#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/88/2208819.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2208819
loop_
_publ_author_name
'Singh, S. S.'
'Prasad, R. S.'
'Upreti, Shailesh'
'Jha, N. K.'
'Ramanan, A.'
_publ_section_title
;
 Tetraphenylarsonium diisothiocyanatodibromonickelate(II)
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1014
_journal_page_last               m1015
_journal_paper_doi               10.1107/S160053680601021X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C24 H20 As)2 [Ni Br2 (C N S)2]'
_chemical_formula_moiety         '2C24 H20 As, C2 Br2 N2 Ni S2'
_chemical_formula_sum            'C50 H40 As2 Br2 N2 Ni S2'
_chemical_formula_weight         1101.31
_chemical_melting_point          527.5
_chemical_name_common            diisothiocyanatodihalonickelates(II)
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 105.3470(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5382(10)
_cell_length_b                   15.7796(11)
_cell_length_c                   23.0555(16)
_cell_measurement_reflns_used    7590
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.39
_cell_volume                     4749.7(6)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'SHELXTL (Bruker, 2000) and DIAMOND (Klaus, 1999)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0765
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17670
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.83
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.597
_exptl_absorpt_correction_T_max  0.711
_exptl_absorpt_correction_T_min  0.401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.351
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.878
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0881P)²+1.9894P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1412
_reflns_number_gt                3556
_reflns_number_total             4430
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ci2014.cif
_cod_data_source_block           I
_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 

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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2208819
_cod_database_fobs_code          2208819
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
As As1 0.58663(3) 0.12653(2) 0.418660(16) 0.04477(16) Uani d . 1
Ni Ni1 1.0000 0.13439(5) 0.2500 0.0385(2) Uani d S 1
S S1 0.73060(10) 0.30693(9) 0.14359(6) 0.0765(4) Uani d . 1
Br Br1 0.92718(4) 0.06174(4) 0.31913(2) 0.0452(2) Uani d . 1
N N1 0.8894(4) 0.2103(3) 0.2063(2) 0.0821(12) Uani d . 1
C C1 0.4984(3) 0.0538(2) 0.36218(17) 0.0484(9) Uani d . 1
C C2 0.5149(4) -0.0318(3) 0.3626(2) 0.0688(12) Uani d . 1
H H2 0.5671 -0.0562 0.3925 0.083 Uiso calc R 1
C C3 0.4534(5) -0.0817(3) 0.3182(3) 0.0882(17) Uani d . 1
H H3 0.4658 -0.1396 0.3173 0.106 Uiso calc R 1
C C4 0.3750(4) -0.0464(4) 0.2761(2) 0.0809(15) Uani d . 1
