Syntheses, X-ray crystal structures and properties of di- and tetra-ferrocenyl nickel-bis(1,4-dithiin-5,6-dithiolate) complexes
Lee, Ha-Jin; Noh, Dong-Youn; Journal of Materials Chemistry 10 (2000) 2167–; doi:10.1039/b001829p

data_7203974
_publ_section_title
;
 Syntheses, X-ray crystal structures and properties of di- and
 tetra-ferrocenyl nickel-bis(1,4-dithiin-5,6-dithiolate) complexes
;
_journal_issue                   9
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2167
_journal_paper_doi               10.1039/b001829p
_journal_volume                  10
_journal_year                    2000
_chemical_formula_moiety         (C16H36N)[Ni(C14H10S4Fe)2](C3H6O)0.5
_chemical_formula_sum            'C45.5 H59 Fe2 N Ni O0.5 S8'
_chemical_formula_weight         1054.83
_chemical_name_common            TBA[Ni(fcvdt)2](COMe2)0.5
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.503(4)
_cell_length_b                   10.841(3)
_cell_length_c                   24.137(5)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.47
_cell_measurement_theta_min      1.70
_cell_volume                     5064(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.593
_diffrn_measured_fraction_theta_max 0.593
_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  0.0659
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            4841
_diffrn_reflns_theta_full        23.47
_diffrn_reflns_theta_max         23.47
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.296
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             2204
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.441
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         4697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.750
_refine_ls_shift/su_mean         0.046
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1589P)^2^+2.2799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1971
_refine_ls_wR_factor_ref         0.2003
_reflns_number_gt                4519
_reflns_number_total             4697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001829p.txt
_cod_data_source_block           ni
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1589P)^2^+2.2799P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1589P)^2^+2.2799P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C45.50 H59 Fe2 N Ni O0.50 S8'
_cod_database_code               7203974