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_1548030
_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 H150 N8 P Si6 Th2, C16 H32 Na O8, 0.5 (C4 H10 O2)'
_chemical_formula_sum            'C84 H187 N8 Na O9 P Si6 Th2'
_chemical_formula_weight         2139.98
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.615(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.1479(7)
_cell_length_b                   17.4133(5)
_cell_length_c                   26.4947(9)
_cell_measurement_reflns_used    23080
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0130
_cell_measurement_theta_min      3.5850
_cell_volume                     10379.4(6)
_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      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1636
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   16.00   71.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3799   19.0000  -90.0000 55

  2 omega   39.00  101.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3799  178.0000    0.0000 62

  3 omega  -67.00   34.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3799  -77.0000    0.0000 101

  4 omega  -12.00   84.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       11.3799   57.0000  120.0000 96

  5 omega  -79.00  -54.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.8486 -178.0000  -30.0000 25

  6 omega   36.00   68.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.8486 -178.0000  -30.0000 32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0261215000
_diffrn_orient_matrix_UB_12      0.0104367000
_diffrn_orient_matrix_UB_13      0.0187129000
_diffrn_orient_matrix_UB_21      0.0044607000
_diffrn_orient_matrix_UB_22      0.0311218000
_diffrn_orient_matrix_UB_23      -0.0159166000
_diffrn_orient_matrix_UB_31      -0.0170924000
_diffrn_orient_matrix_UB_32      0.0240954000
_diffrn_orient_matrix_UB_33      0.0124714000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_unetI/netI     0.1054
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            91450
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.682
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         3.374
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.003
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.619
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             4436
_exptl_crystal_size_max          0.2178
_exptl_crystal_size_mid          0.1416
_exptl_crystal_size_min          0.1077
_refine_diff_density_max         2.613
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1067
_refine_ls_number_reflns         19666
_refine_ls_number_restraints     963
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+34.9565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1271
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13798
_reflns_number_total             19666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms12884-s6.cif
_cod_data_source_block           6
_cod_database_code               1548030
_chemical_oxdiff_formula         'C66 H150 Th2 P Na N8 Si6'
_chemical_oxdiff_usercomment     ' '
_reflns_odcompleteness_completeness 99.72
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C1 \\sim C3A-C1A \\sim C2A-C1A \\sim C2-C1 \\sim C6-C4 \\sim C5-C4 \\sim
C8-C7 \\sim C9-C7 \\sim C27-C26 ~
 C28-C26 \\sim C24-C23 \\sim C25-C23 \\sim C31-C29 \\sim C30-C29 \\sim C36-C34
\\sim C35-C34 \\sim C38-C37
 \\sim C39-C37 \\sim C42-C40 \\sim C41-C40 \\sim C57-C56 \\sim C58-C56 \\sim
C60-C59 \\sim C61-C59 \\sim C53-
 C51 \\sim C52-C51 \\sim C49-C48 \\sim C50-C48 \\sim C46-C45 \\sim C47-C45
\\sim C13-C12 \\sim C14-C12 ~
 C20-C18 \\sim C19-C18
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C1A \\sim C2A \\sim C3A: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 Si1, C1, C2, C3, C1A, C2A, C3A, Na1, O1, O2, O3, O4, O5, O6, O7, O8, C67, C68,
  C69, C70, C71, C72, C73, C74, C75, C76, C77, C78, C79, C80, C81, C82
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(H3C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C4(H4), C7(H7), C12(H12), C15(H15), C18(H18), C23(H23), C26(H26), C29(H29),
 C34(H34), C37(H37), C40(H40), C45(H45), C48(H48), C51(H51), C56(H56), C59(H59),
  C62(H62), C1(H1), C1A(H1A)
6.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), C67(H67A,H67B), C68(H68A,H68B),
  C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,
 H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B),
 C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B),
  C84(H84A,H84B)
6.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), 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), C58(H58A,H58B,H58C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C64(H64A,H64B,
 H64C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,
 H3AC), C83(H83A,H83B,H83C)
;
_shelx_res_checksum              69165
_shelx_hkl_checksum              64878
_olex2_submission_special_instructions 'No special instructions were received'