H H4 0.3342 -0.0804 0.2462 0.097 Uiso calc R 1
C C5 0.3549(4) 0.0390(4) 0.2767(2) 0.0853(16) Uani d . 1
H H5 0.2998 0.0624 0.2482 0.102 Uiso calc R 1
C C6 0.4174(4) 0.0897(3) 0.3203(2) 0.0736(13) Uani d . 1
H H6 0.4048 0.1475 0.3213 0.088 Uiso calc R 1
C C7 0.6236(3) 0.2182(2) 0.37435(17) 0.0464(8) Uani d . 1
C C8 0.7064(3) 0.2124(3) 0.3498(2) 0.0626(11) Uani d . 1
H H8 0.7499 0.1658 0.3581 0.075 Uiso calc R 1
C C9 0.7234(5) 0.2752(4) 0.3135(2) 0.0866(16) Uani d . 1
H H9 0.7799 0.2721 0.2978 0.104 Uiso calc R 1
C C10 0.6581(5) 0.3433(4) 0.2996(3) 0.0805(14) Uani d . 1
H H10 0.6699 0.3856 0.2741 0.097 Uiso calc R 1
C C11 0.5783(4) 0.3486(3) 0.3227(2) 0.0771(14) Uani d . 1
H H11 0.5339 0.3945 0.3126 0.092 Uiso calc R 1
C C12 0.5596(3) 0.2869(3) 0.3617(2) 0.0629(11) Uani d . 1
H H12 0.5049 0.2923 0.3788 0.075 Uiso calc R 1
C C13 0.5172(3) 0.1748(3) 0.47295(17) 0.0516(9) Uani d . 1
C C14 0.5642(4) 0.2396(3) 0.5098(2) 0.0736(13) Uani d . 1
H H14 0.6272 0.2607 0.5076 0.088 Uiso calc R 1
C C15 0.5147(5) 0.2724(4) 0.5504(2) 0.0851(16) Uani d . 1
H H15 0.5463 0.3145 0.5771 0.102 Uiso calc R 1
C C16 0.4208(5) 0.2438(4) 0.5516(2) 0.0810(16) Uani d . 1
H H16 0.3882 0.2670 0.5787 0.097 Uiso calc R 1
C C17 0.3744(4) 0.1822(4) 0.5139(2) 0.0750(14) Uani d . 1
H H17 0.3094 0.1639 0.5147 0.090 Uiso calc R 1
C C18 0.4217(3) 0.1459(3) 0.4742(2) 0.0620(11) Uani d . 1
H H18 0.3899 0.1026 0.4487 0.074 Uiso calc R 1
C C19 0.7033(3) 0.0648(3) 0.46357(19) 0.0531(10) Uani d . 1
C C20 0.7222(4) 0.0613(3) 0.5254(2) 0.0735(13) Uani d . 1
H H20 0.6797 0.0885 0.5453 0.088 Uiso calc R 1
C C21 0.8076(5) 0.0151(4) 0.5569(3) 0.103(2) Uani d . 1
H H21 0.8220 0.0113 0.5985 0.124 Uiso calc R 1
C C22 0.8694(5) -0.0237(4) 0.5284(3) 0.099(2) Uani d . 1
H H22 0.9266 -0.0528 0.5508 0.118 Uiso calc R 1
C C23 0.8502(4) -0.0216(4) 0.4674(3) 0.0904(17) Uani d . 1
H H23 0.8925 -0.0499 0.4480 0.108 Uiso calc R 1
C C24 0.7655(3) 0.0241(3) 0.4346(2) 0.0675(12) Uani d . 1
H H24 0.7514 0.0269 0.3930 0.081 Uiso calc R 1
C C25 0.8254(4) 0.2476(3) 0.18115(18) 0.0468(10) Uani d . 1
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'
As As 0.0499 2.0058 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 As1 C19 . . 110.05(17) y
C1 As1 C13 . . 111.13(17) y
C19 As1 C13 . . 109.14(18) y
C1 As1 C7 . . 107.25(16) y
C19 As1 C7 . . 112.29(17) y
C13 As1 C7 . . 106.97(16) y
N1 Ni1 N1 . 2_755 105.2(3) y
N1 Ni1 Br1 . 2_755 110.11(13) y
N1 Ni1 Br1 2_755 2_755 103.98(13) ?
N1 Ni1 Br1 . . 103.98(13) y
N1 Ni1 Br1 2_755 . 110.11(13) ?
Br1 Ni1 Br1 2_755 . 122.37(4) y
C25 N1 Ni1 . . 175.5(5) ?
C2 C1 C6 . . 120.6(4) ?
C2 C1 As1 . . 121.3(3) ?
C6 C1 As1 . . 118.1(3) ?
C1 C2 C3 . . 119.5(5) ?
C1 C2 H2 . . 120.3 ?
C3 C2 H2 . . 120.3 ?
C4 C3 C2 . . 120.0(5) ?
C4 C3 H3 . . 120.0 ?
C2 C3 H3 . . 120.0 ?
C3 C4 C5 . . 121.0(5) ?
C3 C4 H4 . . 119.5 ?
C5 C4 H4 . . 119.5 ?
C4 C5 C6 . . 119.3(5) ?
C4 C5 H5 . . 120.4 ?
