#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:53:03 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179819 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/15/7011585.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_7011585
loop_
_publ_author_name
'Xie, Jingli'
'Ren, Xiaoming'
'Song, You'
'Zou, Yang'
'Meng, Qingjin'
_publ_section_title
;
 Synthesis, crystal structure and magnetic properties of a novel
 one-dimensional nickel(iii) chain complex showing ferromagnetic
 ordering at low temperature
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2868
_journal_paper_doi               10.1039/b201936c
_journal_year                    2002
_chemical_formula_sum            'C20 H10 Br F N5 Ni S4'
_chemical_formula_weight         606.19
_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                 101.63(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.989(2)
_cell_length_b                   26.363(5)
_cell_length_c                   7.4860(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.50
_cell_measurement_theta_min      3.56
_cell_volume                     2317.5(8)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius 1990)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius 1990)'
_computing_data_reduction        'CAD-4 Software (Enraf-Nonius 1990)'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CAD 4'
_diffrn_measurement_method       '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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4353
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        3.60
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.949
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(North, et.al, 1984)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.035
_refine_diff_density_min         -1.200
_refine_diff_density_rms         0.260
_refine_ls_extinction_coef       0.0080(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1506
_refine_ls_R_factor_gt           0.0793
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+22.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2233
_refine_ls_wR_factor_ref         0.3529
_reflns_number_gt                2493
_reflns_number_total             4022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b201936c.txt
_cod_data_source_block           t
_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 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7011585
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
Ni1 Ni 0.25984(14) 0.72565(6) 1.0428(2) 0.0446(6) Uani 1 1 d . . .
S1 S 0.1539(3) 0.66183(13) 0.9432(5) 0.0527(9) Uani 1 1 d . . .
S2 S 0.4014(3) 0.67808(13) 1.1556(5) 0.0542(9) Uani 1 1 d . . .
S3 S 0.3762(3) 0.78676(13) 1.1283(5) 0.0519(9) Uani 1 1 d . . .
S4 S 0.1234(3) 0.77624(13) 0.9340(5) 0.0516(9) Uani 1 1 d . . .
N1 N 0.1690(14) 0.5226(5) 0.881(2) 0.084(4) Uani 1 1 d . . .
N2 N 0.5070(14) 0.5479(6) 1.167(2) 0.091(5) Uani 1 1 d . . .
N3 N 0.3975(13) 0.9256(5) 1.111(2) 0.082(4) Uani 1 1 d . . .
N4 N 0.0634(11) 0.9114(6) 0.865(2) 0.082(4) Uani 1 1 d . . .
C1 C 0.2057(14) 0.5604(6) 0.938(2) 0.064(4) Uani 1 1 d . . .
C2 C 0.2436(12) 0.6116(5) 0.9952(17) 0.052(3) Uani 1 1 d . . .
C3 C 0.3561(12) 0.6188(5) 1.0888(18) 0.053(3) Uani 1 1 d . . .
C4 C 0.4371(13) 0.5781(5) 1.1313(19) 0.057(4) Uani 1 1 d . . .
C5 C 0.3533(12) 0.8883(5) 1.0908(19) 0.051(3) Uani 1 1 d . . .
C6 C 0.2959(9) 0.8388(5) 1.0547(16) 0.040(3) Uani 1 1 d . . .
C7 C 0.1845(12) 0.8341(4) 0.9717(18) 0.048(3) Uani 1 1 d . . .
C8 C 0.1151(12) 0.8793(5) 0.910(2) 0.054(3) Uani 1 1 d . . .
Br1 Br 0.7231(2) 0.83193(6) 1.0010(2) 0.0823(7) Uani 1 1 d . . .
F1 F 0.5781(7) 0.6481(3) 0.9037(13) 0.071(2) Uani 1 1 d . . .
N5 N 0.7783(10) 0.5727(4) 0.8830(15) 0.051(3) Uani 1 1 d . . .
C9 C 0.6845(16) 0.5540(5) 0.784(2) 0.068(4) Uani 1 1 d . . .
H9A H 0.6176 0.5567 0.8279 0.081 Uiso 1 1 calc R . .
C10 C 0.6796(16) 0.5310(6) 0.619(2) 0.078(5) Uani 1 1 d . . .
H10A H 0.6117 0.5187 0.5502 0.093 Uiso 1 1 calc R . .
C11 C 0.784(2) 0.5270(6) 0.560(3) 0.088(6) Uani 1 1 d . . .
H11A H 0.7859 0.5108 0.4505 0.106 Uiso 1 1 calc R . .
C12 C 0.8795(17) 0.5461(6) 0.661(3) 0.077(5) Uani 1 1 d . . .
H12A H 0.9484 0.5431 0.6227 0.092 Uiso 1 1 calc R . .
C13 C 0.8739(13) 0.5699(6) 0.818(3) 0.075(5) Uani 1 1 d . . .
H13A H 0.9395 0.5850 0.8841 0.090 Uiso 1 1 calc R . .
C14 C 0.7803(12) 0.5991(5) 1.057(2) 0.057(3) Uani 1 1 d . . .
