#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:19:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179407 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/04/4330480.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_4330480
loop_
_publ_author_name
'Ai-Xia Zheng'
'Jing Si'
'Xiao-Yan Tang'
'Li-Li Miao'
'Miao Yu'
'Kai-Peng Hou'
'Fan Wang'
'Hong-Xi Li'
'Jian-Ping Lang'
_publ_contact_author_address
;         
College of Chemistry, Chemical Engineering and Materials Science 
Suzhou University, Suzhou 215123, Jiangsu, 
P. R. China
;
_publ_contact_author_email       jplang@suda.edu.cn
_publ_contact_author_fax         86-512-65880089
_publ_contact_author_name        'Jian-Ping Lang'
_publ_contact_author_phone       86-512-65882865
_publ_section_title
;
 Reactions of the Cationic Zinc Thiolate Model Complex [Zn(Tab)4](PF6)2
 with N-Donor Ligands and Cobalt Dichloride
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10262
_journal_page_last               10273
_journal_paper_doi               10.1021/ic301191n
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C29 H35 N7 S2 Zn, 2(F6 P)'
_chemical_formula_sum            'C29 H35 F12 N7 P2 S2 Zn'
_chemical_formula_weight         901.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 106.03(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.349(7)
_cell_length_b                   10.044(2)
_cell_length_c                   10.502(2)
_cell_measurement_reflns_used    5372
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      3.0355
_cell_volume                     3583.7(13)
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku MercuryCCD area detector'
_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  0.0947
_diffrn_reflns_av_sigmaI/netI    0.1218
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10814
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  0.8268
_exptl_absorpt_correction_T_min  0.8268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4051
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.876
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.0818
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1201P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2016
_refine_ls_wR_factor_ref         0.2325
_reflns_number_gt                1765
_reflns_number_total             4051
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301191n_si_002_5.cif
_cod_data_source_block           5
_cod_original_cell_volume        3583.8(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4330480
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'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
Zn1 Zn 0.5000 0.20603(10) 0.2500 0.0477(3) Uani 1 2 d S
S1 S 0.54541(4) 0.1007(2) 0.16046(16) 0.0630(5) Uani 1 1 d .
N1 N 0.69318(14) 0.1085(5) 0.6243(5) 0.0552(12) Uani 1 1 d U
N3 N 0.46271(13) 0.2689(5) 0.0475(5) 0.0488(12) Uani 1 1 d .
N4 N 0.5000 0.4164(7) 0.2500 0.0514(17) Uani 1 2 d S
P1 P 0.32049(6) 0.6196(2) -0.0330(2) 0.0708(6) Uani 1 1 d .
F1 F 0.3013(5) 0.7294(8) 0.0241(10) 0.280(7) Uani 1 1 d .
F2 F 0.3276(3) 0.5379(7) 0.0957(6) 0.210(4) Uani 1 1 d .
F3 F 0.34171(18) 0.5118(7) -0.0855(8) 0.162(3) Uani 1 1 d .
F4 F 0.31041(19) 0.7016(7) -0.1652(6) 0.139(2) Uani 1 1 d .
F5 F 0.3601(3) 0.6941(7) 0.0113(11) 0.252(6) Uani 1 1 d .
F6 F 0.28141(15) 0.5425(7) -0.0852(8) 0.162(3) Uani 1 1 d .
C1 C 0.58816(17) 0.1013(6) 0.2963(6) 0.0528(15) Uani 1 1 d .
C2 C 0.61634(19) 0.2023(7) 0.3112(7) 0.0625(17) Uani 1 1 d .
H2A H 0.6124 0.2694 0.2464 0.075 Uiso 1 1 calc R
C3 C 0.64956(19) 0.2074(7) 0.4168(7) 0.0604(16) Uani 1 1 d .
H3A H 0.6672 0.2790 0.4258 0.072 Uiso 1 1 calc R
C4 C 0.65674(16) 0.1061(6) 0.5097(6) 0.0499(14) Uani 1 1 d .
C5 C 0.63033(18) 0.0019(7) 0.4959(6) 0.0558(15) Uani 1 1 d .
H5A H 0.6353 -0.0679 0.5581 0.067 Uiso 1 1 calc R
C6 C 0.59679(17) 0.0004(7) 0.3912(6) 0.0578(16) Uani 1 1 d .