C6 C5 H5 . . 120.4 ?
C1 C6 C5 . . 119.5(5) ?
C1 C6 H6 . . 120.3 ?
C5 C6 H6 . . 120.3 ?
C12 C7 C8 . . 119.9(4) ?
C12 C7 As1 . . 118.2(3) ?
C8 C7 As1 . . 121.5(3) ?
C9 C8 C7 . . 119.5(5) ?
C9 C8 H8 . . 120.3 ?
C7 C8 H8 . . 120.3 ?
C8 C9 C10 . . 120.8(5) ?
C8 C9 H9 . . 119.6 ?
C10 C9 H9 . . 119.6 ?
C11 C10 C9 . . 119.8(5) ?
C11 C10 H10 . . 120.1 ?
C9 C10 H10 . . 120.1 ?
C10 C11 C12 . . 121.4(5) ?
C10 C11 H11 . . 119.3 ?
C12 C11 H11 . . 119.3 ?
C7 C12 C11 . . 118.5(4) ?
C7 C12 H12 . . 120.7 ?
C11 C12 H12 . . 120.7 ?
C14 C13 C18 . . 121.1(4) ?
C14 C13 As1 . . 118.3(3) ?
C18 C13 As1 . . 120.5(3) ?
C13 C14 C15 . . 117.9(5) ?
C13 C14 H14 . . 121.1 ?
C15 C14 H14 . . 121.1 ?
C16 C15 C14 . . 120.8(5) ?
C16 C15 H15 . . 119.6 ?
C14 C15 H15 . . 119.6 ?
C17 C16 C15 . . 120.5(5) ?
C17 C16 H16 . . 119.7 ?
C15 C16 H16 . . 119.7 ?
C16 C17 C18 . . 120.8(5) ?
C16 C17 H17 . . 119.6 ?
C18 C17 H17 . . 119.6 ?
C17 C18 C13 . . 118.8(5) ?
C17 C18 H18 . . 120.6 ?
C13 C18 H18 . . 120.6 ?
C24 C19 C20 . . 121.1(4) ?
C24 C19 As1 . . 120.2(3) ?
C20 C19 As1 . . 118.7(3) ?
C19 C20 C21 . . 117.3(5) ?
C19 C20 H20 . . 121.4 ?
C21 C20 H20 . . 121.4 ?
C22 C21 C20 . . 121.5(6) ?
C22 C21 H21 . . 119.3 ?
C20 C21 H21 . . 119.3 ?
C21 C22 C23 . . 121.4(5) ?
C21 C22 H22 . . 119.3 ?
C23 C22 H22 . . 119.3 ?
C22 C23 C24 . . 118.5(6) ?
C22 C23 H23 . . 120.8 ?
C24 C23 H23 . . 120.8 ?
C19 C24 C23 . . 120.2(5) ?
C19 C24 H24 . . 119.9 ?
C23 C24 H24 . . 119.9 ?
N1 C25 S1 . . 178.0(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
As1 C1 . 1.902(4) y
As1 C19 . 1.911(4) y
As1 C13 . 1.911(4) y
As1 C7 . 1.912(4) y
Ni1 N1 . 1.973(5) y
Ni1 N1 2_755 1.973(5) ?
Ni1 Br1 2_755 2.3786(6) ?
Ni1 Br1 . 2.3787(6) y
S1 C25 . 1.639(5) ?
N1 C25 . 1.080(6) ?
C1 C2 . 1.369(6) ?
C1 C6 . 1.376(6) ?
C2 C3 . 1.382(7) ?
C2 H2 . 0.93 ?
C3 C4 . 1.355(8) ?
C3 H3 . 0.93 ?
C4 C5 . 1.376(8) ?
C4 H4 . 0.93 ?
C5 C6 . 1.384(7) ?
C5 H5 . 0.93 ?
C6 H6 . 0.93 ?
C7 C12 . 1.371(6) ?
C7 C8 . 1.387(6) ?
C8 C9 . 1.355(7) ?
