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_4112010
_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_compound_source        'see text'
_chemical_formula_moiety         'C32 H40 F2 Sc, C24 H20 B, 2(C6 H5 F)'
_chemical_formula_sum            'C68 H70 B F4 Sc'
_chemical_formula_weight         1019.01
_chemical_name_systematic
;
  ?
;
_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     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             'Jan  7 12:26:03 2003'
_audit_creation_method
;
 PLATON <TABLE ACC> option 
 SHELXL97-2 & Manual Editing 
;
_cell_angle_alpha                90
_cell_angle_beta                 103.678(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0041(5)
_cell_length_b                   30.858(2)
_cell_length_c                   18.220(1)
_cell_measurement_reflns_used    8114
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.24
_cell_volume                     5465.1(5)
_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, 2002) 
 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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0788
_diffrn_reflns_av_sigmaI/netI    0.0797
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43752
_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        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_max  0.9831
_exptl_absorpt_correction_T_min  0.9193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick, Bruker, 2000))'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       needle
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         11105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+1.6264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                7526
_reflns_number_total             11105
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja054544irom20050708_022404.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4112010
_vrn_publ_code_void_volume       0.0
_vrn_publ_code_frame_time_sec    10.0
_vrn_publ_code_meas_time_hour    8.5