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_1529209
_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            'C52.5 H91.5 N6 Ni O P Si6 Th'
_chemical_formula_weight         1313.07
_chemical_name_common            '[(amid)3Th(OCP)Ni(COD)].(hexane)0.75'
_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                105.8698(27)
_cell_angle_beta                 101.3208(26)
_cell_angle_gamma                96.5472(27)
_cell_formula_units_Z            4
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_cell_length_b                   19.6824(13)
_cell_length_c                   24.2681(17)
_cell_measurement_reflns_used    9658
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.43
_cell_volume                     6587.8(8)
_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-92
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.986
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
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_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            171492
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.395
_diffrn_reflns_theta_min         0.898
_exptl_absorpt_coefficient_mu    2.711
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             2694
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_exptl_crystal_size_mid          0.600
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_refine_diff_density_min         -3.064
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+32.7108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21437
_reflns_number_total             23909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02150b2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 1529203--1529209.cif.'
_cod_original_formula_sum        'C52.50 H91.50 N6 Ni O P Si6 Th'
_cod_database_code               1529209
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.293
_shelx_estimated_absorpt_t_max   0.293
_shelx_res_checksum              19907
_shelx_fab_checksum              94177