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_4112016
_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         'C28 H30 D16 O2 Sc, C24 H20 B'
_chemical_formula_sum            'C52 H50 B D16 O2 Sc'
_chemical_formula_weight         794.85
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2001-02-23  16:16:36'
_audit_creation_method           'PLATON <TABLE ACC> option'
_cell_angle_alpha                90
_cell_angle_beta                 95.8060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4868(5)
_cell_length_b                   21.575(1)
_cell_length_c                   18.957(1)
_cell_measurement_reflns_used    4470
_cell_measurement_temperature    90
_cell_measurement_theta_max      24.49
_cell_measurement_theta_min      2.17
_cell_volume                     4267.1(4)
_computing_cell_refinement       'SAINT, Bruker Version 6.02A, 2000'
_computing_data_collection       'SMART, Bruker Version 5.168, 2000'
_computing_data_reduction        'XPREP, Bruker Version 5.1/NT, 2000'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 2000) 
 PLATON (Spek, 1994, 1996)
;
_computing_publication_material
;
 PLATON (Spek, 1990)
 SHELXL (Sheldrick, 1997)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 DIRDIF-99 (Beurskens et al., 1999)
;
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type
;
  Bruker Smart Apex 
  Enraf Nonius CAD-4F diffractometer
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_detector
;
  CCD area-detector

     scintillation NaI crystal with photomultiplier
;
_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  0.0792
_diffrn_reflns_av_sigmaI/netI    0.0968
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40893
_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 SABABS (Sheldrick, 2000)
;
_diffrn_reflns_theta_full        25.1
_diffrn_reflns_theta_max         29.81
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.9647
_exptl_absorpt_correction_T_min  0.7920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         11341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.1137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                7212
_reflns_number_total             11341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja054544irom20050708_022551.cif
_cod_data_source_block           c52h50bd
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C52 H50 D16 B O2 Sc'
_cod_database_code               4112016