Naked (C5Me5)2M Cations (M = Sc, Ti, and V) and Their Fluoroarene Complexes
Marco W. Bouwkamp; Peter H. M. Budzelaar; Jeroen Gercama; Isabel Del Hierro Morales; Jeanette de Wolf; Auke Meetsma; Sergei I. Troyanov; Jan H. Teuben; Bart Hessen; Journal of the American Chemical Society 127 (2005) 14310–14319; doi:10.1021/ja054544i

data_4112007
_publ_contact_author_address
;
     Crystal Structure Center,
     Inorganic Solid State Chemistry Laboratory
     Chemical Physics,
     Materials Science Center,
     Groningen University,
     Nijenborgh 4,
     NL-9747 AG Groningen,
     The Netherlands.
;
_publ_contact_author_email       A.Meetsma@fwn.rug.nl
_publ_contact_author_fax         '+31 50 3634441'
_publ_contact_author_name
;
   Drs. A. Meetsma
;
_publ_contact_author_phone       '+31 50 3634368'
_publ_section_title
;
 Naked (C5Me5)2M Cations (M = Sc, Ti, and V) and Their Fluoroarene
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14310
_journal_page_last               14319
_journal_paper_doi               10.1021/ja054544i
_journal_volume                  127
_journal_year                    2005
_chemical_absolute_configuration ad
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C44 H30 B F20 Ti'
_chemical_formula_sum            'C44 H30 B F20 Ti'
_chemical_formula_weight         997.37
_chemical_name_systematic        ' ?'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2003-07-15  15:01:01'
_audit_creation_method
;
 PLATON <TABLE ACC> option 
 SHELXL97-2 & Manual Editing 
;
_cell_angle_alpha                90
_cell_angle_beta                 93.967(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9750(8)
_cell_length_b                   17.053(1)
_cell_length_c                   12.0218(9)
_cell_measurement_reflns_used    5376
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      22.61
_cell_measurement_theta_min      2.37
_cell_volume                     2040.1(3)
_computing_cell_refinement       'SAINT, Bruker Version 6.02A, 2000'
_computing_data_collection       'SMART, Bruker Version 5.624, 2001'
_computing_data_reduction        'XPREP, Bruker Version 5.1/NT, 2000'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 2003) 
 PLATON (Spek, 1994)
;
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 DIRDIF-99 (Beurskens et al., 1999)
;
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean '4096x4096 / 62x62 (binned 512)'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
  Bruker Smart Apex 
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_detector
;
  CCD area-detector
;
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14710
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001)
;
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick, Bruker, 2000))'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.034
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
  Enantiomorph twin refinement resulted in 0.47(2) so ultimately set to 0.5
   Flack, H.D. & Bernardinelli, G. (1999, 2000)
;
_refine_ls_abs_structure_Flack   -0.05(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         7044
_refine_ls_number_restraints     285
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0941
_refine_ls_shift/su_max          0.265
_refine_ls_shift/su_mean         0.059
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1956P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2505
_refine_ls_wR_factor_ref         0.2780
_reflns_number_gt                4645
_reflns_number_total             7044
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja054544irom20050708_022308.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4112007
_vrn_publ_code_void_volume       31.3
_vrn_publ_code_frame_time_sec    30.0
_vrn_publ_code_meas_time_hour    18.0