Cationic Thorium Alkyl Complexes of Rigid NON- and NNN-Donor Ligands: π-Arene Coordination as a Persistent Structural Motif
Cruz, Carlos A.; Emslie, David J. H.; Robertson, Craig M.; Harrington, Laura E.; Jenkins, Hilary A.; Britten, James F.; Organometallics 28 (2009) 1891–; doi:10.1021/om800624t

data_4068291
_publ_section_title
;
 Cationic Thorium Alkyl Complexes of Rigid NON- and NNN-Donor Ligands:
 \p-Arene Coordination as a Persistent Structural Motif
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1891
_journal_paper_doi               10.1021/om800624t
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C54 H69 N2 O Th, C24 B F20, C7 H8'
_chemical_formula_sum            'C99 H93 B F20 N2 O Th'
_chemical_formula_weight         1921.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 121.8730(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   47.788(3)
_cell_length_b                   15.0800(8)
_cell_length_c                   27.0268(15)
_cell_measurement_reflns_used    3378
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.73
_cell_measurement_theta_min      2.46
_cell_volume                     16540.0(17)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -62
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            89440
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    1.900
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Face correction'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             7744
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.05
_platon_squeeze_details          ' ?'
_refine_diff_density_max         2.097
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         19101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                13734
_reflns_number_total             19101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800624t_si_004.cif
_cod_data_source_block           cruz27q
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        16540.0(16)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4068291