#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:51:43 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179767 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/63/7006300.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_7006300
loop_
_publ_author_name
'Geary, Elaine A. M.'
'Yellowlees, Lesley J.'
'Parsons, Simon'
'Pilia, Luca'
'Serpe, Angela'
'Mercuri, M. Laura'
'Deplano, Paola'
'Clark, Stewart J.'
'Robertson, Neil'
_publ_section_title
;
 Influence of the R-substituents on the properties of
 [Ni(R2pipdt)(dmit)] complexes and crystal structure where R = CH2C6H5.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5453
_journal_page_last               5459
_journal_paper_doi               10.1039/b712243h
_journal_year                    2007
_chemical_compound_source        'Elaine Geary, Reaction EG25F'
_chemical_formula_moiety         'C21 H18 N2 Ni S7'
_chemical_formula_sum            'C21 H18 N2 Ni S7'
_chemical_formula_weight         581.50
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.1586(6)
_cell_length_b                   19.5819(5)
_cell_length_c                   6.1048(2)
_cell_measurement_reflns_used    7912
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2
_cell_volume                     2290.29(12)
_computing_cell_refinement       Saint
_computing_data_collection       Smart
_computing_data_reduction        Saint
_computing_molecular_graphics    XP
_computing_publication_material  'Platon, Xcif, Encifer'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Dirdif
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       Omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            25384
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         2.08
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.500
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs v2004/1'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1192
_exptl_crystal_recrystallization_method
'From saturated DMF solution layered with MeCN and Et2O'
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2941
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0433P)²+0.7538P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                2487
_reflns_number_total             2941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b712243h.txt
_cod_data_source_block           nr0505
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multiscan' changed to 'multi-scan'
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_database_code               7006300
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, z+1/2'
'x, -y+1/2, z'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, -z-1/2'
'-x, y-1/2, -z'
'x-1/2, y, -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 0.647081(14) 0.2500 0.13242(5) 0.01963(9) Uani 1 2 d S . .
S11 S 0.69260(2) 0.33081(2) -0.06226(7) 0.02516(11) Uani 1 1 d . . .
C21 C 0.73781(8) 0.28445(8) -0.2575(3) 0.0214(3) Uani 1 1 d . . .
S31 S 0.78670(2) 0.32348(2) -0.46334(7) 0.02655(11) Uani 1 1 d . . .
C41 C 0.81680(11) 0.2500 -0.5882(4) 0.0226(5) Uani 1 2 d S . .
S51 S 0.87032(3) 0.2500 -0.80073(11) 0.03205(16) Uani 1 2 d S . .
S12 S 0.59938(3) 0.32812(2) 0.32880(8) 0.03544(14) Uani 1 1 d . . .
C22 C 0.55208(8) 0.28771(8) 0.5234(3) 0.0202(3) Uani 1 1 d . . .
N32 N 0.51728(7) 0.32092(7) 0.6774(2) 0.0216(3) Uani 1 1 d D . .
C42 C 0.4861(2) 0.28722(17) 0.8627(6) 0.0231(7) Uiso 0.50 1 d PD . -1
H42A H 0.4456 0.3141 0.9148 0.028 Uiso 0.50 1 calc PR . -1
H42B H 0.5205 0.2845 0.9835 0.028 Uiso 0.50 1 calc PR . -1
C52 C 0.4625(2) 0.21637(17) 0.8020(6) 0.0227(7) Uiso 0.50 1 d PD . -1
H52A H 0.4511 0.1906 0.9369 0.027 Uiso 0.50 1 calc PR . -1
H52B H 0.4196 0.2194 0.7121 0.027 Uiso 0.50 1 calc PR . -1
C62 C 0.52155(9) 0.39565(8) 0.7071(3) 0.0264(4) Uani 1 1 d . . .
H62A H 0.5561 0.4146 0.6031 0.032 Uiso 1 1 calc R . .
H62B H 0.5379 0.4058 0.8575 0.032 Uiso 1 1 calc R . .
C72 C 0.45191(9) 0.42973(8) 0.6702(3) 0.0246(4) Uani 1 1 d . . .