H6A H 0.5791 -0.0710 0.3834 0.069 Uiso 1 1 calc R
C7 C 0.7040(3) 0.2466(10) 0.6749(11) 0.125(4) Uani 1 1 d U
H7A H 0.7071 0.3025 0.6032 0.188 Uiso 1 1 calc R
H7B H 0.7285 0.2442 0.7450 0.188 Uiso 1 1 calc R
H7C H 0.6833 0.2825 0.7094 0.188 Uiso 1 1 calc R
C8 C 0.7259(2) 0.0502(10) 0.5868(8) 0.104(3) Uani 1 1 d U
H8A H 0.7298 0.0972 0.5107 0.157 Uiso 1 1 calc R
H8B H 0.7203 -0.0428 0.5642 0.157 Uiso 1 1 calc R
H8C H 0.7495 0.0569 0.6602 0.157 Uiso 1 1 calc R
C9 C 0.6886(2) 0.0314(11) 0.7418(8) 0.104(3) Uani 1 1 d U
H9A H 0.7129 0.0362 0.8128 0.156 Uiso 1 1 calc R
H9B H 0.6828 -0.0609 0.7168 0.156 Uiso 1 1 calc R
H9C H 0.6673 0.0691 0.7716 0.156 Uiso 1 1 calc R
N2 N 0.44006(14) 0.2171(6) -0.0647(5) 0.0565(13) Uani 1 1 d .
H2B H 0.4392 0.1325 -0.0833 0.068 Uiso 1 1 calc R
C10 C 0.41847(18) 0.3107(9) -0.1467(7) 0.070(2) Uani 1 1 d .
H10A H 0.4005 0.2962 -0.2301 0.083 Uiso 1 1 calc R
C11 C 0.42813(19) 0.4306(8) -0.0835(7) 0.0670(19) Uani 1 1 d .
H11A H 0.4185 0.5153 -0.1141 0.080 Uiso 1 1 calc R
C12 C 0.45554(17) 0.3987(7) 0.0367(6) 0.0562(16) Uani 1 1 d .
C13 C 0.47749(17) 0.4834(7) 0.1452(7) 0.0563(16) Uani 1 1 d .
C14 C 0.4768(2) 0.6227(7) 0.1406(8) 0.0690(19) Uani 1 1 d .
H14A H 0.4613 0.6684 0.0663 0.083 Uiso 1 1 calc R
C15 C 0.5000 0.6915(11) 0.2500 0.079(3) Uani 1 2 d S
H15 H 0.5000 0.7851 0.2500 0.095 Uiso 1 2 calc SR
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
N4 Zn1 N3 73.79(13) . 2_655
N4 Zn1 N3 73.79(13) . .
N3 Zn1 N3 147.6(3) 2_655 .
N4 Zn1 S1 117.03(5) . .
N3 Zn1 S1 102.66(12) 2_655 .
N3 Zn1 S1 91.99(13) . .
N4 Zn1 S1 117.03(5) . 2_655
N3 Zn1 S1 91.99(13) 2_655 2_655
N3 Zn1 S1 102.66(12) . 2_655
S1 Zn1 S1 125.93(11) . 2_655
C1 S1 Zn1 101.76(19) . .
C8 N1 C7 109.2(7) . .
C8 N1 C4 110.4(5) . .
C7 N1 C4 112.2(6) . .
C8 N1 C9 106.9(7) . .
C7 N1 C9 105.1(7) . .
C4 N1 C9 112.8(5) . .
C12 N3 N2 104.7(5) . .
C12 N3 Zn1 113.7(4) . .
N2 N3 Zn1 140.7(4) . .
C13 N4 C13 120.1(8) 2_655 .
C13 N4 Zn1 120.0(4) 2_655 .
C13 N4 Zn1 120.0(4) . .
F1 P1 F3 177.1(7) . .
F1 P1 F5 89.8(7) . .
F3 P1 F5 87.5(6) . .
F1 P1 F2 91.3(5) . .
F3 P1 F2 87.8(5) . .
F5 P1 F2 94.6(5) . .
F1 P1 F6 92.9(7) . .
F3 P1 F6 89.8(4) . .
F5 P1 F6 176.5(6) . .
F2 P1 F6 87.5(5) . .
