#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:14:31 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180067 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/13/7051353.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_7051353
loop_
_publ_author_name
'Liu Ze-hua'
'Duan Chun-ying'
'Li Ji-hui'
'Liu Yong-jiang'
'Mei Yu-hua'
'You Xiao-zeng'
_publ_section_title
;
 Structural dependence of π--π interactions in dithiocarbazato and
 thiosemicarbazato nickel complexes
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              1057
_journal_page_last               1062
_journal_paper_doi               10.1039/b004846l
_journal_volume                  24
_journal_year                    2000
_chemical_formula_sum            'C42 H30 N4 Ni S4'
_chemical_formula_weight         777.65
_chemical_name_systematic
; 
bis(fluorene-9-one S-phenyl-dithiocarbazato)nickel 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.772(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9236(11)
_cell_length_b                   21.696(3)
_cell_length_c                   18.933(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.41
_cell_measurement_theta_min      4.60
_cell_volume                     3601.0(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2θ/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  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7019
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        18.25
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.4644
_exptl_absorpt_correction_T_min  0.4305
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.074
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.264
_refine_ls_restrained_S_obs      1.083
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_obs          0.0490
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0447P)²+3.0244P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1571
_refine_ls_wR_factor_obs         0.1103
_reflns_number_observed          4304
_reflns_number_total             6247
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004846l.txt
_cod_data_source_block           nickel_complex_3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+3.0244P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+3.0244P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3600.9(8)
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               7051353
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni1 Ni 0.11162(6) 0.24510(2) 0.76095(3) 0.0422(2) Uani 1 d . .
S1 S 0.26950(14) 0.16931(5) 0.77975(6) 0.0560(3) Uani 1 d . .
S2 S -0.07295(13) 0.18106(4) 0.73111(6) 0.0555(3) Uani 1 d . .
S3 S 0.5737(2) 0.17321(6) 0.86864(7) 0.0718(4) Uani 1 d . .
S4 S -0.37604(15) 0.21021(6) 0.64872(7) 0.0667(3) Uani 1 d . .
N1 N 0.4232(4) 0.27418(14) 0.8173(2) 0.0489(8) Uani 1 d . .
N2 N 0.2917(4) 0.29693(14) 0.7726(2) 0.0429(8) Uani 1 d . .
N3 N -0.1846(4) 0.29639(14) 0.7112(2) 0.0482(8) Uani 1 d . .
N4 N -0.0463(4) 0.30672(13) 0.7585(2) 0.0433(8) Uani 1 d . .
C1 C 0.4201(5) 0.2149(2) 0.8211(2) 0.0479(10) Uani 1 d . .
C2 C 0.3025(4) 0.3548(2) 0.7530(2) 0.0430(9) Uani 1 d . .
C3 C 0.5446(7) 0.5123(2) 0.8387(3) 0.0752(15) Uani 1 d . .
H3A H 0.5915(7) 0.5489(2) 0.8563(3) 0.090 Uiso 1 calc R .
C4 C 0.4240(6) 0.5140(2) 0.7818(3) 0.0682(14) Uani 1 d . .
H4A H 0.3883(6) 0.5514(2) 0.7613(3) 0.082 Uiso 1 calc R .
C5 C 0.5967(6) 0.4575(2) 0.8699(3) 0.0700(14) Uani 1 d . .
H5A H 0.6783(6) 0.4575(2) 0.9085(3) 0.084 Uiso 1 calc R .
C6 C 0.5292(5) 0.4017(2) 0.8447(2) 0.0574(11) Uani 1 d . .
H6A H 0.5642(5) 0.3646(2) 0.8663(2) 0.069 Uiso 1 calc R .
C7 C 0.4095(5) 0.4029(2) 0.7870(2) 0.0492(10) Uani 1 d . .
C8 C 0.3565(5) 0.4593(2) 0.7555(2) 0.0501(10) Uani 1 d . .
C9 C 0.2294(5) 0.4480(2) 0.6964(2) 0.0513(11) Uani 1 d . .
C10 C 0.1963(5) 0.3843(2) 0.6938(2) 0.0450(9) Uani 1 d . .
C11 C 0.0908(5) 0.3597(2) 0.6385(2) 0.0578(11) Uani 1 d . .
H11A H 0.0743(5) 0.3174(2) 0.6351(2) 0.069 Uiso 1 calc R .
