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_1548031
_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         'C43 H98 N5 O Si3 Th, C24 H20 B, 2(C4 H8 O)'
_chemical_formula_sum            'C75 H134 B N5 O3 Si3 Th'
_chemical_formula_weight         1480.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 108.190(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4228(13)
_cell_length_b                   21.7375(13)
_cell_length_c                   20.5577(13)
_cell_measurement_reflns_used    8364
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.8680
_cell_measurement_theta_min      4.3640
_cell_volume                     7821.2(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1806
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
  1 omega  -69.00  -22.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000   60.0000 47

  2 omega  -49.00   17.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -60.0000 66

  3 omega  -43.00   31.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000    0.0000 74

  4 omega  -36.00   33.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -120.0000 69

  5 omega   32.00   86.00   1.0000  260.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000    0.0000 54

  6 omega   56.00   91.00   1.0000  260.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000 -150.0000 35

  7 omega   40.00  107.00   1.0000  260.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -95.0000 -120.0000 67

  8 omega  135.00  178.00   1.0000  260.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  125.0000   90.0000 43

  9 omega   96.00  169.00   1.0000  260.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  125.0000  -60.0000 73

 10 omega   32.00   87.00   1.0000  260.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000  -90.0000 55

 11 omega   52.00   89.00   1.0000  260.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000 -180.0000 37

 12 omega  120.00  149.00   1.0000  260.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   77.0000  -60.0000 29

 13 omega   39.00  151.00   1.0000  260.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -15.0000  -30.0000 112

 14 omega   16.00  113.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1277   57.0000  -30.0000 97

 15 omega    1.00   27.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1277  -99.0000   90.0000 26

 16 omega   12.00  117.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1277   77.0000 -150.0000 105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      -0.0518530000
_diffrn_orient_matrix_UB_12      -0.0029472000
_diffrn_orient_matrix_UB_13      0.0460208000
_diffrn_orient_matrix_UB_21      -0.0339010000
_diffrn_orient_matrix_UB_22      -0.0612409000
_diffrn_orient_matrix_UB_23      -0.0339496000
_diffrn_orient_matrix_UB_31      0.0623691000
_diffrn_orient_matrix_UB_32      -0.0355992000
_diffrn_orient_matrix_UB_33      0.0543806000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1812
_diffrn_reflns_av_unetI/netI     0.1910
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43946
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.965
_diffrn_reflns_theta_min         4.383
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.933
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       block
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.3219
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.0297
_refine_diff_density_max         3.834
_refine_diff_density_min         -3.188
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         15597
_refine_ls_number_restraints     221
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.0888
_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^)+(0.0648P)^2^+13.3083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1983
_refine_ls_wR_factor_ref         0.2472
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8954
_reflns_number_total             15597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms12884-s7.cif
_cod_data_source_block           SI-1
_cod_database_code               1548031
_chemical_oxdiff_formula         'C75 H134 N5 Th B Si3 O3'
_chemical_oxdiff_usercomment
'THEPWA #15096 SN-689 FOR EPW/STL ON MICROMOUNT IN FOMBLIN OIL'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 O2-C71 \\sim O2-C68
 with sigma of 0.02
 C71-C70 \\sim C69-C68
 with sigma of 0.02
 O2-C71 \\sim O2-C68
 with sigma of 0.02
 C71-C70 \\sim C69-C68
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C16, C17, C15, Si2, C20, C19, C18, C14, C13, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Si2, C17, C15, C16, C12, C14, C13, C18, C20, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Si1, Si3, C1, C2, C3, C6, C4, C5, C7, C9, C8, C23, C24, C25, C26, C27, C28,
 C29, C30, C31, O2, C68, C69, C70, C71
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C14(H14), C17(H17), C20(H20), C25(H25), C28(H28),
 C31(H31)
4.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), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C40(H40A,H40B), C42(H42A,H42B), C68(H68A,H68B),
  C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C1AA(H1AA,H1AB), C2AA(H2AA,
 H2AB), C4AA(H4AA,H4AB), C3AA(H3AA,H3AB)
4.c Aromatic/amide H refined with riding coordinates:
 C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C51(H51), C52(H52),
 C53(H53), C54(H54), C55(H55), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61),
  C63(H63), C64(H64), C65(H65), C66(H66), C67(H67)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C7(H7A,
 H7B,H7C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,
 H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C41(H41A,
 H41B,H41C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              54213
_shelx_hkl_checksum              9125
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'