H14A H 0.8509 0.5914 1.1414 0.068 Uiso 1 1 calc R . .
H14B H 0.7179 0.5870 1.1104 0.068 Uiso 1 1 calc R . .
C15 C 0.7700(12) 0.6563(5) 1.0312(17) 0.051(3) Uani 1 1 d . . .
C16 C 0.6686(13) 0.6779(5) 0.9655(19) 0.054(3) Uani 1 1 d . . .
C17 C 0.6516(13) 0.7304(5) 0.9534(19) 0.058(4) Uani 1 1 d . . .
H17A H 0.5800 0.7439 0.9071 0.069 Uiso 1 1 calc R . .
C18 C 0.7415(11) 0.7607(6) 1.0104(18) 0.055(3) Uani 1 1 d . . .
C19 C 0.8511(14) 0.7397(6) 1.078(2) 0.066(4) Uani 1 1 d . . .
H19A H 0.9144 0.7606 1.1116 0.079 Uiso 1 1 calc R . .
C20 C 0.8609(14) 0.6879(6) 1.091(2) 0.068(4) Uani 1 1 d . . .
H20A H 0.9311 0.6738 1.1425 0.081 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'
N N 0.0061 0.0033 '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'
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'
Br Br -0.2901 2.4595 '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
S4 Ni1 S2 177.28(15) . . ?
S4 Ni1 S3 92.67(14) . . ?
S2 Ni1 S3 84.62(14) . . ?
S4 Ni1 S1 90.16(14) . . ?
S2 Ni1 S1 92.55(15) . . ?
S3 Ni1 S1 174.88(16) . . ?
C2 S1 Ni1 103.2(5) . . ?
C3 S2 Ni1 104.0(5) . . ?
C6 S3 Ni1 102.6(4) . . ?
C7 S4 Ni1 103.1(5) . . ?
N1 C1 C2 173.7(18) . . ?
C3 C2 C1 118.9(13) . . ?
C3 C2 S1 120.5(10) . . ?
C1 C2 S1 120.5(11) . . ?
C2 C3 C4 123.1(13) . . ?
C2 C3 S2 119.4(10) . . ?
C4 C3 S2 117.4(11) . . ?
N2 C4 C3 175.6(17) . . ?
N3 C5 C6 177.2(16) . . ?
C7 C6 C5 122.9(11) . . ?
C7 C6 S3 120.9(9) . . ?
C5 C6 S3 116.2(9) . . ?
C6 C7 C8 120.6(11) . . ?
C6 C7 S4 120.8(9) . . ?
C8 C7 S4 118.6(11) . . ?
N4 C8 C7 178.7(17) . . ?
C9 N5 C13 118.3(14) . . ?
C9 N5 C14 122.5(13) . . ?
C13 N5 C14 119.1(12) . . ?
N5 C9 C10 123.7(17) . . ?
C9 C10 C11 115.9(16) . . ?
C12 C11 C10 120.6(18) . . ?
C11 C12 C13 118.6(18) . . ?
N5 C13 C12 122.8(16) . . ?
N5 C14 C15 111.7(11) . . ?
C16 C15 C20 117.7(14) . . ?
C16 C15 C14 120.7(13) . . ?
C20 C15 C14 121.3(13) . . ?
C15 C16 F1 119.3(13) . . ?
C15 C16 C17 123.4(14) . . ?
F1 C16 C17 117.2(13) . . ?
C18 C17 C16 118.1(14) . . ?
C17 C18 C19 120.6(16) . . ?
C17 C18 Br1 119.9(11) . . ?
C19 C18 Br1 119.5(12) . . ?
C20 C19 C18 118.2(15) . . ?
C15 C20 C19 121.9(15) . . ?
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 S4 2.140(4) . ?
Ni1 S2 2.142(4) . ?
Ni1 S3 2.143(4) . ?
Ni1 S1 2.149(4) . ?
S1 C2 1.702(14) . ?
S2 C3 1.696(14) . ?
S3 C6 1.702(12) . ?
S4 C7 1.690(13) . ?
N1 C1 1.137(19) . ?
N2 C4 1.146(19) . ?
N3 C5 1.112(18) . ?
N4 C8 1.063(18) . ?
C1 C2 1.46(2) . ?
C2 C3 1.40(2) . ?
C3 C4 1.440(19) . ?
C5 C6 1.476(18) . ?
C6 C7 1.360(18) . ?
C7 C8 1.475(17) . ?
Br1 C18 1.891(16) . ?
F1 C16 1.342(16) . ?
N5 C9 1.312(19) . ?
N5 C13 1.334(19) . ?
N5 C14 1.475(18) . ?
C9 C10 1.36(2) . ?
C10 C11 1.41(3) . ?
C11 C12 1.34(3) . ?
C12 C13 1.35(2) . ?
C14 C15 1.52(2) . ?
C15 C16 1.34(2) . ?
C15 C20 1.37(2) . ?
C16 C17 1.402(19) . ?
C17 C18 1.34(2) . ?
C18 C19 1.42(2) . ?
C19 C20 1.37(2) . ?
