New Tetrathiapentalene-Derived Charge Transfer Salts with Paramagnetic Transition Metal Complex Anion: κ-(EDDH-TTP)3[Cr(phen)(NCS)4].2CH2Cl2 and κ21-(BDH-TTP)5[Cr(phen)(NCS)4]2.2CH2Cl2
Fatima Setifi; Lahcène Ouahab; Stéphane Golhen; Olivier Hernandez; Akira Miyazaki; Toshiaki Enoki; Takashi Toita; Jun-ichi Yamada; Hiroyuki Nishikawa; Andrzej Łapiński; Roman Świetlik; Inorganic Chemistry 41 (2002) 3761–3768; doi:10.1021/ic0255961

data_4318226
_publ_section_title
;
 New Tetrathiapentalene-Derived Charge Transfer Salts with Paramagnetic
 Transition Metal Complex Anion: \k-(EDDH-TTP)3[Cr(phen)(NCS)4].2CH2Cl2
 and \k21-(BDH-TTP)5[Cr(phen)(NCS)4]2.2CH2Cl2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3761
_journal_page_last               3768
_journal_paper_doi               10.1021/ic0255961
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C42 H28 Cl2 Cr N6 S24'
_chemical_formula_weight         1509.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 99.9297(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.8275(4)
_cell_length_b                   9.1015(2)
_cell_length_c                   27.04200(12)
_cell_measurement_reflns_used    11081
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     5776.64(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.1108
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            22157
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    1.199
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3056
_refine_diff_density_max         1.444
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         12961
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1660
_reflns_number_gt                6790
_reflns_number_total             12961
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255961_s1_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318226