Bis(tetraphenylphosphonium) bis[<i>cis</i>-1,2-bis(methoxycarbonyl)ethylenedithiolato-κ^2^<i>S</i>,<i>S</i>']nickelate(II) and bis(tetraphenylphosphonium) bis[<i>cis</i>-1,2-bis(methoxycarbonyl)ethylenedithiolato-κ^2^<i>S</i>,<i>S</i>']nickelate(III) iodide
Baudron, Stephane A.; Batail, Patrick; Acta Crystallographica Section C 58 (2002) m575–m577; doi:10.1107/S0108270102019212

data_2013060
_publ_section_title
;Bis(tetraphenylphosphonium)
 bis[<i>cis</i>-1,2-bis(methoxycarbonyl)ethylenedithiolato-\k^2^<i>S</i>,<i>S</i>']nickelate(II)
 and bis(tetraphenylphosphonium)
 bis[<i>cis</i>-1,2-bis(methoxycarbonyl)ethylenedithiolato-\k^2^<i>S</i>,<i>S</i>']nickelate(III)
 iodide
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m575
_journal_page_last               m577
_journal_paper_doi               10.1107/S0108270102019212
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(C24 H20 P)2 [Ni (C6 H6 O4 S2)2]'
_chemical_formula_moiety         '2C24 H20 P + , C12 H12 O8 S4 Ni 2-'
_chemical_formula_sum            'C60 H52 Ni O8 P2 S4'
_chemical_formula_weight         1149.91
_chemical_name_systematic
;
Bis(tetraphenylphosphonium)
bis(cis-1,2-dimethoxycarbonylethylenedithiolato-\k^2^S,S')nickelate(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                68.023(16)
_cell_angle_beta                 68.730(15)
_cell_angle_gamma                80.092(17)
_cell_formula_units_Z            1
_cell_length_a                   10.2994(14)
_cell_length_b                   11.1508(16)
_cell_length_c                   13.8197(19)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_volume                     1370.3(4)
_computing_cell_refinement       'SELECT and CELL, both in IPDS'
_computing_data_collection       'EXPOSE in IPDS (Stoe & Cie, 1995)'
_computing_data_reduction        'INTEGRATE in IPDS'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.93
_diffrn_measured_fraction_theta_max 0.93
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'oscillation, \D\f = 1.4\%'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14269
_diffrn_reflns_theta_full        25.91
_diffrn_reflns_theta_max         25.91
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.62
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(FACEIT in IPDS; Stoe & Cie, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.16
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_gt           0.029
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0386P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.071
_reflns_number_gt                3899
_reflns_number_total             4966
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn1015.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1370.3(3)
_cod_database_code               2013060
_cod_database_fobs_code          2013060