Synthesis and structural characterization of transition metal dithiolene derivatives containing divalent metals as counter-cations
Castillo, Oscar; Delgado, Esther; Hernández, Diego; Hernández, Elisa; Martín, Avelino; Zamora, Félix; CrystEngComm 21 (2019) 1423–; doi:10.1039/C8CE01916A

data_7232206
_publ_section_title
;
 Synthesis and structural characterization of transition metal dithiolene
 derivatives containing divalent metals as counter-cations
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1423
_journal_paper_doi               10.1039/C8CE01916A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C48 H56 Cl8 Fe3 O10 S8'
_chemical_formula_sum            'C48 H56 Cl8 Fe3 O10 S8'
_chemical_formula_weight         1500.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2018-01-16T12:23:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-04-04 deposited with the CCDC.
2019-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                93.025(2)
_cell_angle_beta                 111.050(2)
_cell_angle_gamma                98.246(2)
_cell_formula_units_Z            1
_cell_length_a                   10.6545(3)
_cell_length_b                   11.3055(3)
_cell_length_c                   14.3597(4)
_cell_measurement_reflns_used    6367
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      2.52
_cell_measurement_wavelength     0.71073
_cell_volume                     1587.36(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker Kappa Apex II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24353
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.106
_diffrn_reflns_theta_max         24.106
_diffrn_reflns_theta_min         2.994
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.57
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.146
_refine_diff_density_min         -2.355
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5033
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1355P)^2^+1.4768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2013
_refine_ls_wR_factor_ref         0.2165
_reflns_Friedel_coverage         0
_reflns_number_gt                3792
_reflns_number_total             5033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01916a2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7232202--7232208.cif.'
_cod_database_code               7232206
_shelx_res_checksum              6789