#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:18:11 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179684 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/06/7000665.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_7000665
loop_
_publ_author_name
'Ding, Nini'
'Zhang, Jun'
'Hor, T. S. Andy'
_publ_section_title
;
 Formation and crystallographic elucidation of stable [4 +
 2]-coordinate nickel(ii) N,S-heterocyclic carbene (NSHC) complexes
;
_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              1853
_journal_page_last               1858
_journal_paper_doi               10.1039/b815876b
_journal_year                    2009
_chemical_formula_sum            'C42 H38 Br2 N2 Ni S2'
_chemical_formula_weight         853.39
_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                98.2140(10)
_cell_angle_beta                 104.9500(10)
_cell_angle_gamma                102.2930(10)
_cell_formula_units_Z            1
_cell_length_a                   8.3327(5)
_cell_length_b                   8.7543(5)
_cell_length_c                   14.4928(9)
_cell_measurement_reflns_used    4425
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.90
_cell_measurement_theta_min      2.44
_cell_volume                     975.85(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12903
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    2.683
_exptl_absorpt_correction_T_max  0.5000
_exptl_absorpt_correction_T_min  0.2959
_exptl_absorpt_correction_type   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             434
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4481
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0366
_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)+(0.0590P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                3640
_reflns_number_total             4481
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815876b.txt
_cod_data_source_block           Compound6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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
_cod_database_code               7000665
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.0000 0.0000 0.03325(12) Uani 1 2 d S . .
Br1 Br 0.61703(3) -0.08693(3) -0.119753(18) 0.04746(11) Uani 1 1 d . . .
S1 S 0.59854(7) 0.35541(7) -0.02023(5) 0.04094(15) Uani 1 1 d . . .
N1 N 0.8171(2) 0.2574(2) 0.09218(13) 0.0350(4) Uani 1 1 d . . .
C1 C 0.6582(3) 0.2038(3) 0.03125(16) 0.0342(5) Uani 1 1 d . . .
C2 C 0.8974(3) 0.4209(3) 0.10330(17) 0.0368(5) Uani 1 1 d . . .
C3 C 1.0606(3) 0.5064(3) 0.16319(19) 0.0474(6) Uani 1 1 d . . .
H3 H 1.1313 0.4579 0.2032 0.057 Uiso 1 1 calc R . .
C4 C 1.1134(3) 0.6657(3) 0.1610(2) 0.0542(7) Uani 1 1 d . . .
H4 H 1.2222 0.7253 0.2003 0.065 Uiso 1 1 calc R . .
C5 C 1.0089(3) 0.7399(3) 0.1019(2) 0.0510(7) Uani 1 1 d . . .
H5 H 1.0487 0.8476 0.1021 0.061 Uiso 1 1 calc R . .
C6 C 0.8471(3) 0.6556(3) 0.0431(2) 0.0451(6) Uani 1 1 d . . .
H6 H 0.7763 0.7046 0.0035 0.054 Uiso 1 1 calc R . .
C7 C 0.7928(3) 0.4945(3) 0.04497(17) 0.0375(5) Uani 1 1 d . . .
C8 C 0.9078(3) 0.1515(3) 0.14131(19) 0.0450(6) Uani 1 1 d . . .
H8A H 1.0142 0.1580 0.1246 0.054 Uiso 1 1 calc R . .
H8B H 0.8376 0.0422 0.1168 0.054 Uiso 1 1 calc R . .
C9 C 0.9494(3) 0.1901(3) 0.2515(2) 0.0490(6) Uani 1 1 d . . .
C10 C 1.0892(5) 0.1480(5) 0.3071(3) 0.0800(10) Uani 1 1 d . . .
H10 H 1.1577 0.1008 0.2769 0.096 Uiso 1 1 calc R . .
C11 C 1.1260(7) 0.1768(6) 0.4078(3) 0.1118(16) Uani 1 1 d . . .
H11 H 1.2187 0.1473 0.4452 0.134 Uiso 1 1 calc R . .
C12 C 1.0280(7) 0.2477(6) 0.4525(3) 0.1000(14) Uani 1 1 d . . .
H12 H 1.0540 0.2666 0.5202 0.120 Uiso 1 1 calc R . .
