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_2013061
_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] I'
_chemical_formula_moiety         '2C24 H20 P + , C12 H12 O8 S4 Ni - , I -'
_chemical_formula_sum            'C60 H52 I Ni O8 P2 S4'
_chemical_formula_weight         1276.81
_chemical_name_systematic
;Bis(tetraphenylphosphonium)
bis(cis-1,2-dimethoxycarbonylethylenedithiolato-\k^2^S,S')nickelate(III)
 iodide
;
_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                85.671(4)
_cell_angle_beta                 77.541(4)
_cell_angle_gamma                80.240(4)
_cell_formula_units_Z            1
_cell_length_a                   9.4071(3)
_cell_length_b                   10.2501(6)
_cell_length_c                   15.4642(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2.2
_cell_volume                     1433.75(12)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       'non-profiled \w/2\q'
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8773
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        14
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.132
_exptl_absorpt_correction_T_max  0.601
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             651
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.63
_refine_ls_extinction_coef       0.0107(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         8343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_gt           0.032
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.1901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.097
_reflns_number_gt                6177
_reflns_number_total             8343
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn1015.cif
_cod_data_source_block           II
_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_database_code               2013061
_cod_database_fobs_code          2013061