Stereochemical Inversion of a Coordinated, Curved Hydrocarbon: Syntheses and Structures of exo- and endo-[Ru(η6-fluoradene)(η-C5Me5)][CF3SO3]
Aibing Xia; John P. Selegue; Alberto Carrillo; Carolyn P. Brock; Journal of the American Chemical Society 122 (2000) 3973–3974; doi:10.1021/ja994266l

data_4115982
_publ_section_title
;
 Stereochemical Inversion of a Coordinated, Curved Hydrocarbon: Syntheses
 and Structures of exo- and endo-[Ru(\h6-fluoradene)(\h-C5Me5)][CF3SO3]
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3973
_journal_page_last               3974
_journal_paper_doi               10.1021/ja994266l
_journal_volume                  122
_journal_year                    2000
_chemical_compound_source
;
Synthesized in the laboratory of J. P. Selegue
;
_chemical_formula_moiety         '(C29 H27 Ru 1+), (C F3 S O3 1-)'
_chemical_formula_sum            'C30 H27 F3 O3 Ru S'
_chemical_formula_weight         625.67
_chemical_melting_point          506(2)
_chemical_name_systematic
;
endo-pentahapto-pentamethylcyclopentadienyl-hexahapto-7bH-
indeno[1,2,3-jk]fluoreneruthenium(II) trifluoromethanesulfonate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             96-03-28
_audit_creation_method           'created by SHELXL-93 and C P Brock'
_audit_update_record
;
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.723(4)
_cell_length_b                   7.1323(9)
_cell_length_c                   15.452(2)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    296(1)
_cell_measurement_theta_max      12.4
_cell_measurement_theta_min      11.7
_cell_volume                     2614.5(6)
_computing_cell_refinement       'CAD4-VAX (ENRAF-Nonius, 1988)'
_computing_data_collection       'CAD4-VAX (ENRAF-Nonius, 1988)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(1)
_diffrn_measurement_device       'ENRAF-Nonius CAD4-VAX diffractometer'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2385
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        <0.2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'based on 11 psi scans (Flack, 1977)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description
;
block
;
_exptl_crystal_F_000             1272
_exptl_crystal_preparation
;
Crystals were grown from dichloromethane by passing a slow stream of
nitrogen saturated with ethyl ether through the solution.
;
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.00
_refine_diff_density_min         -0.57
_refine_diff_density_rms         0.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.085
_refine_ls_goodness_of_fit_obs   1.102
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         2385
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_obs          0.0317
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+0.2338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0862
_refine_ls_wR_factor_obs         0.0772
_reflns_number_observed          1928
_reflns_number_total             2385
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja994266l_1.cif
_cod_data_source_block           RUFL2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+0.2338P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+0.2338P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115982