A new family of sulfur-rich ligands based on the dmit system: synthesis and metal complexation of 4‒4'-covalently bridged bis(2-thioxo-1,3-dithiol-5-thiolato) units
Allen, David W.; Berridge, Rory; Bricklebank, Neil; Cerrada, Elena; Light, Mark E.; Hursthouse, Michael B.; Laguna, Mariano; Moreno, Ana; Skabara, Peter J.; Journal of the Chemical Society, Dalton Transactions  (2002) 2654–; doi:10.1039/b201615j

data_7011567
_publ_section_title
;
 A new family of sulfur-rich ligands based on the dmit system:
 synthesis and metal complexation of 4--4'-covalently bridged
 bis(2-thioxo-1,3-dithiol-5-thiolato) units
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2654
_journal_paper_doi               10.1039/b201615j
_journal_year                    2002
_chemical_formula_sum            'C24 H18 N2 Ni S10'
_chemical_formula_weight         713.71
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.558(3)
_cell_angle_beta                 86.314(3)
_cell_angle_gamma                67.969(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5662(6)
_cell_length_b                   12.5254(8)
_cell_length_c                   14.0131(8)
_cell_measurement_reflns_used    4319
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2.95
_cell_volume                     1513.33(17)
_computing_cell_refinement
;
DENZO (Otwinowski and MInor, 1997), COLLECT (Hooft, 1998)
;
_computing_data_collection
;
DENZO (Otwinowski and Minor, 1997), COLLECT (Hooft, 1998)
;
_computing_data_reduction
;
DENZO (Otwinowski and MInor, 1997), COLLECT (Hooft, 1998),
MAXUS (Mackay et al., 1998)
;
_computing_molecular_graphics    'ORTEP-III (Burnett et al., 1996)'
_computing_publication_material  'WINGX (Farrugia (1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean '9.091 pixels/mm'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans to fill Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1189
_diffrn_reflns_av_sigmaI/netI    0.0918
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18864
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_T_max  0.8768
_exptl_absorpt_correction_T_min  0.7740
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+0.1975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1364
_reflns_number_gt                2692
_reflns_number_total             4319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b201615j.txt
_cod_data_source_block           s92
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+0.1975P] 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^)+(0.0599P)^2^+0.1975P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1513.32(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011567