Thorium-phosphorus triamidoamine complexes containing Th-P single- and multiple-bond interactions
Elizabeth P. Wildman; Gabor Balazs; Ashley J. Wooles; Manfred Scheer; Stephen T. Liddle; Nature Communications 7 (2016) 12884–; doi:10.1038/ncomms12884

data_1548029
_publ_section_title
;
 Thorium-phosphorus triamidoamine complexes containing Th-P single- and
 multiple-bond interactions
;
_journal_name_full               'Nature Communications'
_journal_page_first              12884
_journal_paper_doi               10.1038/ncomms12884
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C66 H151 N8 P Si6 Th2, 2(C7 H8)'
_chemical_formula_sum            'C80 H167 N8 P Si6 Th2'
_chemical_formula_weight         1904.80
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                96.043(2)
_cell_angle_beta                 91.075(2)
_cell_angle_gamma                98.324(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8618(4)
_cell_length_b                   15.2608(5)
_cell_length_c                   22.2411(6)
_cell_measurement_reflns_used    12140
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1720
_cell_measurement_theta_min      3.9000
_cell_volume                     4626.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1636
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.813
_diffrn_measurement_details
;
  1 omega   35.00  101.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3799  178.0000 -120.0000 66

  2 omega  -85.00   15.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.8486  -57.0000 -120.0000 100

  3 omega  -41.00   55.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.8486   57.0000   30.0000 96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0107706000
_diffrn_orient_matrix_UB_12      -0.0431742000
_diffrn_orient_matrix_UB_13      -0.0159928000
_diffrn_orient_matrix_UB_21      0.0192655000
_diffrn_orient_matrix_UB_22      -0.0184466000
_diffrn_orient_matrix_UB_23      0.0247754000
_diffrn_orient_matrix_UB_31      -0.0468015000
_diffrn_orient_matrix_UB_32      -0.0053686000
_diffrn_orient_matrix_UB_33      0.0126531000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.813
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34570
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.813
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.530
_diffrn_reflns_theta_min         3.345
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.348
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       plate
_exptl_crystal_F_000             1964
_exptl_crystal_size_max          0.2554
_exptl_crystal_size_mid          0.1324
_exptl_crystal_size_min          0.0486
_refine_diff_density_max         1.828
_refine_diff_density_min         -1.670
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1090
_refine_ls_number_reflns         21036
_refine_ls_number_restraints     2702
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+10.1006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                16150
_reflns_number_total             21036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms12884-s5.cif
_cod_data_source_block           5
_cod_database_code               1548029
_chemical_oxdiff_formula         Th2C66H151N8Si6P
