Thiophene-Fused Nickel Dithiolenes: A Synthetic Scaffold for Highly Delocalized π-Electron Systems.
Amb, Chad M.; Heth, Christopher L.; Evenson, Sean J.; Pokhodnya, Konstantin I.; Rasmussen, Seth C.; Inorganic chemistry 55 (2016) 10978–10989; doi:10.1021/acs.inorgchem.6b01513

data_4348682
_publ_section_title
;
 Thiophene-Fused Nickel Dithiolenes: A Synthetic Scaffold for Highly
 Delocalized \p-Electron Systems.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10978
_journal_page_last               10989
_journal_paper_doi               10.1021/acs.inorgchem.6b01513
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C20 H12 Ni S6, C6 H8 N, C3 H7 N O'
_chemical_formula_sum            'C29 H27 N2 Ni O S6'
_chemical_formula_weight         670.60
_chemical_melting_point_gt       573
_chemical_name_common
'Methylpyridinium Bis(phenylthiophenedithiolato)nickelate'
_chemical_name_systematic
; 
N-Methylpyridinium Bis(5-phenyl-2,3-thiophenedithiolato)nickelate(III) 
;
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 105.043(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.799(3)
_cell_length_b                   10.7709(15)
_cell_length_c                   16.151(2)
_cell_measurement_reflns_used    1008
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.23
_cell_measurement_theta_min      2.74
_cell_volume                     2990.2(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9816
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_T_max  0.7565
_exptl_absorpt_correction_T_min  0.6685
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'wine red'
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lump
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.15(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5626
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+1.3359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                3652
_reflns_number_total             5626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01513_si_002.cif
_cod_data_source_block           cxa5m
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_chemical_melting_point' was changed to
'_chemical_melting_point_gt' since the value was specified as 'more
than' ('>') a certain temperature.

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2990.2(7)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4348682