#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/12/7201260.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_7201260
loop_
_publ_author_name
'Dalgleish, Simon'
'Morrison, Carole A.'
'Middlemiss, Derek S.'
'Mount, Andrew R.'
'Collins, Anna'
'Pilia, Luca'
'Serpe, Angela'
'Mercuri, M. Laura'
'Roberts-Bleming, Susan J.'
'Charlton, Adam'
'Deplano, Paola'
'Murphy, Patrick J.'
'Robertson, Neil'
_publ_section_related_literature
;
?
;
_publ_section_title
;
 Synthesis, structure and spectroscopic properties of a new class of
 polymerisable nickel dithiolenes
;
_journal_issue                   34
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              6194
_journal_paper_doi               10.1039/b907028a
_journal_volume                  19
_journal_year                    2009
_chemical_compound_source        'Simon Dalgleish, SD068'
_chemical_formula_moiety         'C20 H24 N2 Ni1 S6'
_chemical_formula_sum            'C20 H24 N2 Ni S6'
_chemical_formula_weight         543.53
_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
_audit_creation_date             08-05-26
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 114.935(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4169(2)
_cell_length_b                   27.4559(7)
_cell_length_c                   10.0584(2)
_cell_measurement_reflns_used    7654
_cell_measurement_temperature    150
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     2358.18(9)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16512
_diffrn_reflns_theta_full        27.836
_diffrn_reflns_theta_max         29.613
_diffrn_reflns_theta_min         1.483
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_recrystallization_method
;
Slow diffusion of Et₂O into DMF.
;
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.77
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         6023
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.001471
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[σ²(F²) + ( 0.03P)² + 0.07P]
,where P=(max(Fo²,0) + 2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1109
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1109
_reflns_limit_h_max              11
_reflns_limit_h_min              -13
_reflns_limit_k_max              37
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                5060
_reflns_number_total             6040
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0551
_oxford_refine_ls_scale          0.26519(19)
_oxford_reflns_number_all        6023
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'nr8009 in P2(1)/n'
_cod_data_source_file            b907028a.txt
_cod_data_source_block           NR8009
_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      'P 1 21/n 1 '
_cod_original_formula_sum        'C20 H24 N2 Ni1 S6'
_cod_database_code               7201260
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Ni1 Ni 0.69746(4) 0.571233(12) 0.50703(4) 0.0184 1.0000 Uani . . . . . . .
S2 S 0.66078(9) 0.63688(2) 0.38208(7) 0.0191 1.0000 Uani . . . . . . .
C3 C 0.5930(3) 0.67919(9) 0.4726(3) 0.0171 1.0000 Uani . . . . . . .
C4 C 0.5556(3) 0.72795(9) 0.4052(3) 0.0169 1.0000 Uani . . . . . . .
C5 C 0.5906(4) 0.77119(10) 0.4817(3) 0.0208 1.0000 Uani . . . . . . .
S6 S 0.52219(10) 0.82006(3) 0.36894(8) 0.0253 1.0000 Uani . . . . . . .
C7 C 0.4512(3) 0.78548(10) 0.2145(3) 0.0187 1.0000 Uani . . . . . . .
C8 C 0.4773(3) 0.73621(10) 0.2505(3) 0.0204 1.0000 Uani . . . . . . .
S9 S 0.63956(9) 0.60677(2) 0.66633(7) 0.0211 1.0000 Uani . . . . . . .
C10 C 0.5831(3) 0.66564(9) 0.5974(3) 0.0178 1.0000 Uani . . . . . . .
C11 C 0.5188(3) 0.69642(10) 0.6799(3) 0.0189 1.0000 Uani . . . . . . .
C12 C 0.5809(4) 0.69986(11) 0.8289(3) 0.0248 1.0000 Uani . . . . . . .
S13 S 0.46863(11) 0.73510(3) 0.88786(9) 0.0330 1.0000 Uani . . . . . . .
C14 C 0.3349(4) 0.74594(11) 0.7128(3) 0.0247 1.0000 Uani . . . . . . .
