Experimental and computational studies on a three-membered diphosphido thorium metallaheterocycle [η<sup>5</sup>-1,3-(Me<sub>3</sub>C)<sub>2</sub>C<sub>5</sub>H<sub>3</sub>]<sub>2</sub>Th[η<sup>2</sup>-P<sub>2</sub>(2,4,6-<sup>i</sup>Pr<sub>3</sub>C<sub>6</sub>H<sub>2</sub>)<sub>2</sub>].
Zhang, Congcong; Wang, Yongsong; Hou, Guohua; Ding, Wanjian; Zi, Guofu; Walter, Marc D.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6921–6930; doi:10.1039/c9dt01160a

data_7049926
_publ_section_title
;
 Experimental and computational studies on a three-membered diphosphido
 thorium metallaheterocycle
 [\h<sup>5</sup>-1,3-(Me<sub>3</sub>C)<sub>2</sub>C<sub>5</sub>H<sub>3</sub>]<sub>2</sub>Th[\h<sup>2</sup>-P<sub>2</sub>(2,4,6-<sup>i</sup>Pr<sub>3</sub>C<sub>6</sub>H<sub>2</sub>)<sub>2</sub>].
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6921
_journal_page_last               6930
_journal_paper_doi               10.1039/c9dt01160a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C56 H90 P2 Th'
_chemical_formula_sum            'C56 H90 P2 Th'
_chemical_formula_weight         1057.25
_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   mixed
_audit_creation_date             2016-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2019-02-25 deposited with the CCDC.    2019-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.268(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.3071(7)
_cell_length_b                   10.1096(3)
_cell_length_c                   22.2903(6)
_cell_measurement_reflns_used    7585
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.9360
_cell_measurement_theta_min      4.6990
_cell_volume                     5501.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.6a (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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_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    -45.00 -17.00   1.00    1.00    --  -41.49 -37.00 -60.00   28
  2  \w    -64.00  11.00   1.00    1.00    --  -41.49  19.00-120.00   75
  3  \w      3.00  28.00   1.00    1.00    --   41.49 -99.00 -90.00   25
  4  \w     33.00  66.00   1.00    3.00    --  107.19 -94.00  30.00   33
  5  \w     84.00 133.00   1.00    3.00    --  107.19 -30.00 120.00   49
  6  \w     88.00 115.00   1.00    3.00    --  107.19 -45.00 120.00   27
  7  \w     82.00 155.00   1.00    3.00    --  107.19  30.00  60.00   73
  8  \w    131.00 175.00   1.00    3.00    --  107.19  45.00 150.00   44
  9  \w     98.00 168.00   1.00    3.00    --  107.19 125.00  90.00   70
 10  \w     94.00 156.00   1.00    3.00    --  107.19 125.00 -30.00   62
 11  \w     81.00 178.00   1.00    3.00    --  107.19  45.00 -60.00   97
 12  \w     42.00  77.00   1.00    3.00    --  107.19 -45.00 120.00   35
 13  \w    -96.00  -2.00   1.00    1.00    --  -41.49 125.00 -90.00   94
 14  \w   -114.00 -75.00   1.00    1.00    --  -41.49 -37.00 -60.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0406440000
_diffrn_orient_matrix_UB_12      -0.0967959000
_diffrn_orient_matrix_UB_13      0.0415667000
_diffrn_orient_matrix_UB_21      -0.0440008000
_diffrn_orient_matrix_UB_22      -0.0400611000
_diffrn_orient_matrix_UB_23      0.0329116000
_diffrn_orient_matrix_UB_31      -0.0196561000
_diffrn_orient_matrix_UB_32      -0.1107494000
_diffrn_orient_matrix_UB_33      -0.0482374000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_unetI/netI     0.1020
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22837
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.280
_diffrn_reflns_theta_min         3.621
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.514
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.02610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         4.533
_refine_diff_density_min         -3.668
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         10736
_refine_ls_number_restraints     348
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0865
_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^)+(0.0650P)^2^+86.6636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1957
_refine_ls_wR_factor_ref         0.2091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8526
_reflns_number_total             10736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01160a2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7049925--7049929.cif.'
_cod_original_cell_volume        5501.5(3)
_cod_database_code               7049926
_chemical_oxdiff_formula         c1h1p1Th1
_reflns_odcompleteness_completeness 99.91
_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, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C38') \\sim Ueq,
Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq,
Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq,
Uanis(C53) \\sim Ueq, Uanis(C53') \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Others
 Sof(H36A)=Sof(C38')=Sof(H38D)=Sof(H38E)=Sof(H38F)=1-FVAR(1)
 Sof(H36)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(1)
 Sof(H51A)=Sof(C53')=Sof(H53D)=Sof(H53E)=Sof(H53F)=1-FVAR(2)
 Sof(H51)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=FVAR(2)
4.a Riding coordinates:
 P1(H1), P2(H2)
4.b Ternary CH refined with riding coordinates:
 C33(H33), C36(H36), C36(H36A), C39(H39), C48(H48), C51(H51), C51(H51A),
 C54(H54)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C4(H4), C5(H5), C15(H15), C17(H17), C18(H18), C29(H29), C31(H31),
 C44(H44), C46(H46)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C38'(H38D,H38E,H38F), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C), C53'(H53D,H53E,H53F), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              34558
_shelx_shelxl_version_number     2014/7
_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 13.396
_oxdiff_exptl_absorpt_empirical_full_min 0.391