Carbon-Fluorine Bond Cleavage in the Preparation of Osmium(III) and Osmium(IV) Fluorothiolate Complexes. Fluorine by Fluorine NMR-Assignment and Fluxional Processes
Maribel Arroyo; Sylvain Bernès; Margarita Cerón; Verónica Cortina; Consuelo Mendoza; Hugo Torrens; Inorganic Chemistry 46 (2007) 4857–4867; doi:10.1021/ic0619660

data_4307492
_publ_contact_author_address
;
Centro de Qu\'imica del Instituto de Ciencias de la BUAP 
Edificio 193 del Complejo de Ciencias 
Ciudad Universitaria 
San Manuel 
72571 Puebla, Pue. 
Mexico
;
_publ_contact_author_email       slarroyo@siu.buap.mx
_publ_contact_author_fax         (52)2222295551
_publ_contact_author_name        'Arroyo, Maribel'
_publ_contact_author_phone       (52)2222295500x7293
_publ_section_title
;
Carbon-Fluorine Bond Cleavage in the Preparation of Osmium(III) and
Osmium(IV) Fluorothiolate Complexes. Fluorine by Fluorine NMR-Assignment
and Fluxional Processes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4857
_journal_page_last               4867
_journal_paper_doi               10.1021/ic0619660
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C30 H5 F19 Os S5'
_chemical_formula_sum            'C30 H5 F19 Os S5'
_chemical_formula_weight         1076.84
_chemical_melting_point          485
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-02-15
_audit_creation_method           SHELXTL-Plus
_cell_angle_alpha                90.00
_cell_angle_beta                 97.707(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.3106(17)
_cell_length_b                   9.2362(11)
_cell_length_c                   20.0791(19)
_cell_measurement_reflns_used    85
_cell_measurement_temperature    296(1)
_cell_measurement_theta_max      13.02
_cell_measurement_theta_min      4.59
_cell_volume                     3365.1(6)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  SHELXTL-Plus
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1998)'
_diffrn_ambient_temperature      296(1)
_diffrn_detector                 'Scintillation counter'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10857
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.05
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30
_diffrn_source_power             1.5
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.230
_exptl_absorpt_correction_T_max  0.428
_exptl_absorpt_correction_T_min  0.216
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'XSCAnS (Bruker, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.483
_refine_diff_density_min         -2.649
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         8940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0773P)^2^+3.5751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1510
_reflns_number_gt                5979
_reflns_number_total             8940
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0619660si20061013_021620_3.cif
_cod_data_source_block           ed4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4307492