C15 C 0.3752(3) 0.72337(10) 0.6137(3) 0.0215 1.0000 Uani . . . . . . .
S16 S 0.74550(10) 0.50485(3) 0.63574(8) 0.0241 1.0000 Uani . . . . . . .
C17 C 0.7934(3) 0.46289(10) 0.5381(3) 0.0192 1.0000 Uani . . . . . . .
N18 N 0.8586(3) 0.42033(8) 0.5919(3) 0.0203 1.0000 Uani . . . . . . .
C19 C 0.8942(4) 0.38646(10) 0.4970(3) 0.0229 1.0000 Uani . . . . . . .
C20 C 0.8977(4) 0.40605(10) 0.7459(3) 0.0223 1.0000 Uani . . . . . . .
C21 C 1.0553(4) 0.38062(14) 0.8177(4) 0.0385 1.0000 Uani . . . . . . .
C22 C 0.7642(4) 0.37617(13) 0.7489(4) 0.0356 1.0000 Uani . . . . . . .
S23 S 0.73362(10) 0.53424(2) 0.33424(8) 0.0245 1.0000 Uani . . . . . . .
C24 C 0.7590(3) 0.47492(9) 0.3842(3) 0.0178 1.0000 Uani . . . . . . .
N25 N 0.7452(3) 0.43941(8) 0.2905(3) 0.0200 1.0000 Uani . . . . . . .
C26 C 0.7698(4) 0.38886(10) 0.3425(3) 0.0234 1.0000 Uani . . . . . . .
C27 C 0.6886(4) 0.44918(10) 0.1307(3) 0.0254 1.0000 Uani . . . . . . .
C28 C 0.8275(5) 0.45770(13) 0.0938(4) 0.0376 1.0000 Uani . . . . . . .
C29 C 0.5810(4) 0.40871(13) 0.0393(3) 0.0365 1.0000 Uani . . . . . . .
H51 H 0.6447 0.7738 0.5823 0.0257 1.0000 Uiso R . . . . . .
H81 H 0.4476 0.7116 0.1818 0.0240 1.0000 Uiso R . . . . . .
H121 H 0.6722 0.6851 0.8925 0.0302 1.0000 Uiso R . . . . . .
H141 H 0.2474 0.7642 0.6892 0.0302 1.0000 Uiso R . . . . . .
H151 H 0.3167 0.7252 0.5138 0.0257 1.0000 Uiso R . . . . . .
H191 H 0.9952 0.3945 0.4984 0.0289 1.0000 Uiso R . . . . . .
H192 H 0.8970 0.3538 0.5332 0.0287 1.0000 Uiso R . . . . . .
H201 H 0.9051 0.4357 0.7985 0.0269 1.0000 Uiso R . . . . . .
H211 H 1.0823 0.3782 0.9209 0.0583 1.0000 Uiso R . . . . . .
H213 H 1.1326 0.3995 0.8022 0.0594 1.0000 Uiso R . . . . . .
H212 H 1.0475 0.3489 0.7741 0.0595 1.0000 Uiso R . . . . . .
H221 H 0.7820 0.3700 0.8481 0.0536 1.0000 Uiso R . . . . . .
H223 H 0.6670 0.3926 0.7002 0.0539 1.0000 Uiso R . . . . . .
H222 H 0.7604 0.3460 0.7003 0.0535 1.0000 Uiso R . . . . . .
H261 H 0.8034 0.3700 0.2802 0.0284 1.0000 Uiso R . . . . . .
H262 H 0.6738 0.3761 0.3376 0.0275 1.0000 Uiso R . . . . . .
H271 H 0.6268 0.4789 0.1108 0.0305 1.0000 Uiso R . . . . . .
H281 H 0.7905 0.4655 -0.0072 0.0594 1.0000 Uiso R . . . . . .
H283 H 0.8920 0.4838 0.1516 0.0597 1.0000 Uiso R . . . . . .
H282 H 0.8894 0.4283 0.1136 0.0594 1.0000 Uiso R . . . . . .
H291 H 0.5342 0.4181 -0.0615 0.0513 1.0000 Uiso R . . . . . .
