Nickel dithiolene complexes as a source of a new family of S,S-dinegative chiral ligands R4btimdt = 5,5′-bis(1,3-dialkyl-4-imidazolidine-2-thione-4-thiolate)
Bigoli, Francesco; Curreli, Simona; Deplano, Paola; Leoni, Laura; Mercuri, Maria Laura; Pellinghelli, Maria Angela; Serpe, Angela; Trogu, Emanuele F.; Journal of the Chemical Society, Dalton Transactions  (2002) 1985–; doi:10.1039/b108471b

data_7702726
_publ_section_title
;
 Nickel dithiolene complexes as a source of a new family of S,S-dinegative
 chiral ligands R4btimdt =
 5,5&#x2032;-bis(1,3-dialkyl-4-imidazolidine-2-thione-4-thiolate)
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1985
_journal_paper_doi               10.1039/b108471b
_journal_year                    2002
_chemical_formula_sum            'C64 H69 N4 Ni P3 S4'
_chemical_formula_weight         1174.09
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                78.69(2)
_cell_angle_beta                 75.88(2)
_cell_angle_gamma                69.89(2)
_cell_formula_units_Z            2
_cell_length_a                   11.057(4)
_cell_length_b                   12.973(6)
_cell_length_c                   23.023(9)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      18
_cell_volume                     2985(2)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Enraf_Nonius CAD4 local upgrade'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    ZORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Enraf-Nonius CAD4 diffractometer -diffrn_measurement_method \q/2\q'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1024
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11289
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_diffrn_reflns_theta_min         3.66
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    2.866
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.00005(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         11289
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1907
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          1.972
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1507P)^2^+2.8699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2243
_refine_ls_wR_factor_ref         0.3316
_reflns_number_gt                4884
_reflns_number_total             11289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108471b.txt
_cod_data_source_block           '[Ni(tp)(Bu4btimdt)]'
_cod_depositor_comments
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The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file
'/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/lists/replacement-tags.lst'.

Automatic conversion script
Id: cif_correct_tags 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702726