C82 C 0.41821(10) 0.42409(10) 0.4704(3) 0.0358(4) Uani 1 1 d . . .
H82 H 0.4390 0.3983 0.3559 0.043 Uiso 1 1 calc R . .
C92 C 0.35456(11) 0.45563(12) 0.4357(4) 0.0474(5) Uani 1 1 d . . .
H92 H 0.3313 0.4507 0.2992 0.057 Uiso 1 1 calc R . .
C102 C 0.32488(11) 0.49437(10) 0.6002(4) 0.0455(5) Uani 1 1 d . . .
H102 H 0.2817 0.5170 0.5752 0.055 Uiso 1 1 calc R . .
C112 C 0.35749(10) 0.50033(10) 0.7998(4) 0.0393(5) Uani 1 1 d . . .
H112 H 0.3368 0.5268 0.9128 0.047 Uiso 1 1 calc R . .
C122 C 0.42076(10) 0.46753(9) 0.8359(3) 0.0309(4) Uani 1 1 d . . .
H122 H 0.4428 0.4710 0.9748 0.037 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'
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
S12 Ni1 S12 90.84(3) . 3 ?
S12 Ni1 S11 87.544(16) . . ?
S12 Ni1 S11 178.23(2) 3 . ?
S12 Ni1 S11 178.23(2) . 3 ?
S12 Ni1 S11 87.541(16) 3 3 ?
S11 Ni1 S11 94.07(2) . 3 ?
C21 S11 Ni1 101.32(6) . . ?
C21 C21 S11 121.65(5) 3 . ?
C21 C21 S31 116.00(5) 3 . ?
S11 C21 S31 122.35(9) . . ?
C41 S31 C21 97.60(9) . . ?
S51 C41 S31 123.59(7) . . ?
S51 C41 S31 123.59(7) . 3 ?
S31 C41 S31 112.81(13) . 3 ?
C22 S12 Ni1 106.68(5) . . ?
N32 C22 C22 119.43(9) . 3 ?
N32 C22 S12 122.64(12) . . ?
C22 C22 S12 117.90(5) 3 . ?
C22 N32 C42 122.83(18) . . ?
C22 N32 C62 123.11(14) . . ?
C42 N32 C62 112.38(18) . . ?
C22 N32 C52 118.52(17) . 3 ?
C42 N32 C52 23.14(16) . 3 ?
C62 N32 C52 117.56(17) . 3 ?
N32 C42 C52 110.7(3) . . ?
N32 C52 C42 111.5(3) 3 . ?
N32 C62 C72 111.77(13) . . ?
C82 C72 C122 118.94(17) . . ?
C82 C72 C62 120.57(15) . . ?
C122 C72 C62 120.50(16) . . ?
C92 C82 C72 120.67(19) . . ?
C102 C92 C82 119.8(2) . . ?
C112 C102 C92 120.27(19) . . ?
C102 C112 C122 119.86(19) . . ?
C72 C122 C112 120.41(19) . . ?
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 S12 2.1477(5) . ?
Ni1 S12 2.1477(5) 3 ?
Ni1 S11 2.1627(4) . ?
Ni1 S11 2.1628(4) 3 ?
S11 C21 1.7306(16) . ?
C21 C21 1.349(3) 3 ?
C21 S31 1.7440(16) . ?
S31 C41 1.7274(14) . ?
C41 S51 1.654(2) . ?
C41 S31 1.7275(13) 3 ?
S12 C22 1.6908(16) . ?
C22 N32 1.323(2) . ?
C22 C22 1.477(3) 3 ?
N32 C42 1.440(3) . ?
N32 C62 1.477(2) . ?
N32 C52 1.488(4) 3 ?
C42 C52 1.506(4) . ?
C52 N32 1.488(4) 3 ?
C62 C72 1.509(2) . ?
C72 C82 1.385(3) . ?
C72 C122 1.388(2) . ?
C82 C92 1.383(3) . ?
C92 C102 1.381(3) . ?
C102 C112 1.374(3) . ?
C112 C122 1.389(3) . ?