C12 C 0.0096(6) 0.3997(3) 0.5880(3) 0.0734(14) Uani 1 d . .
H12A H -0.0627(6) 0.3841(3) 0.5505(3) 0.088 Uiso 1 calc R .
C13 C 0.0355(6) 0.4627(3) 0.5931(3) 0.076(2) Uani 1 d . .
H13A H -0.0228(6) 0.4890(3) 0.5601(3) 0.091 Uiso 1 calc R .
C14 C 0.1461(6) 0.4871(2) 0.6463(3) 0.0680(13) Uani 1 d . .
H14A H 0.1646(6) 0.5293(2) 0.6484(3) 0.082 Uiso 1 calc R .
C15 C 0.7200(5) 0.2307(2) 0.8921(3) 0.0676(13) Uani 1 d . .
H15A H 0.7970(5) 0.2353(2) 0.8655(3) 0.081 Uiso 1 calc R .
C16 C 0.7142(5) 0.2713(2) 0.9561(2) 0.0530(11) Uani 1 d . .
C17 C 0.6128(6) 0.2644(2) 1.0010(3) 0.0670(13) Uani 1 d . .
H17A H 0.5402(6) 0.2331(2) 0.9930(3) 0.080 Uiso 1 calc R .
C18 C 0.6180(7) 0.3044(3) 1.0595(3) 0.081(2) Uani 1 d . .
H18A H 0.5486(7) 0.2996(3) 1.0901(3) 0.097 Uiso 1 calc R .
C19 C 0.7230(8) 0.3501(3) 1.0720(3) 0.088(2) Uani 1 d . .
H19A H 0.7241(8) 0.3769(3) 1.1104(3) 0.105 Uiso 1 calc R .
C20 C 0.8269(7) 0.3568(3) 1.0282(3) 0.089(2) Uani 1 d . .
H20A H 0.9007(7) 0.3875(3) 1.0372(3) 0.106 Uiso 1 calc R .
C21 C 0.8215(6) 0.3177(2) 0.9708(3) 0.0718(14) Uani 1 d . .
H21A H 0.8923(6) 0.3226(2) 0.9409(3) 0.086 Uiso 1 calc R .
C22 C -0.2054(5) 0.2379(2) 0.6986(2) 0.0482(10) Uani 1 d . .
C23 C -0.0348(5) 0.3617(2) 0.7880(2) 0.0435(9) Uani 1 d . .
C24 C -0.0860(8) 0.5275(2) 0.7883(4) 0.092(2) Uani 1 d . .
H24A H -0.0373(8) 0.5600(2) 0.8154(4) 0.111 Uiso 1 calc R .
C25 C -0.2002(9) 0.5386(3) 0.7305(4) 0.106(3) Uani 1 d . .
H25A H -0.2286(9) 0.5791(3) 0.7188(4) 0.127 Uiso 1 calc R .
C26 C -0.2752(7) 0.4910(3) 0.6888(3) 0.088(2) Uani 1 d . .
H26A H -0.3528(7) 0.5000(3) 0.6501(3) 0.106 Uiso 1 calc R .
C27 C -0.2340(6) 0.4295(2) 0.7050(3) 0.0667(13) Uani 1 d . .
H27A H -0.2828(6) 0.3973(2) 0.6776(3) 0.080 Uiso 1 calc R .
C28 C -0.1186(5) 0.4187(2) 0.7630(3) 0.0541(11) Uani 1 d . .
C29 C -0.0444(6) 0.4668(2) 0.8057(3) 0.0666(14) Uani 1 d . .
C30 C 0.0744(6) 0.4419(2) 0.8621(3) 0.0679(14) Uani 1 d . .
C31 C 0.0796(5) 0.3779(2) 0.8520(2) 0.0519(11) Uani 1 d . .
C32 C 0.1704(5) 0.3414(2) 0.9018(2) 0.0634(12) Uani 1 d . .
H32A H 0.1693(5) 0.2988(2) 0.8970(2) 0.076 Uiso 1 calc R .
C33 C 0.2643(7) 0.3699(3) 0.9598(3) 0.092(2) Uani 1 d . .
H33A H 0.3279(7) 0.3461(3) 0.9937(3) 0.111 Uiso 1 calc R .
C34 C 0.2638(9) 0.4328(4) 0.9673(4) 0.120(3) Uani 1 d . .
H34A H 0.3292(9) 0.4511(4) 1.0055(4) 0.144 Uiso 1 calc R .