C13 C 0.8902(5) 0.2918(5) 0.3981(3) 0.0832(11) Uani 1 1 d . . .
H13 H 0.8242 0.3420 0.4287 0.100 Uiso 1 1 calc R . .
C14 C 0.8511(4) 0.2606(4) 0.2976(2) 0.0638(8) Uani 1 1 d . . .
H14 H 0.7565 0.2879 0.2605 0.077 Uiso 1 1 calc R . .
C1S C 0.5933(9) 0.6961(10) 0.3192(5) 0.131(7) Uani 0.482(8) 1 d PGU A 1
C2S C 0.5906(9) 0.8558(9) 0.3310(5) 0.077(3) Uani 0.482(8) 1 d PGU A 1
H2S H 0.6614 0.9265 0.3069 0.092 Uiso 0.482(8) 1 calc PR A 1
C3S C 0.4822(11) 0.9099(8) 0.3788(5) 0.111(4) Uani 0.482(8) 1 d PGU A 1
H3S H 0.4804 1.0168 0.3867 0.133 Uiso 0.482(8) 1 calc PR A 1
C4S C 0.3764(11) 0.8043(12) 0.4148(6) 0.105(4) Uani 0.482(8) 1 d PGU A 1
H4S H 0.3038 0.8405 0.4468 0.126 Uiso 0.482(8) 1 calc PR A 1
C5S C 0.3791(10) 0.6445(11) 0.4030(6) 0.107(4) Uani 0.482(8) 1 d PGU A 1
H5S H 0.3084 0.5739 0.4271 0.128 Uiso 0.482(8) 1 calc PR A 1
C6S C 0.4876(10) 0.5904(8) 0.3552(5) 0.084(3) Uani 0.482(8) 1 d PGU A 1
H6S H 0.4894 0.4836 0.3473 0.100 Uiso 0.482(8) 1 calc PR A 1
C7S C 0.6956(14) 0.6380(17) 0.2658(7) 0.112(4) Uani 0.482(8) 1 d PU A 1
H7S1 H 0.7540 0.7233 0.2418 0.169 Uiso 0.482(8) 1 calc PR A 1
H7S2 H 0.6235 0.5537 0.2117 0.169 Uiso 0.482(8) 1 calc PR A 1
H7S3 H 0.7788 0.5975 0.3075 0.169 Uiso 0.482(8) 1 calc PR A 1
C8S C 0.6037(9) 0.7251(8) 0.3120(5) 0.102(5) Uani 0.518(8) 1 d PGDU A 2
C9S C 0.5249(11) 0.8107(8) 0.3668(5) 0.087(3) Uani 0.518(8) 1 d PGU A 2
H9S H 0.5479 0.9212 0.3742 0.105 Uiso 0.518(8) 1 calc PR A 2
C10S C 0.4118(11) 0.7312(14) 0.4106(6) 0.147(7) Uani 0.518(8) 1 d PGU A 2
H10S H 0.3592 0.7885 0.4473 0.176 Uiso 0.518(8) 1 calc PR A 2
C11S C 0.3775(11) 0.5660(14) 0.3996(7) 0.166(7) Uani 0.518(8) 1 d PGU A 2
H11S H 0.3018 0.5128 0.4289 0.199 Uiso 0.518(8) 1 calc PR A 2
C12S C 0.4562(11) 0.4804(8) 0.3448(7) 0.153(6) Uani 0.518(8) 1 d PGU A 2
H12S H 0.4332 0.3699 0.3374 0.184 Uiso 0.518(8) 1 calc PR A 2
C13S C 0.5693(10) 0.5600(8) 0.3010(5) 0.087(3) Uani 0.518(8) 1 d PGU A 2
H13S H 0.6220 0.5027 0.2643 0.105 Uiso 0.518(8) 1 calc PR A 2
C14S C 0.7256(11) 0.8159(14) 0.2740(7) 0.116(4) Uani 0.518(8) 1 d PDU A 2
H14A H 0.6667 0.8369 0.2128 0.173 Uiso 0.518(8) 1 calc PR A 2
H14B H 0.8066 0.7567 0.2643 0.173 Uiso 0.518(8) 1 calc PR A 2
H14C H 0.7855 0.9154 0.3195 0.173 Uiso 0.518(8) 1 calc PR A 2
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'
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
C1 Ni1 C1 180.0 2_655 . ?
