Uranium and thorium complexes of the phosphaethynolate ion
Camp, Clément; Settineri, Nicholas; Lefèvre, Julia; Jupp, Andrew R.; Goicoechea, José M.; Maron, Laurent; Arnold, John; Chem. Sci. 6 (2015) 6379–; doi:10.1039/C5SC02150B

data_1529203
_publ_section_title
;
 Uranium and thorium complexes of the phosphaethynolate ion
;
_journal_issue                   11
_journal_name_full               'Chem. Sci.'
_journal_page_first              6379
_journal_paper_doi               10.1039/C5SC02150B
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C43.5 H73 N6 O P Si6 U'
_chemical_formula_weight         1133.61
_chemical_name_common            '[U(OCP)(amid)3].[0.5toluene]'
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-06-14 deposited with the CCDC.
2015-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                86.747(5)
_cell_angle_beta                 83.810(5)
_cell_angle_gamma                75.030(5)
_cell_formula_units_Z            2
_cell_length_a                   11.5703(12)
_cell_length_b                   11.7055(13)
_cell_length_c                   21.152(2)
_cell_measurement_reflns_used    9497
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.33
_cell_volume                     2750.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67609
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.384
_diffrn_reflns_theta_min         1.802
_exptl_absorpt_coefficient_mu    3.146
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             1150
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.600
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.865
_refine_diff_density_min         -2.201
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.371
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         10048
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.369
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+10.2716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9841
_reflns_number_total             10048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02150b2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1529203--1529209.cif.'
_cod_original_formula_sum        'C43.50 H73 N6 O P Si6 U'
_cod_database_code               1529203
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.187
_shelx_estimated_absorpt_t_max   0.572
_shelx_res_checksum              78653