#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:29:24 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180476 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/45/7214596.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_7214596
loop_
_publ_author_name
'Singh, Santosh K.'
'Drew, Michael G. B.'
'Singh, Nanhai'
_publ_section_title
;
 Self assembly of homoleptic Ni(ii) dithiocarbamates and dithiocarbimates
 via Ni⋯H--C anagostic and C--H⋯π (chelate) interactions
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              10255
_journal_paper_doi               10.1039/c3ce41358f
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C30 H28 N2 Ni S4'
_chemical_formula_weight         603.49
_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                76.800(7)
_cell_angle_beta                 84.592(7)
_cell_angle_gamma                73.686(8)
_cell_formula_units_Z            1
_cell_length_a                   6.4700(6)
_cell_length_b                   10.5728(9)
_cell_length_c                   11.0821(9)
_cell_measurement_reflns_used    4943
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.05
_cell_volume                     707.97(11)
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.96
_diffrn_measured_fraction_theta_max 0.96
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0841
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4943
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.442
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             314
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details 
  w=1/[σ²(Fo²)+(0.0752P)²+0.0000P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                1735
_reflns_number_total             2904
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41358f.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7214596
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
C12 C 0.2301(6) 0.4123(4) -0.1113(4) 0.0416(10) Uani 1 1 d .
C41 C -0.0298(7) 0.2810(5) -0.0916(5) 0.0545(13) Uani 1 1 d .
H41A H -0.1820 0.3279 -0.0928 0.065 Uiso 1 1 calc R
H41B H 0.0138 0.2575 -0.0062 0.065 Uiso 1 1 calc R
C42 C 0.0013(7) 0.1545(5) -0.1371(4) 0.0461(11) Uani 1 1 d .
C43 C 0.2002(8) 0.0640(6) -0.1396(5) 0.0657(15) Uani 1 1 d .
H43 H 0.3204 0.0823 -0.1150 0.079 Uiso 1 1 calc R
C44 C 0.2220(12) -0.0562(7) -0.1794(6) 0.090(2) Uani 1 1 d .
H44 H 0.3562 -0.1182 -0.1801 0.108 Uiso 1 1 calc R
C45 C 0.0477(17) -0.0816(7) -0.2167(6) 0.099(2) Uani 1 1 d .
H45 H 0.0638 -0.1605 -0.2447 0.118 Uiso 1 1 calc R
C46 C -0.1492(14) 0.0055(8) -0.2141(6) 0.093(2) Uani 1 1 d .
H46 H -0.2682 -0.0134 -0.2395 0.112 Uiso 1 1 calc R
C47 C -0.1725(8) 0.1226(6) -0.1736(5) 0.0667(15) Uani 1 1 d .
H47 H -0.3089 0.1817 -0.1707 0.080 Uiso 1 1 calc R
C51 C 0.0311(7) 0.4352(6) -0.2948(5) 0.0607(14) Uani 1 1 d .
H51A H 0.0640 0.5217 -0.3179 0.073 Uiso 1 1 calc R
H51B H -0.1233 0.4515 -0.3003 0.073 Uiso 1 1 calc R
C52 C 0.1429(7) 0.3509(5) -0.3860(4) 0.0564(13) Uani 1 1 d .
C53 C 0.3557(9) 0.3408(8) -0.4227(6) 0.092(2) Uani 1 1 d .
H53 H 0.4311 0.3884 -0.3910 0.110 Uiso 1 1 calc R
C54 C 0.4598(11) 0.2613(9) -0.5059(7) 0.111(3) Uani 1 1 d .
H54 H 0.6032 0.2558 -0.5296 0.133 Uiso 1 1 calc R
C55 C 0.3494(14) 0.1916(8) -0.5523(7) 0.105(2) Uani 1 1 d .
H55 H 0.4187 0.1384 -0.6082 0.126 Uiso 1 1 calc R
C56 C 0.1430(14) 0.1982(8) -0.5189(6) 0.101(2) Uani 1 1 d .
H56 H 0.0707 0.1483 -0.5497 0.121 Uiso 1 1 calc R
C57 C 0.0368(10) 0.2807(7) -0.4376(5) 0.0794(18) Uani 1 1 d .
H57 H -0.1085 0.2885 -0.4178 0.095 Uiso 1 1 calc R
S11 S 0.36432(19) 0.53114(13) -0.18302(11) 0.0506(3) Uani 1 1 d .
S13 S 0.29941(18) 0.35689(13) 0.04164(11) 0.0502(4) Uani 1 1 d .
Ni1 Ni 0.5000 0.5000 0.0000 0.0423(3) Uani 1 2 d S
N14 N 0.0916(6) 0.3734(4) -0.1648(3) 0.0462(9) Uani 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'
O O 0.0106 0.0060 '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'
N N 0.0061 0.0033 '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
N14 C12 S13 125.5(3) . .
N14 C12 S11 125.2(3) . .
S13 C12 S11 109.3(2) . .
N14 C41 C42 114.1(4) . .
C43 C42 C47 118.0(5) . .
C43 C42 C41 121.6(4) . .
C47 C42 C41 120.4(4) . .
C42 C43 C44 119.9(6) . .
C45 C44 C43 119.9(6) . .
C46 C45 C44 121.1(7) . .
C45 C46 C47 119.4(6) . .
C46 C47 C42 121.7(6) . .
N14 C51 C52 114.0(4) . .
C57 C52 C53 117.1(5) . .
C57 C52 C51 121.4(5) . .
C53 C52 C51 121.6(5) . .
C52 C53 C54 121.5(6) . .
C55 C54 C53 119.3(7) . .
C56 C55 C54 121.1(7) . .
C55 C56 C57 119.5(7) . .
C52 C57 C56 121.4(6) . .
C12 S11 Ni1 85.60(15) . .
C12 S13 Ni1 85.85(15) . .
S13 Ni1 S13 180.00(4) . 2_665
S13 Ni1 S11 79.28(4) . .
S13 Ni1 S11 100.72(4) 2_665 .
S13 Ni1 S11 100.72(4) . 2_665
S13 Ni1 S11 79.28(4) 2_665 2_665
S11 Ni1 S11 180.0 . 2_665
C12 N14 C41 120.6(4) . .
C13 N14 C51 121.1(4) . .
C41 N14 C51 117.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C12 N14 1.320(5) .
C12 S13 1.720(4) .
C12 S11 1.730(4) .
C41 N14 1.476(6) .
C41 C42 1.491(6) .
C42 C43 1.373(6) .
C42 C47 1.379(6) .
C43 C44 1.405(9) .
C44 C45 1.350(9) .
C45 C46 1.348(10) .
C46 C47 1.376(8) .
C51 N4 1.480(6) .
C51 C52 1.500(7) .
C52 C57 1.379(8) .
C52 C53 1.380(7) .
C53 C54 1.389(9) .
C54 C55 1.363(10) .
C55 C56 1.338(9) .
C56 C57 1.397(10) .
S11 Ni1 2.2048(12) .
S13 Ni1 2.2041(12) .
Ni1 S13 2.2041(12) 2_665
Ni1 S11 2.2048(12) 2_665