H293 H 0.4981 0.4025 0.0690 0.0519 1.0000 Uiso R . . . . . .
H292 H 0.6425 0.3796 0.0503 0.0514 1.0000 Uiso R . . . . . .
H71 H 0.4047 0.7972 0.1268 0.0223 1.0000 Uiso R . . . . . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S2 . Ni1 . S9 . 91.54(3) yes
S2 . Ni1 . S16 . 177.48(4) yes
S9 . Ni1 . S16 . 89.49(3) yes
S2 . Ni1 . S23 . 87.97(3) yes
S9 . Ni1 . S23 . 174.81(4) yes
S16 . Ni1 . S23 . 91.21(3) yes
Ni1 . S2 . C3 . 104.88(9) yes
S2 . C3 . C4 . 115.53(19) yes
S2 . C3 . C10 . 118.9(2) yes
C4 . C3 . C10 . 125.5(2) yes
C3 . C4 . C5 . 124.8(2) yes
C3 . C4 . C8 . 123.9(2) yes
C5 . C4 . C8 . 111.3(2) yes
C4 . C5 . S6 . 111.9(2) yes
C4 . C5 . H51 . 124.8 no
S6 . C5 . H51 . 123.3 no
C5 . S6 . C7 . 93.52(13) yes
S6 . C7 . C8 . 110.2(2) yes
S6 . C7 . H71 . 124.0 no
C8 . C7 . H71 . 125.7 no
C4 . C8 . C7 . 112.9(2) yes
C4 . C8 . H81 . 123.6 no
C7 . C8 . H81 . 123.4 no
Ni1 . S9 . C10 . 104.83(9) yes
S9 . C10 . C3 . 119.6(2) yes
S9 . C10 . C11 . 115.63(19) yes
C3 . C10 . C11 . 124.7(2) yes
C10 . C11 . C12 . 124.6(3) yes
C10 . C11 . C15 . 124.2(2) yes
C12 . C11 . C15 . 111.0(2) yes
C11 . C12 . S13 . 112.2(2) yes
C11 . C12 . H121 . 125.1 no
S13 . C12 . H121 . 122.7 no
C12 . S13 . C14 . 92.07(14) yes
S13 . C14 . C15 . 111.4(2) yes
S13 . C14 . H141 . 124.2 no
C15 . C14 . H141 . 124.4 no
C11 . C15 . C14 . 113.3(3) yes
C11 . C15 . H151 . 123.2 no
C14 . C15 . H151 . 123.5 no
Ni1 . S16 . C17 . 105.37(10) yes
S16 . C17 . N18 . 123.7(2) yes
S16 . C17 . C24 . 117.4(2) yes
N18 . C17 . C24 . 118.9(2) yes
C17 . N18 . C19 . 119.1(2) yes
C17 . N18 . C20 . 121.8(2) yes
C19 . N18 . C20 . 119.1(2) yes
N18 . C19 . C26 . 110.6(2) yes
N18 . C19 . H191 . 109.7 no
C26 . C19 . H191 . 109.7 no
N18 . C19 . H192 . 108.7 no
C26 . C19 . H192 . 108.5 no
H191 . C19 . H192 . 109.7 no
N18 . C20 . C21 . 112.3(2) yes
N18 . C20 . C22 . 108.7(2) yes
C21 . C20 . C22 . 113.3(3) yes
N18 . C20 . H201 . 106.2 no
C21 . C20 . H201 . 107.4 no
C22 . C20 . H201 . 108.5 no
C20 . C21 . H211 . 107.8 no
C20 . C21 . H213 . 109.4 no
H211 . C21 . H213 . 109.9 no
C20 . C21 . H212 . 109.1 no
H211 . C21 . H212 . 111.3 no
H213 . C21 . H212 . 109.3 no
C20 . C22 . H221 . 109.6 no
C20 . C22 . H223 . 111.2 no
H221 . C22 . H223 . 109.3 no
C20 . C22 . H222 . 108.2 no
H221 . C22 . H222 . 109.5 no
H223 . C22 . H222 . 109.0 no
