16 N12 N11 109.4(5) yes . . .
B1 N12 N11 119.6(6) yes . . .
C24 C23 C21 113(1) yes . . .
C24 C23 C22 113.3(7) yes . . .
C21 C23 C22 109(1) yes . . .
C25 C24 N21 110.2(6) yes . . .
C25 C24 C23 129.7(6) yes . . .
N21 C24 C23 120.0(6) yes . . .
C26 C25 C24 106.3(6) yes . . .
C27 C26 N22 124.4(6) yes . . .
C27 C26 C25 128.8(6) yes . . .
N22 C26 C25 106.8(6) yes . . .
C28 C27 C29 112.4(8) yes . . .
C28 C27 C26 110.5(8) yes . . .
C29 C27 C26 112.6(8) yes . . .
C34 C33 C31 112.9(6) yes . . .
C34 C33 C32 110.1(5) yes . . .
C31 C33 C32 110.4(8) yes . . .
C35 C34 N31 108.9(6) yes . . .
C35 C34 C33 128.7(7) yes . . .
N31 C34 C33 122.4(6) yes . . .
C36 C35 C34 107.3(7) yes . . .
C37 C36 N32 124.1(7) yes . . .
C37 C36 C35 128.9(7) yes . . .
N32 C36 C35 107.1(6) yes . . .
C39 C37 C38 109.6(8) yes . . .
C39 C37 C36 111.8(6) yes . . .
C38 C37 C36 111.1(7) yes . . .
C14 C13 C11 112.3(7) yes . . .
C14 C13 C12 110.9(6) yes . . .
C11 C13 C12 110.2(7) yes . . .
C15 C14 N11 109.7(6) yes . . .
C15 C14 C13 129.9(7) yes . . .
N11 C14 C13 120.4(7) yes . . .
C16 C15 C14 107.4(7) yes . . .
C17 C16 N12 124.0(7) yes . . .
C17 C16 C15 128.9(8) yes . . .
N12 C16 C15 107.1(6) yes . . .
C18 C17 C19 111.2(9) yes . . .
C18 C17 C16 109.4(8) yes . . .
C19 C17 C16 113.0(8) yes . . .
C41 C40 C45 115.2(6) yes . . .
C41 C40 S1 123.6(6) yes . . .
C45 C40 S1 121.1(6) yes . . .
C42 C41 F41 116.7(8) yes . . .
C42 C41 C40 122.8(8) yes . . .
F41 C41 C40 120.4(6) yes . . .
C43 C42 F42 119.5(8) yes . . .
C43 C42 C41 121(1) yes . . .
F42 C42 C41 119.1(9) yes . . .
C44 C43 F43 118(1) yes . . .
C44 C43 C42 119.4(9) yes . . .
F43 C43 C42 121(1) yes . . .
C45 C44 F44 117.7(9) yes . . .
C45 C44 C43 119(1) yes . . .
F44 C44 C43 122.9(9) yes . . .
F45 C45 C40 119.9(8) yes . . .
F45 C45 C44 118.4(9) yes . . .
C40 C45 C44 121.7(8) yes . . .
N22 B1 N32 108.2(6) yes . . .
N22 B1 N12 109.7(5) yes . . .
N32 B1 N12 109.3(5) yes . . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Zn1 S1 2.248(2) yes . .
Zn1 N21 2.032(4) yes . .
Zn1 N31 2.024(6) yes . .
Zn1 N11 2.019(6) yes . .
S1 C40 1.739(6) yes . .
F41 C41 1.33(1) yes . .
F42 C42 1.35(1) yes . .
F43 C43 1.31(1) yes . .
F44 C44 1.33(1) yes . .
F45 C45 1.33(1) yes . .
N21 N22 1.387(7) yes . .
N21 C24 1.315(8) yes . .
N22 C26 1.360(8) yes . .
N22 B1 1.559(8) yes . .
N31 N32 1.368(7) yes . .
N31 C34 1.34(1) yes . .
N32 C36 1.357(9) yes . .
N32 B1 1.56(1) yes . .
N11 N12 1.379(7) yes . .
N11 C14 1.340(9) yes . .
N12 C16 1.35(1) yes . .
N12 B1 1.543(9) yes . .
C21 C23 1.40(2) yes . .
C22 C23 1.47(2) yes . .