F1 P1 F4 87.2(4) . .
F3 P1 F4 93.9(4) . .
F5 P1 F4 88.7(4) . .
F2 P1 F4 176.4(5) . .
F6 P1 F4 89.3(4) . .
C6 C1 C2 116.0(6) . .
C6 C1 S1 122.9(5) . .
C2 C1 S1 121.0(5) . .
C3 C2 C1 122.6(6) . .
C3 C2 H2A 118.7 . .
C1 C2 H2A 118.7 . .
C2 C3 C4 119.4(6) . .
C2 C3 H3A 120.3 . .
C4 C3 H3A 120.3 . .
C3 C4 C5 119.7(6) . .
C3 C4 N1 120.2(6) . .
C5 C4 N1 120.1(6) . .
C6 C5 C4 119.9(6) . .
C6 C5 H5A 120.0 . .
C4 C5 H5A 120.0 . .
C5 C6 C1 122.2(6) . .
C5 C6 H6A 118.9 . .
C1 C6 H6A 118.9 . .
N1 C7 H7A 109.5 . .
N1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
N1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N1 C8 H8A 109.5 . .
N1 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
N1 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N1 C9 H9A 109.5 . .
N1 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N1 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N3 N2 C10 112.7(6) . .
N3 N2 H2B 123.7 . .
C10 N2 H2B 123.7 . .
N2 C10 C11 106.2(6) . .
N2 C10 H10A 126.9 . .
C11 C10 H10A 126.9 . .
C10 C11 C12 104.7(6) . .
C10 C11 H11A 127.7 . .
C12 C11 H11A 127.7 . .
N3 C12 C11 111.7(6) . .
N3 C12 C13 117.3(6) . .
C11 C12 C13 131.0(7) . .
N4 C13 C14 121.9(7) . .
N4 C13 C12 114.4(6) . .
C14 C13 C12 123.7(7) . .
C15 C14 C13 117.8(8) . .
C15 C14 H14A 121.1 . .
C13 C14 H14A 121.1 . .
C14 C15 C14 120.7(10) . 2_655
C14 C15 H15 119.7 . .
C14 C15 H15 119.7 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N4 2.113(7) .
Zn1 N3 2.261(5) 2_655
Zn1 N3 2.261(5) .
Zn1 S1 2.3267(16) .
Zn1 S1 2.3267(16) 2_655
S1 C1 1.769(6) .
N1 C8 1.444(8) .
N1 C7 1.496(10) .
N1 C4 1.501(7) .
N1 C9 1.503(9) .
N3 C12 1.328(8) .
N3 N2 1.334(7) .
N4 C13 1.347(7) 2_655
N4 C13 1.347(7) .
P1 F1 1.504(7) .
P1 F3 1.506(6) .
P1 F5 1.542(7) .
P1 F2 1.542(6) .
P1 F6 1.546(6) .
P1 F4 1.568(6) .
C1 C6 1.395(9) .
C1 C2 1.401(9) .
C2 C3 1.375(9) .
C2 H2A 0.9400 .
C3 C4 1.384(9) .
C3 H3A 0.9400 .
C4 C5 1.383(8) .
C5 C6 1.377(9) .
C5 H5A 0.9400 .
C6 H6A 0.9400 .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C7 H7C 0.9700 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C8 H8C 0.9700 .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C9 H9C 0.9700 .
N2 C10 1.358(8) .
N2 H2B 0.8700 .
C10 C11 1.372(10) .
C10 H10A 0.9400 .
C11 C12 1.400(9) .
C11 H11A 0.9400 .
C12 C13 1.461(9) .
C13 C14 1.400(9) .
C14 C15 1.396(9) .
C14 H14A 0.9400 .
C15 C14 1.396(9) 2_655
C15 H15 0.9400 .
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
C5 H5A F5 0.94 2.52 3.113(10) 121.4 2_645
C8 H8B F1 0.97 2.51 3.470(13) 171.6 2_645
C9 H9B F4 0.97 2.47 3.412(13) 162.7 2_645
C7 H7A F6 0.97 2.46 3.203(13) 133.2 2_655
C9 H9A F6 0.97 2.36 3.283(10) 158.1 3_546
N2 H2B S1 0.87 2.59 3.428(6) 163.3 5_655