C35 C 0.1694(8) 0.4687(3) 0.9199(4) 0.106(2) Uani 1 d . .
H35A H 0.1686(8) 0.5111(3) 0.9263(4) 0.127 Uiso 1 calc R .
C36 C -0.4898(5) 0.2792(2) 0.6294(2) 0.0617(12) Uani 1 d . .
H36A H -0.5601(5) 0.2908(2) 0.6576(2) 0.074 Uiso 1 calc R .
C37 C -0.4663(5) 0.3172(2) 0.5660(2) 0.0577(11) Uani 1 d . .
C38 C -0.5544(7) 0.3690(3) 0.5501(3) 0.090(2) Uani 1 d . .
H38A H -0.6252(7) 0.3792(3) 0.5785(3) 0.108 Uiso 1 calc R .
C39 C -0.5396(9) 0.4064(3) 0.4926(4) 0.115(2) Uani 1 d . .
H39A H -0.5973(9) 0.4422(3) 0.4839(4) 0.137 Uiso 1 calc R .
C40 C -0.4415(8) 0.3910(3) 0.4491(3) 0.094(2) Uani 1 d . .
H40A H -0.4338(8) 0.4154(3) 0.4096(3) 0.112 Uiso 1 calc R .
C41 C -0.3550(7) 0.3402(3) 0.4636(3) 0.086(2) Uani 1 d . .
H41A H -0.2866(7) 0.3298(3) 0.4340(3) 0.103 Uiso 1 calc R .
C42 C -0.3663(6) 0.3029(2) 0.5219(3) 0.0706(14) Uani 1 d . .
H42A H -0.3053(6) 0.2680(2) 0.5311(3) 0.085 Uiso 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'
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'
Ni Ni 0.3393 1.1124 '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
N4 Ni1 N2 100.71(13) . . ?
N4 Ni1 S2 85.50(10) . . ?
N2 Ni1 S2 169.43(10) . . ?
N4 Ni1 S1 169.35(10) . . ?
N2 Ni1 S1 85.49(10) . . ?
S2 Ni1 S1 89.73(5) . . ?
C1 S1 Ni1 93.87(13) . . ?
C22 S2 Ni1 94.10(14) . . ?
C1 S3 C15 103.4(2) . . ?
C22 S4 C36 103.0(2) . . ?
C1 N1 N2 111.2(3) . . ?
C2 N2 N1 114.1(3) . . ?
C2 N2 Ni1 128.5(3) . . ?
N1 N2 Ni1 116.5(2) . . ?
C22 N3 N4 110.6(3) . . ?
C23 N4 N3 113.9(3) . . ?
C23 N4 Ni1 128.2(3) . . ?
N3 N4 Ni1 117.1(2) . . ?
N1 C1 S1 124.5(3) . . ?
N1 C1 S3 121.5(3) . . ?
S1 C1 S3 113.9(2) . . ?
N2 C2 C10 124.0(4) . . ?
N2 C2 C7 128.7(4) . . ?
C10 C2 C7 107.2(3) . . ?
C5 C3 C4 120.9(4) . . ?
C3 C4 C8 119.1(4) . . ?
C3 C5 C6 121.0(5) . . ?
C7 C6 C5 118.4(4) . . ?
C6 C7 C8 120.1(4) . . ?
C6 C7 C2 132.4(4) . . ?
C8 C7 C2 107.0(4) . . ?
C4 C8 C7 120.4(4) . . ?
C4 C8 C9 130.3(4) . . ?
C7 C8 C9 109.3(4) . . ?
C14 C9 C10 119.6(4) . . ?
C14 C9 C8 131.7(4) . . ?
C10 C9 C8 108.7(3) . . ?
C11 C10 C9 121.0(4) . . ?
C11 C10 C2 131.3(4) . . ?
C9 C10 C2 107.4(4) . . ?
C10 C11 C12 118.3(4) . . ?
C11 C12 C13 120.6(5) . . ?
C14 C13 C12 121.1(5) . . ?
C13 C14 C9 119.1(5) . . ?
C16 C15 S3 118.1(4) . . ?
C17 C16 C21 118.1(5) . . ?
C17 C16 C15 124.4(4) . . ?
C21 C16 C15 117.5(4) . . ?
C16 C17 C18 119.8(5) . . ?
C19 C18 C17 120.8(5) . . ?
