White phosphorus activation by a Th(iii) complex.
Formanuik, Alasdair; Ortu, Fabrizio; Beekmeyer, Reece; Kerridge, Andrew; Adams, Ralph W.; Mills, David P.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2390–2393; doi:10.1039/c5dt04528b

data_7037880
_publ_section_title
;
 White phosphorus activation by a Th(iii) complex.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2390
_journal_page_last               2393
_journal_paper_doi               10.1039/c5dt04528b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C66 H120 P4 Si10.8 Th2, 1(C7 H8)'
_chemical_formula_sum            'C73 H128 P4 Si10.8 Th2'
_chemical_formula_weight         1896.98
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-19 deposited with the CCDC.
2016-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.10705(17)
_cell_length_b                   21.10705(17)
_cell_length_c                   21.10705(17)
_cell_measurement_reflns_used    11087
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      23.0300
_cell_measurement_theta_min      3.8400
_cell_volume                     9403.35(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.02(10)
_diffrn_detector_area_resol_mean 16.1428
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -68.00  -31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  115.0000 -101.0000 37

  2 omega  -86.00   19.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -19.0000 -120.0000 105

  3 omega  -87.00   -8.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -57.0000 -180.0000 79

  4 omega  -88.00   12.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -77.0000   60.0000 100
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0114474000
_diffrn_orient_matrix_UB_12      -0.0152622000
_diffrn_orient_matrix_UB_13      0.0276617000
_diffrn_orient_matrix_UB_21      -0.0085142000
_diffrn_orient_matrix_UB_22      0.0268642000
_diffrn_orient_matrix_UB_23      0.0183111000
_diffrn_orient_matrix_UB_31      -0.0304362000
_diffrn_orient_matrix_UB_32      -0.0132239000
_diffrn_orient_matrix_UB_33      0.0052924000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52308
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.336
_diffrn_reflns_theta_min         3.344
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.399
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.294
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       block
_exptl_crystal_F_000             3829
_exptl_crystal_size_max          0.4156
_exptl_crystal_size_mid          0.3631
_exptl_crystal_size_min          0.2902
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         2868
_refine_ls_number_restraints     431
_refine_ls_restrained_S_all      1.393
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1114P)^2^+24.2308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1685
_refine_ls_wR_factor_ref         0.1918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2024
_reflns_number_total             2868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04528b2.cif
_cod_data_source_block           adpm199
_cod_depositor_comments          'Adding full bibliography for 7037880.cif.'
_cod_original_cell_volume        9403.3(2)
_cod_original_formula_sum        'C73 H128 P4 Si10.80 Th2'
_cod_database_code               7037880
_manchester_internal_coll_name   adpm199
_manchester_internal_coll_client AF/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 10s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   AF
_manchester_internal_coll_date   05/07/2015
_manchester_internal_process_user AF
_manchester_internal_process_date 05/07/2015
_manchester_internal_solution_user AF
_manchester_internal_solution_date 05/07/2015
_manchester_internal_refinement_user AF/FO
_manchester_internal_refinement_date 18/08/2015
_manchester_internal_validation_user FO
_manchester_internal_validation_date 18/08/2015
_manchester_internal_archive_date 18/08/2015
_chemical_oxdiff_formula         Th2Si12C66P4
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C6A
 3.53 with sigma of 0.02
 C7A-C1
 3 with sigma of 0.02
 C1-C8A
 3 with sigma of 0.02
 C6A-C1
 3 with sigma of 0.02
 C14-C13
 1.5 with sigma of 0.02
 C14-C16
 1.4 with sigma of 0.02
 C18-C15
 1.5 with sigma of 0.02
 Si1-C6 \\sim Si1-C7 \\sim Si1-C8
 with sigma of 0.02
 C11-C10 \\sim C9-C11 \\sim C10-C11 \\sim C11A-C10A \\sim C10A-C9A \\sim
C9A-C11A \\sim C7-C8 \\sim C7-C6
 \\sim C8-C6
 with sigma of 0.02
 C5-C1 \\sim C4-C3
 with sigma of 0.02
 C3-C2 \\sim C2-C1
 with sigma of 0.02
 Si1A-C6A \\sim Si1-C6 \\sim Si1-C7 \\sim Si1A-C7A \\sim Si1A-C8A \\sim Si1-C8
 with sigma of 0.02
 C7-C8 \\sim C7-C6 \\sim C8-C7 \\sim C7A-C8A \\sim C7A-C6A \\sim C8A-C7A
 with sigma of 0.02
 Si1A-C1 \\sim Si1-C1
 with sigma of 0.02
 Si3A-C9 \\sim Si3A-C10 \\sim Si3A-C11 \\sim Si1A-C7A \\sim Si1-C8 \\sim
Si1A-C8A \\sim Si1-C6 \\sim Si1A-
 C6A \\sim Si1-C7 \\sim Si3A-C9A \\sim Si3A-C11 \\sim Si3A-C10A \\sim Si3A-C10
\\sim Si3A-C11A \\sim Si3A-C9
 with sigma of 0.02
 Si3A-C3 \\sim Si1A-C1 \\sim Si1-C1
 with sigma of 0.02
 C18-C16 \\sim C14-C18
 with sigma of 0.02
3. Restrained planarity
 C16, C15, C14, C13, C12, C17, C18
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq:
with sigma of 0.002 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C10)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C9)=Sof(H9C)=Sof(H9A)=Sof(H9B)=
 Sof(C11)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(Si3A)=1-FVAR(1)
 Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11A)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=Sof(C9A)=Sof(H9AC)=Sof(H9AA)=Sof(H9AB)=FVAR(1)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(Si1A)=1-FVAR(2)
 Sof(Si1)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=
 Sof(H8C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(2)
 Fixed Sof: P2(0.33333) C16(0.16662) H16(0.16662) C15(0.16662) C14(0.16662)
 H14(0.16662) C13(0.16662) H13(0.16662) C12(0.16662) H12(0.16662) C17(0.16662)
 H17(0.16662) C18(0.16666) H18A(0.16666) H18B(0.16666) H18C(0.16666)
7.a Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C10A(H10A,H10B,H10C),
 C11A(H11A,H11B,H11C), C9A(H9AC,H9AA,H9AB), C10(H10D,H10E,H10F), C9(H9C,H9A,
 H9B), C11(H11D,H11E,H11F), C8A(H8AA,H8AB,H8AC), C7A(H7AA,H7AB,H7AC), C6A(H6AA,
 H6AB,H6AC), C18(H18A,H18B,H18C)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C16(H16), C14(H14), C13(H13), C12(H12), C17(H17)
7.c Fitted hexagon refined as free rotating group:
 C16(C15,C14,C13,C12,C17)
;
_shelx_res_checksum              6909
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'