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_7232205
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C45 H56 Ca Cl8 Fe2 O10 S8'
_chemical_formula_sum            'C45 H56 Ca Cl8 Fe2 O10 S8'
_chemical_formula_weight         1448.75
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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             2017-12-07T12:54:12-00:00
_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                86.715(12)
_cell_angle_beta                 89.542(12)
_cell_angle_gamma                63.187(12)
_cell_formula_units_Z            2
_cell_length_a                   12.7382(14)
_cell_length_b                   13.0035(11)
_cell_length_c                   21.730(4)
_cell_measurement_reflns_used    156
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     3206.5(8)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Mercury (CCDC, 2008)'
_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_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46297
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.241
_diffrn_reflns_theta_min         3.025
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.174
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.511
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     705
_refine_ls_number_reflns         11552
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0656
_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^)+(0.0583P)^2^+12.6036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1779
_reflns_Friedel_coverage         0
_reflns_number_gt                7670
_reflns_number_total             11552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01916a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7232202--7232208.cif.'
_cod_database_code               7232205
_shelx_res_checksum              47727