Formation of a Bridging Phosphinidene Thorium Complex.
Behrle, Andrew C.; Castro, Ludovic; Maron, Laurent; Walensky, Justin R.; Journal of the American Chemical Society 137 (2015) 14846–14849; doi:10.1021/jacs.5b09826

data_4129714
_publ_section_title
;
 Formation of a Bridging Phosphinidene Thorium Complex.
;
_journal_issue                   47
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14846
_journal_page_last               14849
_journal_paper_doi               10.1021/jacs.5b09826
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C55 H81 P Th2'
_chemical_formula_weight         1237.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.300(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0279(16)
_cell_length_b                   18.200(3)
_cell_length_c                   25.124(4)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.78
_cell_measurement_theta_min      2.16
_cell_volume                     5028.4(14)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            56074
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.798
_diffrn_reflns_theta_min         1.383
_exptl_absorpt_coefficient_mu    5.973
_exptl_absorpt_correction_T_max  0.586
_exptl_absorpt_correction_T_min  0.374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

 Data were corrected for decay and absorption using the program SADABS
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 G\"ottingen, Germany).
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       needle
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         10714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+5.8482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9330
_reflns_number_total             10714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b09826_si_002.cif
_cod_data_source_block           compound(2)
_cod_original_cell_volume        5028.4(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4129714
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.276
_shelx_estimated_absorpt_t_max   0.586