Bis(tetraphenylphosphonium) bis[<i>N</i>-(octylsulfonyl)dithiocarbimato(2‒)-κ^2^<i>S</i>,<i>S</i>']nickelate(II)
Cunha, Leandro M. G.; Rubinger, Mayura M. M.; Oliveira, Marcelo R. L.; Sabino, Jose R.; Acta Crystallographica Section E 64 (2008) m148–m149; doi:10.1107/S1600536807065014

data_2217349
_publ_section_title
;Bis(tetraphenylphosphonium)
 bis[<i>N</i>-(octylsulfonyl)dithiocarbimato(2--)-\k^2^<i>S</i>,<i>S</i>']nickelate(II)
;
_journal_coeditor_code           TK2230
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m148
_journal_page_last               m149
_journal_paper_doi               10.1107/S1600536807065014
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '(C24 H20 P)2 [Ni (C9 H17 N O2 S3)2]'
_chemical_formula_moiety         '2(C24 H20 P +), C18 H34 N2 Ni O4 S6 2-'
_chemical_formula_sum            'C66 H74 N2 Ni O4 P2 S6'
_chemical_formula_weight         1272.32
_chemical_melting_point          428
_chemical_name_systematic
;
Bis(tetraphenylphosphonium)
bis[<i>N</i>-(octylsulfonyl)dithiocarbimato(2-)-\k^2^S,S']nickelate(II)
;
_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_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 115.500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.113(4)
_cell_length_b                   10.425(2)
_cell_length_c                   22.966(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      16.2
_cell_volume                     6291.2(18)
_computing_cell_refinement       'CAD-4-PC (Enraf--Nonius, 1993)'
_computing_data_collection       'CAD-4-PC (Enraf--Nonius, 1993)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled \w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.079
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11798
_diffrn_reflns_theta_full        68
_diffrn_reflns_theta_max         68
_diffrn_reflns_theta_min         3.4
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.172
_exptl_absorpt_correction_T_max  0.787
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(Spek, 2003)'
_exptl_crystal_colour            dark-yellow
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.61
_refine_ls_extinction_coef       0.00064(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5696
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_gt           0.061
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1159P)^2^+8.6294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.208
_reflns_number_gt                3927
_reflns_number_total             5696
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2230.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
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:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' 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_cell_volume        6291.3(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2217349
_cod_database_fobs_code          2217349