Synthesis and (spectro)electrochemistry of mixed-valent diferrocenyl-dihydrothiopyran derivatives.
Kowalski, Konrad; Karpowicz, Rafał; Mlostoń, Grzegorz; Miesel, Dominique; Hildebrandt, Alexander; Lang, Heinrich; Czerwieniec, Rafał; Therrien, Bruno; Dalton transactions (Cambridge, England : 2003) 44 (2015) 6268–6276; doi:10.1039/c5dt00246j

data_7034169
_publ_section_title
;
 Synthesis and (spectro)electrochemistry of mixed-valent
 diferrocenyl-dihydrothiopyran derivatives.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6268
_journal_page_last               6276
_journal_paper_doi               10.1039/c5dt00246j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C27 H28 Fe2 O2 S'
_chemical_formula_sum            'C27 H28 Fe2 O2 S'
_chemical_formula_weight         528.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-27 deposited with the CCDC.
2015-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                103.754(6)
_cell_angle_beta                 115.357(6)
_cell_angle_gamma                92.709(6)
_cell_formula_units_Z            4
_cell_length_a                   12.7358(10)
_cell_length_b                   14.2608(12)
_cell_length_c                   14.4554(11)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.00
_cell_measurement_theta_min      1.95
_cell_volume                     2271.0(4)
_computing_cell_refinement       'CELL (Stoe IPDS Software, 2000)'
_computing_data_collection       'EXPOSE (Stoe IPDS Software, 2000)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS Software, 2000)'
_computing_molecular_graphics    'ORTEP (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'phi oscillation'
_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  0.1299
_diffrn_reflns_av_sigmaI/netI    0.1794
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42615
_diffrn_reflns_theta_full        29.28
_diffrn_reflns_theta_max         29.28
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.392
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.470
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Walker, N. & Stuart, D. (1983)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.676
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         12288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.676
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                5481
_reflns_number_total             12288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00246j2.cif
_cod_data_source_block           complex10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 7034168--7034169.cif.
;
_cod_original_cell_volume        2271.0(3)
_cod_database_code               7034169