Fusing Rigid Spin Probes to Paramagnetic Sandwiches. Synthesis, Crystal Structures, and NMR Spectroscopy of Bis(isodicyclopentadienyl)metal Compounds
Irene Gattinger; Martin A. Herker; Wolfgang Hiller; Frank H. Köhler; Inorganic Chemistry 38 (1999) 2359–2368; doi:10.1021/ic9812407

data_4322014
_publ_contact_author
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      Prof. Dr. Frank H. K\"ohler
      Technische Universit\"at M\"unchen
      Anorganisch-chemisches Institut 
      Lichtenbergstrasse 4
      D-85747 Garching
      Bundesrepublik Deutschland
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_publ_contact_author_email       F.H.Koehler@lrz.tu-muenchen.de
_publ_contact_author_fax         '049 89 289 13762'
_publ_contact_author_phone       '049 89 289 13109'
_publ_section_title
;
 Fusing Rigid Spin Probes to Paramagnetic Sandwiches. Synthesis, Crystal
 Structures, and NMR Spectroscopy of Bis(isodicyclopentadienyl)metal
 Compounds
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2359
_journal_page_last               2368
_journal_paper_doi               10.1021/ic9812407
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         'C20 H22 Cr F6 P'
_chemical_formula_sum            'C20 H22 Cr F6 P'
_chemical_formula_weight         229.67
_chemical_name_systematic
'Bis(tricyclo(5.2.1.0^2.6^)deca-2,4-dienyl)chromium(III) hexafluorophosphat'
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   9.7360(10)
_cell_length_b                   9.7360(10)
_cell_length_c                   16.7500(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    205(2)
_cell_measurement_theta_max      13.17
_cell_measurement_theta_min      9.47
_cell_volume                     1375.0(2)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        'CADSHEL V3.10 (Kopf, Ruebcke, 1993)'
_computing_molecular_graphics    'SHELXTL(TM) PC'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, Giacovazzo, 1992)'
_diffrn_ambient_temperature      205(2)
_diffrn_measurement_device       'CAD4 (ENRAF-NONIUS)'
_diffrn_measurement_method       'Omega / Theta'
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1840
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         3.43
_diffrn_standards_decay_%        2.09
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.444
_exptl_absorpt_correction_type   empiric
_exptl_crystal_colour            light_brown
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_F_000             705
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.208
_refine_diff_density_min         -.927
_refine_diff_density_rms         .103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_goodness_of_fit_obs   1.047
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1783
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.047
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_obs          0.0548
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1043P)^2^+2.3991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1523
_refine_ls_wR_factor_obs         0.1505
_reflns_number_observed          1733
_reflns_number_total             1783
_reflns_observed_criterion       >4sigma(F)
_cod_data_source_file            ic9812407_1.cif
_cod_data_source_block           5a+PF6-
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1043P)^2^+2.3991P] 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^)+(0.1043P)^2^+2.3991P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322014