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_1548027
_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         'C33 H77 N4 P Si3 Th'
_chemical_formula_sum            'C33 H77 N4 P Si3 Th'
_chemical_formula_weight         877.26
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 113.726(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.6189(5)
_cell_length_b                   22.6046(7)
_cell_length_c                   22.2818(5)
_cell_measurement_reflns_used    18550
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.5440
_cell_measurement_theta_min      3.4990
_cell_volume                     8585.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_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      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     26.00  68.00   1.00   20.00    --   18.86  57.00   0.00   42
  2  \w     10.00  86.00   1.00   20.00    --   18.86  77.00  90.00   76
  3  \w     23.00  60.00   1.00   20.00    --   18.86 -99.00-150.00   37
  4  \w    -54.00  35.00   1.00   20.00    --   18.86 -37.00-180.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0062678000
_diffrn_orient_matrix_UB_12      -0.0297097000
_diffrn_orient_matrix_UB_13      0.0068916000
_diffrn_orient_matrix_UB_21      -0.0292671000
_diffrn_orient_matrix_UB_22      0.0095137000
_diffrn_orient_matrix_UB_23      0.0106236000
_diffrn_orient_matrix_UB_31      -0.0289520000
_diffrn_orient_matrix_UB_32      -0.0032227000
_diffrn_orient_matrix_UB_33      -0.0323874000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.1359
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            42874
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.211
_diffrn_reflns_theta_min         3.282
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.620
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
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    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.397
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.088
_refine_diff_density_max         3.620
_refine_diff_density_min         -2.373
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         19920
_refine_ls_number_restraints     1765
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0337P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12109
_reflns_number_total             19920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms12884-s3.cif
_cod_data_source_block           2
_cod_database_code               1548027
_chemical_oxdiff_formula         C33H77N4ThPSi3
_reflns_odcompleteness_completeness 99.73
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H1A-H1B = H2E-H2D
 2.245 with sigma of 0.02
 H1A-Th1 = Th1-H1B = H2E-Th2 = Th2-H2D
 3.79 with sigma of 0.01
 P1-H1B = P1-H1A = P2-H2E = P2-H2D
 1.43 with sigma of 0.02
 C24A-C23A \\sim C24-C23 \\sim C25A-C23A \\sim C25-C23 \\sim C27-C26 \\sim
C28-C26 \\sim C19-C18 \\sim C20-
 C18 \\sim C17-C15 \\sim C16-C15 \\sim C14-C12 \\sim C13-C12 \\sim C3-C1 \\sim
C2-C1 \\sim C5A-C4A \\sim C5-C4
 \\sim C6A-C4A \\sim C6-C4 \\sim C8-C7 \\sim C9-C7 \\sim C30-C29 \\sim C31-C29
\\sim C57-C56 \\sim C58-C56 ~
 C60-C59 \\sim C61-C59 \\sim C41-C40 \\sim C42-C40 \\sim C63-C62 \\sim C64-C62
\\sim C53-C51 \\sim C52-C51
 \\sim C50-C48 \\sim C49-C48 \\sim C47-C45 \\sim C46-C45 \\sim C36-C34 \\sim
C35-C34 \\sim C38-C37 \\sim C39-C37
 with sigma of 0.02
 C17-C16 \\sim C13-C14 \\sim C3-C2 \\sim C9-C8 \\sim C6A-C5A \\sim C5-C6 \\sim
C53-C52 \\sim C36-C35 \\sim C39-
 C38 \\sim C41-C42 \\sim C49-C50 \\sim C46-C47 \\sim C61-C60 \\sim C58-C57
\\sim C63-C64 \\sim C28-C27 ~
 C30-C31 \\sim C24A-C25A \\sim C24-C25 \\sim C19-C20
 with sigma of 0.01
3. 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
4. Others
 Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(H6AC)=1-FVAR(1)
 Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=FVAR(1)
 Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=Sof(H25C)=1-FVAR(2)
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25A)=
 Sof(H25D)=Sof(H25E)=Sof(H25F)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C7(H7), C12(H12), C15(H15), C18(H18), C26(H26), C29(H29), C4(H4),
 C23(H23), C4A(H4A), C23A(H23A), C34(H34), C37(H37), C40(H40), C45(H45),
 C48(H48), C51(H51), C56(H56), C59(H59), C62(H62)
5.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)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), 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), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C5(H5A,H5B,H5C), C6(H6A,H6B,
 H6C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C5A(H5AA,H5AB,H5AC), C6A(H6AA,
 H6AB,H6AC), C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F), 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)
;
_shelx_res_checksum              75793
_shelx_hkl_checksum              78236
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.089
_oxdiff_exptl_absorpt_empirical_full_min 0.502