_chemical_oxdiff_usercomment     'ostl5 for THEW2'
_reflns_odcompleteness_completeness 98.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C70A-C69A = C68A-C69A = C73A-C68A = C72A-C73A = C71A-C72A = C70A-C71A
 1.39 with sigma of 0.01
 C70-C69 = C71-C72 = C71-C70 = C71A-C72A = C72A-C73A = C73A-C68A = C70A-C69A =
 C70A-C71A = C73-C72 = C73-C68 = C68-C69 = C77A-C76A = C77A-C78A = C76-C77 =
 C78A-C79A = C78-C77 = C79-C78 = C80A-C79A = C75A-C76A = C76-C75 = C80-C75 =
 C79-C80 = C75A-C80A
 1.39 with sigma of 0.01
 C74-C75 = C75A-C74A = C68-C67 = C67A-C68A
 1.55 with sigma of 0.01
 P1-H1
 1.43 with sigma of 0.001
 C69-C67 \\sim C67-C73 \\sim C80-C74 \\sim C74-C76
 with sigma of 0.02
 C73A-C70A \\sim C69A-C72A \\sim C73-C70 \\sim C69-C72 \\sim C76A-C79A \\sim
C77A-C80A \\sim C76-C79 ~
 C77-C80
 with sigma of 0.02
 C68-C71 \\sim C68A-C71A \\sim C75A-C78A \\sim C75-C78 \\sim C69A-C67A \\sim
C67A-C73A \\sim C80A-C74A
 \\sim C74A-C76A
 with sigma of 0.02
 Si3-C26 \\sim Si3-C29 \\sim Si3-C23 \\sim Si1-C1 \\sim Si1-C7 \\sim Si1-C4
\\sim Si2-C12A \\sim Si2-C12 ~
 Si2-C15A \\sim Si2-C15 \\sim Si2-C18A \\sim Si2-C18 \\sim Si4-C40 \\sim
Si4-C34 \\sim Si5-C51 \\sim Si4-
 C37 \\sim Si5-C45 \\sim Si5-C48 \\sim Si6A-C59A \\sim Si6-C56 \\sim Si6A-C56A
\\sim Si6-C59 \\sim Si6A-
 C62A \\sim Si6-C62
 with sigma of 0.02
 C41-C40 \\sim C40-C42 \\sim C36-C34 \\sim C34-C35 \\sim C38-C37 \\sim C39-C37
\\sim C6-C4 \\sim C5-C4 ~
 C3-C1 \\sim C2-C1 \\sim C8-C7 \\sim C7-C9 \\sim C30-C29 \\sim C31-C29 \\sim
C25-C23 \\sim C24-C23 \\sim C28-
 C26 \\sim C26-C27 \\sim C13A-C12A \\sim C14A-C12A \\sim C12-C13 \\sim C14-C12
\\sim C18-C20 \\sim C19-C18
 \\sim C19A-C18A \\sim C20A-C18A \\sim C15A-C16A \\sim C16-C15 \\sim C15A-C17A
\\sim C15-C17 \\sim C52-C51
 \\sim C53-C51 \\sim C48-C49 \\sim C50-C48 \\sim C47-C45 \\sim C46-C45 \\sim
C57A-C56A \\sim C58-C56 \\sim C57-
 C56 \\sim C58A-C56A \\sim C64-C62 \\sim C62A-C64A \\sim C63-C62 \\sim
C63A-C62A \\sim C60-C59 \\sim C60A-
 C59A \\sim C61-C59 \\sim C61A-C59A
 with sigma of 0.02
 H1-Th1 \\sim H1-Th2
 with sigma of 0.02
3. Restrained planarity
 C73, C67, C69, C68, C71, C72, C70
 with sigma of 0.1
 C67A, C68A, C69A, C70A, C71A, C72A, C73A
 with sigma of 0.1
 C74, C75, C76, C77, C78, C79, C80
 with sigma of 0.1
 C74A, C75A, C76A, C77A, C78A, C79A, C80A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C73 \\sim C67 \\sim C67A \\sim C68A \\sim C69 \\sim C68 \\sim C69A \\sim C70A
\\sim C71 \\sim C71A \\sim C72 \\sim C72A \\sim C70 \\sim C73A \\sim C74 \\sim
C74A \\sim C75 \\sim C75A \\sim C76 \\sim C76A \\sim C77 \\sim C77A \\sim C78
\\sim C78A \\sim C79 \\sim C79A \\sim C80 \\sim C80A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Si2 \\sim C12 \\sim C12A \\sim C13 \\sim C13A \\sim C14 \\sim C14A \\sim C15
\\sim C15A \\sim C16 \\sim C16A \\sim C17 \\sim C17A \\sim C18 \\sim C18A \\sim
C19 \\sim C19A \\sim C20 \\sim C20A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
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(Si6A)=Sof(C56A)=Sof(H56A)=Sof(C57A)=Sof(H57D)=Sof(H57E)=Sof(H57F)=
 Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=Sof(C59A)=Sof(H59A)=Sof(C60A)=
 Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(C61A)=Sof(H61D)=Sof(H61E)=Sof(H61F)=
