Coupling of CpCr(CO)3 and Heterocyclic Dithiadiazolyl Radicals. Synthetic, X-ray Diffraction, Dynamic NMR, EPR, CV, and DFT Studies
Hiu Fung Lau; Pearly Chwee Ying Ang; Victor Wee Lin Ng; Seah Ling Kuan; Lai Yoong Goh; Alexey S. Borisov; Paul Hazendonk; Tracey L. Roemmele; René T. Boeré; Richard D. Webster; Inorganic Chemistry 47 (2008) 632–644; doi:10.1021/ic702128f

data_4304586
_publ_contact_author
;
 Dr. Lai Yoong Goh
 Professor Rene T. Boere
;
_publ_contact_author_email
;
 LaiYoongGoh@ntu.edu.sg.
 boere@uleth.ca
;
_publ_contact_author_fax
;
+65 6316 6984
+1-403-329-2057
;
_publ_contact_author_phone       +65-6316-8792;
_publ_section_title
;
Coupling of CpCr(CO)3 and Heterocyclic Dithiadiazolyl Radicals. Synthetic,
X-ray Diffraction, Dynamic NMR, EPR, CV, and DFT Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              632
_journal_page_last               644
_journal_paper_doi               10.1021/ic702128f
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C8 H4 F3 N2 S2'
_chemical_formula_sum            'C8 H4 F3 N2 S2'
_chemical_formula_weight         249.25
_chemical_melting_point          143.5(15)
_chemical_name_common            pCF3DTDA
_chemical_name_systematic
4-(4-trifluoromethylphenyl)-1,2,3,5-dithiadiazolyl
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                91.579(1)
_cell_angle_beta                 97.329(1)
_cell_angle_gamma                102.755(1)
_cell_formula_units_Z            16
_cell_length_a                   9.4916(9)
_cell_length_b                   18.1887(17)
_cell_length_c                   22.275(2)
_cell_measurement_reflns_used    6940
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.52
_cell_volume                     3713.8(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury 1.5'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0812
_diffrn_reflns_av_sigmaI/netI    0.1217
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39140
_diffrn_reflns_theta_full        26.22
_diffrn_reflns_theta_max         26.22
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.9771
_exptl_absorpt_correction_T_min  0.9024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_meas      0
_exptl_crystal_description       needle
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.812
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1089
_refine_ls_number_reflns         14828
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0402P)^2^+1.2536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                7671
_reflns_number_total             14828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702128f-file001_6.cif
_cod_data_source_block           2d
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '142-145' was changed to '143.5(15)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4304586