C18 C19 C20 119.9(5) . . ?
C19 C20 C21 119.3(6) . . ?
C20 C21 C16 122.0(5) . . ?
N3 C22 S2 124.3(3) . . ?
N3 C22 S4 121.1(3) . . ?
S2 C22 S4 114.5(2) . . ?
N4 C23 C31 123.6(4) . . ?
N4 C23 C28 129.1(4) . . ?
C31 C23 C28 107.2(3) . . ?
C25 C24 C29 118.7(6) . . ?
C24 C25 C26 122.0(5) . . ?
C25 C26 C27 120.1(6) . . ?
C28 C27 C26 117.7(5) . . ?
C27 C28 C29 122.1(4) . . ?
C27 C28 C23 131.1(4) . . ?
C29 C28 C23 106.3(4) . . ?
C24 C29 C28 119.4(6) . . ?
C24 C29 C30 130.4(5) . . ?
C28 C29 C30 110.2(4) . . ?
C35 C30 C31 119.5(6) . . ?
C35 C30 C29 132.8(5) . . ?
C31 C30 C29 107.7(4) . . ?
C32 C31 C30 120.5(5) . . ?
C32 C31 C23 131.0(4) . . ?
C30 C31 C23 108.2(4) . . ?
C31 C32 C33 118.3(5) . . ?
C34 C33 C32 120.6(6) . . ?
C35 C34 C33 121.1(6) . . ?
C34 C35 C30 119.8(6) . . ?
C37 C36 S4 117.3(3) . . ?
C42 C37 C38 117.6(5) . . ?
C42 C37 C36 124.7(5) . . ?
C38 C37 C36 117.7(4) . . ?
C37 C38 C39 121.2(6) . . ?
C40 C39 C38 120.2(6) . . ?
C41 C40 C39 119.4(6) . . ?
C40 C41 C42 121.0(6) . . ?
C37 C42 C41 120.5(5) . . ?
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
Ni1 N4 1.936(3) . ?
Ni1 N2 1.939(3) . ?
Ni1 S2 2.1482(12) . ?
Ni1 S1 2.1512(12) . ?
S1 C1 1.733(4) . ?
S2 C22 1.738(4) . ?
S3 C1 1.745(4) . ?
S3 C15 1.801(5) . ?
S4 C22 1.742(4) . ?
S4 C36 1.808(5) . ?
N1 C1 1.290(5) . ?
N1 N2 1.402(4) . ?
N2 C2 1.317(5) . ?
N3 C22 1.299(5) . ?
N3 N4 1.401(4) . ?
N4 C23 1.314(4) . ?
C2 C10 1.472(5) . ?
C2 C7 1.478(5) . ?
C3 C5 1.370(7) . ?
C3 C4 1.374(7) . ?
C4 C8 1.380(6) . ?
C5 C6 1.397(6) . ?
C6 C7 1.378(6) . ?
C7 C8 1.406(5) . ?
C8 C9 1.457(6) . ?
C9 C14 1.381(6) . ?
C9 C10 1.413(5) . ?
C10 C11 1.378(6) . ?
C11 C12 1.391(6) . ?
C12 C13 1.387(7) . ?
C13 C14 1.377(7) . ?
C15 C16 1.505(6) . ?
C16 C17 1.362(6) . ?
C16 C21 1.381(6) . ?
C17 C18 1.401(7) . ?
C18 C19 1.354(8) . ?
C19 C20 1.361(8) . ?
C20 C21 1.373(7) . ?
C23 C31 1.474(6) . ?
C23 C28 1.475(5) . ?
C24 C25 1.369(9) . ?
C24 C29 1.392(7) . ?
C25 C26 1.392(9) . ?
C26 C27 1.402(6) . ?
C27 C28 1.378(6) . ?
C28 C29 1.407(6) . ?
C29 C30 1.460(7) . ?
C30 C35 1.381(8) . ?
C30 C31 1.403(6) . ?
C31 C32 1.374(6) . ?
C32 C33 1.395(7) . ?
C33 C34 1.371(9) . ?
C34 C35 1.355(9) . ?
C36 C37 1.502(6) . ?
C37 C42 1.367(6) . ?
C37 C38 1.373(7) . ?
C38 C39 1.383(8) . ?
C39 C40 1.351(9) . ?
C40 C41 1.345(8) . ?
C41 C42 1.387(7) . ?
