Structural Diversity in Cyanido Thorocene Complexes
Hervé, Alexandre; Thuéry, Pierre; Ephritikhine, Michel; Berthet, Jean-Claude; Organometallics 33 (2014) 2088–; doi:10.1021/om500252v

data_4083047
_publ_section_title
;
 Structural Diversity in Cyanido Thorocene Complexes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2088
_journal_paper_doi               10.1021/om500252v
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C87 H125 N5 Th3'
_chemical_formula_weight         1937.04
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.045(2)
_cell_angle_beta                 92.420(3)
_cell_angle_gamma                96.205(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2097(4)
_cell_length_b                   12.4122(5)
_cell_length_c                   26.7910(12)
_cell_measurement_reflns_used    223527
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.11
_cell_volume                     3999.6(3)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two \f and thirteen \w scans with 2\% steps (743 frames)'
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            223527
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.609
_exptl_absorpt_correction_T_max  0.540
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent dark yellow'
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.212
_refine_diff_density_min         -1.731
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     864
_refine_ls_number_reflns         24440
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0254P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0594
_reflns_number_gt                18464
_reflns_number_total             24440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500252v_si_003.cif
_cod_data_source_block           3(NBu4)2.py
_cod_depositor_comments
'Adding full bibliography for 4083046--4083050.cif.'
_cod_database_code               4083047