C23 C24 1.50(1) yes . .
C24 C25 1.392(9) yes . .
C25 C26 1.39(1) yes . .
C26 C27 1.50(1) yes . .
C27 C28 1.51(2) yes . .
C27 C29 1.48(1) yes . .
C31 C33 1.47(1) yes . .
C32 C33 1.52(1) yes . .
C33 C34 1.51(1) yes . .
C34 C35 1.381(9) yes . .
C35 C36 1.37(1) yes . .
C36 C37 1.492(9) yes . .
C37 C39 1.49(1) yes . .
C37 C38 1.51(1) yes . .
C11 C13 1.51(1) yes . .
C12 C13 1.53(1) yes . .
C13 C14 1.504(9) yes . .
C14 C15 1.37(1) yes . .
C15 C16 1.37(1) yes . .
C16 C17 1.49(1) yes . .
C17 C18 1.55(1) yes . .
C17 C19 1.50(2) yes . .
C40 C41 1.40(1) yes . .
C40 C45 1.37(1) yes . .
C41 C42 1.39(1) yes . .
C42 C43 1.33(2) yes . .
C43 C44 1.37(2) yes . .
C44 C45 1.45(1) yes . .
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_publ_flag
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
N21 Zn1 S1 C40 -154.8(3) yes . . . .
S1 Zn1 N21 N22 178.1(4) yes . . . .
S1 Zn1 N31 N32 170.6(3) yes . . . .
S1 Zn1 N11 N12 -172.8(3) yes . . . .
Zn1 S1 C40 C41 -36.9(8) yes . . . .
Zn1 N21 N22 C26 -176.0(5) yes . . . .
Zn1 N21 C24 C23 -6(1) yes . . . .
N21 N22 C26 C25 -1.3(9) yes . . . .
N21 N22 B1 N32 57.3(8) yes . . . .
N21 N22 B1 N12 -61.8(8) yes . . . .
Zn1 N31 N32 C36 -179.0(4) yes . . . .
Zn1 N31 C34 C33 0(1) yes . . . .
N31 N32 C36 C35 -0.5(7) yes . . . .
N31 N32 B1 N22 -60.0(6) yes . . . .
N31 N32 B1 N12 59.4(7) yes . . . .
Zn1 N11 N12 C16 -176.5(5) yes . . . .
Zn1 N11 C14 C13 -6(1) yes . . . .
N11 N12 C16 C15 -1.2(8) yes . . . .
N11 N12 B1 N22 57.0(8) yes . . . .
N11 N12 B1 N32 -61.5(7) yes . . . .
C21 C23 C24 N21 112.4(8) yes . . . .
C22 C23 C24 N21 -121.8(8) yes . . . .
N21 C24 C25 C26 0(1) yes . . . .
C24 C25 C26 N22 0(1) yes . . . .
N22 C26 C27 C28 -84(1) yes . . . .
C31 C33 C34 N31 -136.9(6) yes . . . .
C32 C33 C34 N31 99.2(7) yes . . . .
N31 C34 C35 C36 -0.9(7) yes . . . .
C34 C35 C36 N32 0.8(7) yes . . . .
N32 C36 C37 C39 127.2(9) yes . . . .
C11 C13 C14 N11 136.1(7) yes . . . .
C12 C13 C14 N11 -100.1(8) yes . . . .
N11 C14 C15 C16 -0.2(9) yes . . . .
C14 C15 C16 N12 0.8(9) yes . . . .
N12 C16 C17 C18 -90(1) yes . . . .
S1 C40 C41 F41 2(1) yes . . . .
S1 C40 C45 F45 0(1) yes . . . .
S1 C40 C45 C44 -178(1) yes . . . .
F41 C41 C42 F42 0(1) yes . . . .
C40 C41 C42 F42 -175.8(9) yes . . . .
F42 C42 C43 F43 -1(1) yes . . . .
C41 C42 C43 F43 -179(719) yes . . . .
F43 C43 C44 F44 0(2) yes . . . .
C42 C43 C44 F44 -176(1) yes . . . .
F44 C44 C45 F45 0(2) yes . . . .
F44 C44 C45 C40 178(1) yes . . . .
C43 C44 C45 F45 -179(622) yes . . . .
C43 C44 C45 C40 0(2) yes . . . .