C8 H8 . 0.93 ?
C9 C10 . 1.374(8) ?
C9 H9 . 0.93 ?
C10 C11 . 1.328(7) ?
C10 H10 . 0.93 ?
C11 C12 . 1.393(7) ?
C11 H11 . 0.93 ?
C12 H12 . 0.93 ?
C13 C14 . 1.372(6) ?
C13 C18 . 1.380(6) ?
C14 C15 . 1.387(7) ?
C14 H14 . 0.93 ?
C15 C16 . 1.356(8) ?
C15 H15 . 0.93 ?
C16 C17 . 1.343(8) ?
C16 H16 . 0.93 ?
C17 C18 . 1.374(7) ?
C17 H17 . 0.93 ?
C18 H18 . 0.93 ?
C19 C24 . 1.365(6) ?
C19 C20 . 1.381(6) ?
C20 C21 . 1.397(8) ?
C20 H20 . 0.93 ?
C21 C22 . 1.341(9) ?
C21 H21 . 0.93 ?
C22 C23 . 1.361(9) ?
C22 H22 . 0.93 ?
C23 C24 . 1.394(7) ?
C23 H23 . 0.93 ?
C24 H24 . 0.93 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C19 As1 C1 C2 8.1(4)
C13 As1 C1 C2 -112.9(4)
C7 As1 C1 C2 130.6(4)
C19 As1 C1 C6 -171.4(4)
C13 As1 C1 C6 67.6(4)
C7 As1 C1 C6 -49.0(4)
C6 C1 C2 C3 4.0(8)
As1 C1 C2 C3 -175.5(4)
C1 C2 C3 C4 -2.4(9)
C2 C3 C4 C5 -0.4(9)
C3 C4 C5 C6 1.6(9)
C2 C1 C6 C5 -2.7(8)
As1 C1 C6 C5 176.8(4)
C4 C5 C6 C1 -0.1(9)
C1 As1 C7 C12 86.2(4)
C19 As1 C7 C12 -152.8(3)
C13 As1 C7 C12 -33.1(4)
C1 As1 C7 C8 -86.8(4)
C19 As1 C7 C8 34.2(4)
C13 As1 C7 C8 153.9(3)
C12 C7 C8 C9 0.2(7)
As1 C7 C8 C9 173.1(4)
C7 C8 C9 C10 -1.6(8)
C8 C9 C10 C11 1.1(9)
C9 C10 C11 C12 1.0(9)
C8 C7 C12 C11 1.7(7)
As1 C7 C12 C11 -171.4(3)
C10 C11 C12 C7 -2.4(8)
C1 As1 C13 C14 -169.1(4)
C19 As1 C13 C14 69.4(4)
C7 As1 C13 C14 -52.3(4)
C1 As1 C13 C18 10.0(4)
C19 As1 C13 C18 -111.5(4)
C7 As1 C13 C18 126.8(4)
C18 C13 C14 C15 2.9(8)
As1 C13 C14 C15 -178.0(4)
C13 C14 C15 C16 -2.9(9)
C14 C15 C16 C17 0.9(9)
C15 C16 C17 C18 1.2(8)
C16 C17 C18 C13 -1.1(7)
C14 C13 C18 C17 -1.0(7)
As1 C13 C18 C17 180.0(4)
C1 As1 C19 C24 57.7(4)
C13 As1 C19 C24 179.9(3)
C7 As1 C19 C24 -61.7(4)
C1 As1 C19 C20 -121.4(4)
C13 As1 C19 C20 0.8(4)
C7 As1 C19 C20 119.2(4)
C24 C19 C20 C21 0.5(7)
As1 C19 C20 C21 179.5(4)
C19 C20 C21 C22 0.5(9)
C20 C21 C22 C23 -1.5(10)
C21 C22 C23 C24 1.6(9)
C20 C19 C24 C23 -0.4(7)
As1 C19 C24 C23 -179.4(4)
C22 C23 C24 C19 -0.6(8)