 Sof(C62A)=Sof(H62A)=Sof(C63A)=Sof(H63D)=Sof(H63E)=Sof(H63F)=Sof(C64A)=
 Sof(H64D)=Sof(H64E)=Sof(H64F)=1-FVAR(1)
 Sof(Si6)=Sof(C56)=Sof(H56)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C58)=
 Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C59)=Sof(H59)=Sof(C60)=Sof(H60A)=Sof(H60B)=
 Sof(H60C)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C62)=Sof(H62)=Sof(C63)=
 Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=FVAR(1)
 Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=
 Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=
 Sof(H18A)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20A)=Sof(H20D)=
 Sof(H20E)=Sof(H20F)=1-FVAR(2)
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=
 Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19A)=
 Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(2)
 Sof(C74A)=Sof(H74D)=Sof(H74E)=Sof(H74F)=Sof(C75A)=Sof(C76A)=Sof(H76A)=
 Sof(C77A)=Sof(H77A)=Sof(C78A)=Sof(H78A)=Sof(C79A)=Sof(H79A)=Sof(C80A)=
 Sof(H80A)=1-FVAR(3)
 Sof(C74)=Sof(H74B)=Sof(H74A)=Sof(H74C)=Sof(C75)=Sof(C76)=Sof(H76)=Sof(C77)=
 Sof(H77)=Sof(C78)=Sof(H78)=Sof(C79)=Sof(H79)=Sof(C80)=Sof(H80)=FVAR(3)
 Sof(C67A)=Sof(H67D)=Sof(H67E)=Sof(H67F)=Sof(C68A)=Sof(C69A)=Sof(H69A)=
 Sof(C70A)=Sof(H70A)=Sof(C71A)=Sof(H71A)=Sof(C72A)=Sof(H72A)=Sof(C73A)=
 Sof(H73A)=1-FVAR(4)
 Sof(C73)=Sof(H73)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C69)=Sof(H69)=
 Sof(C68)=Sof(C71)=Sof(H71)=Sof(C72)=Sof(H72)=Sof(C70)=Sof(H70)=FVAR(4)
7.a Ternary CH refined with riding coordinates:
 C1(H1A), C4(H4), C7(H7), C12(H12), C12A(H12A), C15(H15), C15A(H15A), C18(H18),
  C18A(H18A), C23(H23), C26(H26), C29(H29), C34(H34), C37(H37), C40(H40),
 C45(H45), C48(H48), C51(H51), C56(H56), C56A(H56A), C59(H59), C59A(H59A),
 C62(H62), C62A(H62A)
7.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C21(H21A,H21B), C22(H22A,H22B), C32(H32A,
 H32B), C33(H33A,H33B), C43(H43A,H43B), C44(H44A,H44B), C54(H54A,H54B),
 C55(H55A,H55B), C65(H65A,H65B), C66(H66A,H66B)
7.c Aromatic/amide H refined with riding coordinates:
 C73(H73), C69(H69), C69A(H69A), C70A(H70A), C71(H71), C71A(H71A), C72(H72),
 C72A(H72A), C70(H70), C73A(H73A), C76(H76), C76A(H76A), C77(H77), C77A(H77A),
 C78(H78), C78A(H78A), C79(H79), C79A(H79A), C80(H80), C80A(H80A)
7.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C13A(H13D,H13E,H13F), C14(H14A,
 H14B,H14C), C14A(H14D,H14E,H14F), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F),
 C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F), C19(H19A,H19B,H19C), C19A(H19D,H19E,
 H19F), C20(H20A,H20B,H20C), C20A(H20D,H20E,H20F), C24(H24A,H24B,H24C),
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C57(H57A,H57B,H57C),
 C57A(H57D,H57E,H57F), C58(H58A,H58B,H58C), C58A(H58D,H58E,H58F), C60(H60A,H60B,
 H60C), C60A(H60D,H60E,H60F), C61(H61A,H61B,H61C), C61A(H61D,H61E,H61F),
 C63(H63A,H63B,H63C), C63A(H63D,H63E,H63F), C64(H64A,H64B,H64C), C64A(H64D,H64E,
 H64F), C67(H67A,H67B,H67C), C67A(H67D,H67E,H67F), C74(H74B,H74A,H74C),
 C74A(H74D,H74E,H74F)
;
_shelx_res_checksum              7897
_shelx_hkl_checksum              14386
_olex2_exptl_crystal_mounting_method 'on micromount in fomblin film.'
_olex2_submission_special_instructions 'No special instructions were received'