C1 Ni1 Br1 90.62(7) 2_655 2_655 ?
C1 Ni1 Br1 89.38(7) . 2_655 ?
C1 Ni1 Br1 89.38(7) 2_655 . ?
C1 Ni1 Br1 90.62(7) . . ?
Br1 Ni1 Br1 180.0 2_655 . ?
C1 S1 C7 93.10(11) . . ?
C1 N1 C2 116.25(19) . . ?
C1 N1 C8 122.07(18) . . ?
C2 N1 C8 121.60(19) . . ?
N1 C1 S1 109.70(15) . . ?
N1 C1 Ni1 130.58(17) . . ?
S1 C1 Ni1 119.69(12) . . ?
C7 C2 C3 120.8(2) . . ?
C7 C2 N1 111.62(18) . . ?
C3 C2 N1 127.6(2) . . ?
C4 C3 C2 117.5(3) . . ?
C3 C4 C5 121.9(2) . . ?
C6 C5 C4 120.7(2) . . ?
C5 C6 C7 117.8(2) . . ?
C2 C7 C6 121.4(2) . . ?
C2 C7 S1 109.30(16) . . ?
C6 C7 S1 129.2(2) . . ?
N1 C8 C9 114.0(2) . . ?
C14 C9 C10 119.2(3) . . ?
C14 C9 C8 122.3(3) . . ?
C10 C9 C8 118.4(3) . . ?
C11 C10 C9 119.5(4) . . ?
C12 C11 C10 120.6(4) . . ?
C11 C12 C13 120.3(4) . . ?
C12 C13 C14 119.2(4) . . ?
C9 C14 C13 121.1(3) . . ?
C2S C1S C6S 120.0 . . ?
C2S C1S C7S 120.4(8) . . ?
C6S C1S C7S 119.5(8) . . ?
C3S C2S C1S 120.0 . . ?
C2S C3S C4S 120.0 . . ?
C5S C4S C3S 120.0 . . ?
C4S C5S C6S 120.0 . . ?
C5S C6S C1S 120.0 . . ?
C9S C8S C13S 120.0 . . ?
C9S C8S C14S 116.7(8) . . ?
C13S C8S C14S 123.2(8) . . ?
C10S C9S C8S 120.0 . . ?
C9S C10S C11S 120.0 . . ?
C12S C11S C10S 120.0 . . ?
C11S C12S C13S 120.0 . . ?
C12S C13S C8S 120.0 . . ?
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 C1 1.893(2) 2_655 ?
Ni1 C1 1.893(2) . ?
Ni1 Br1 2.3138(3) 2_655 ?
Ni1 Br1 2.3139(3) . ?
S1 C1 1.714(2) . ?
S1 C7 1.743(2) . ?
N1 C1 1.329(3) . ?
N1 C2 1.412(3) . ?
N1 C8 1.465(3) . ?
C2 C7 1.379(3) . ?
C2 C3 1.391(3) . ?
C3 C4 1.377(4) . ?
C4 C5 1.389(4) . ?
C5 C6 1.375(4) . ?
C6 C7 1.393(3) . ?
C8 C9 1.515(4) . ?
C9 C14 1.370(4) . ?
C9 C10 1.388(4) . ?
C10 C11 1.386(6) . ?
C11 C12 1.359(6) . ?
C12 C13 1.378(6) . ?
C13 C14 1.381(5) . ?
C1S C2S 1.3900 . ?
C1S C6S 1.3900 . ?
C1S C7S 1.413(11) . ?
C2S C3S 1.3900 . ?
C3S C4S 1.3900 . ?
C4S C5S 1.3900 . ?
C5S C6S 1.3900 . ?
C8S C9S 1.3900 . ?
C8S C13S 1.3900 . ?
C8S C14S 1.427(7) . ?
C9S C10S 1.3900 . ?
C10S C11S 1.3900 . ?
C11S C12S 1.3900 . ?
C12S C13S 1.3900 . ?
