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_4318225
_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_compound_source
;
?
;
_chemical_formula_moiety         ' C54.00 H36 Cr1 Cl4 N6 S34 '
_chemical_formula_sum            'C54 H36 Cl4 Cr N6 S34'
_chemical_formula_weight         2052.73
_chemical_melting_point          ?
_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
_audit_creation_date             01-12-12
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90.0000
_cell_angle_beta                 95.1951(16)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   25.07520(50)
_cell_length_b                   10.67320(29)
_cell_length_c                   28.16010(59)
_cell_measurement_reflns_used    40160
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.700
_cell_measurement_theta_min      0.998
_cell_volume                     7505.6(3)
_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_molecular_graphics
;                                                                               
 CAMERON (Watkin, Prout & Pearce,  1996)                                        
;
_computing_publication_material
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_computing_structure_refinement
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_computing_structure_solution    'SHELXS86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 9
_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_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.04
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21736
_diffrn_reflns_theta_max         0.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.29
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' black '
_exptl_crystal_density_diffrn    1.78
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' elongated plates '
_exptl_crystal_F_000             4026.45
_exptl_crystal_size_max          0.00
_exptl_crystal_size_mid          0.00
_exptl_crystal_size_min          0.00
_refine_diff_density_max         0.93
_refine_diff_density_min         -1.35
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.2034
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         6741
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.004314
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 5 parameters, Carruthers & Watkin , 1979, 
 1.01    0.464    0.741    0.332E-010.146    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0640
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                6741
_reflns_number_total             11765
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            ic0255961_s1_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

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.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        7505.602(304)
_cod_original_sg_symbol_H-M      'P 1 21/a 1 '
_cod_original_formula_sum        ' C54.00 H36 Cr1 Cl4 N6 S34 '
_cod_database_code               4318225