Ni1 . S23 . C24 . 105.31(10) yes
C17 . C24 . S23 . 117.87(19) yes
C17 . C24 . N25 . 119.5(2) yes
S23 . C24 . N25 . 122.6(2) yes
C24 . N25 . C26 . 119.3(2) yes
C24 . N25 . C27 . 121.2(2) yes
C26 . N25 . C27 . 119.1(2) yes
C19 . C26 . N25 . 110.3(2) yes
C19 . C26 . H261 . 108.8 no
N25 . C26 . H261 . 108.9 no
C19 . C26 . H262 . 110.3 no
N25 . C26 . H262 . 109.0 no
H261 . C26 . H262 . 109.5 no
N25 . C27 . C28 . 109.8(3) yes
N25 . C27 . C29 . 111.4(2) yes
C28 . C27 . C29 . 112.7(3) yes
N25 . C27 . H271 . 106.5 no
C28 . C27 . H271 . 108.8 no
C29 . C27 . H271 . 107.4 no
C27 . C28 . H281 . 109.3 no
C27 . C28 . H283 . 110.8 no
H281 . C28 . H283 . 109.4 no
C27 . C28 . H282 . 109.1 no
H281 . C28 . H282 . 109.1 no
H283 . C28 . H282 . 109.1 no
C27 . C29 . H291 . 109.6 no
C27 . C29 . H293 . 111.3 no
H291 . C29 . H293 . 107.9 no
C27 . C29 . H292 . 108.6 no
H291 . C29 . H292 . 109.4 no
H293 . C29 . H292 . 110.1 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . S2 . 2.1404(7) yes
Ni1 . S9 . 2.1338(7) yes
Ni1 . S16 . 2.1700(8) yes
Ni1 . S23 . 2.1604(8) yes
S2 . C3 . 1.754(3) yes
C3 . C4 . 1.475(4) yes
C3 . C10 . 1.350(4) yes
C4 . C5 . 1.377(4) yes
C4 . C8 . 1.431(4) yes
C5 . S6 . 1.699(3) yes
C5 . H51 . 0.924 no
S6 . C7 . 1.699(3) yes
C7 . C8 . 1.395(4) yes
C7 . H71 . 0.864 no
C8 . H81 . 0.922 no
S9 . C10 . 1.751(3) yes
C10 . C11 . 1.481(4) yes
C11 . C12 . 1.363(4) yes
C11 . C15 . 1.435(4) yes
C12 . S13 . 1.713(3) yes
C12 . H121 . 0.922 no
S13 . C14 . 1.704(3) yes
C14 . C15 . 1.357(4) yes
C14 . H141 . 0.907 no
C15 . H151 . 0.922 no
S16 . C17 . 1.694(3) yes
C17 . N18 . 1.324(3) yes
C17 . C24 . 1.479(4) yes
N18 . C19 . 1.469(3) yes
N18 . C20 . 1.486(3) yes
C19 . C26 . 1.502(4) yes
C19 . H191 . 0.971 no
C19 . H192 . 0.964 no
C20 . C21 . 1.519(4) yes
C20 . C22 . 1.512(4) yes
C20 . H201 . 0.957 no
C21 . H211 . 0.961 no
C21 . H213 . 0.958 no
C21 . H212 . 0.963 no
C22 . H221 . 0.954 no
C22 . H223 . 0.950 no
C22 . H222 . 0.954 no
S23 . C24 . 1.691(3) yes
C24 . N25 . 1.324(3) yes
N25 . C26 . 1.466(3) yes
N25 . C27 . 1.489(4) yes
C26 . H261 . 0.964 no
C26 . H262 . 0.951 no
C27 . C28 . 1.521(5) yes
C27 . C29 . 1.524(4) yes
C27 . H271 . 0.974 no
C28 . H281 . 0.949 no
C28 . H283 . 0.961 no
C28 . H282 . 0.966 no
C29 . H291 . 0.955 no
C29 . H293 . 0.961 no
C29 . H292 . 0.965 no
