Pentaarylfullerenes as Noncoordinating Cyclopentadienyl Anions
Marco W. Bouwkamp; Auke Meetsma; Inorganic Chemistry 48 (2009) 8–9; doi:10.1021/ic802034m

data_4301162
_publ_contact_author_address
;
  Crystal Structure Center, Chemical Physics,
  Zernike Institute for Advanced Materials,
  University of Groningen,
  Nijenborgh 4,
  NL-9747 AG Groningen, The Netherlands.
;
_publ_contact_author_email       A.Meetsma@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
;
Pentaarylfullerenes as Noncoordinating Cyclopentadienyl Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8
_journal_page_last               9
_journal_paper_doi               10.1021/ic802034m
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C90 H25, C14 H34 N3 O2 Zr'
_chemical_formula_sum            'C104 H59 N3 O2 Zr'
_chemical_formula_weight         1473.76
_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     direct
_atom_sites_solution_secondary   direct
_audit_creation_date             '2008-09-23  18:28:14'
_audit_creation_method
;
 PLATON <TABLE ACC> option    (version ::  80708)
 SHELXL97-2 & Manual Editing 
;
_audit_update_record
;
?

2008-09-24 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 96.175(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.309(3)
_cell_length_b                   18.453(3)
_cell_length_c                   26.167(5)
_cell_measurement_reflns_used    5699
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      21.80
_cell_measurement_theta_min      2.71
_cell_volume                     6869(2)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_molecular_graphics
;
 PLATON (Spek, 2003)
 PLUTO (Meetsma, 2008) 
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
;
 SIR2004 (Burla et al., 2005)
;
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
  Bruker Smart Apex; CCD area detector 
;
_diffrn_measurement_method       '\f and \w 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1211
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43916
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT-Plus & SADABS (Bruker, 2007).
;
_diffrn_reflns_theta_full        21.49
_diffrn_reflns_theta_max         21.49
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  0.9610
_exptl_absorpt_correction_T_min  0.9047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, (Bruker, 2007))'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.26
_platon_squeeze_details
;
;
_refine_diff_density_max         1.588
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.362
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         7844
_refine_ls_number_restraints     1101
_refine_ls_restrained_S_all      3.314
_refine_ls_R_factor_all          0.2276
_refine_ls_R_factor_gt           0.1390
_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^)+(0.0P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2271
_refine_ls_wR_factor_ref         0.2346
_reflns_number_gt                4174
_reflns_number_total             7844
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic802034m_si_002_3.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4301162
_vrn_publ_code_void_volume       563.9
_vrn_publ_code_number_frames     1800
_vrn_publ_code_frame_time_sec    30.0
_vrn_publ_code_meas_time_hour    17.8