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_7049925
_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         'C70 H98 Cl2 O2 P2 Th, C3 H3'
_chemical_formula_sum            'C73 H101 Cl2 O2 P2 Th'
_chemical_formula_weight         1375.41
_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   geom
_audit_creation_date             2018-10-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-02-25 deposited with the CCDC.    2019-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                85.745(2)
_cell_angle_beta                 83.053(2)
_cell_angle_gamma                84.314(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5508(2)
_cell_length_b                   13.8153(3)
_cell_length_c                   21.1736(4)
_cell_measurement_reflns_used    18254
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.0010
_cell_measurement_theta_min      3.7220
_cell_volume                     3330.90(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(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 0.973
_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    -69.00  27.00   1.00    1.00    --  -41.49  57.00-150.00   96
  2  \w   -115.00 -19.00   1.00    1.00    --  -41.49 -57.00  60.00   96
  3  \w    -31.00  64.00   1.00    1.00    --   41.49 -37.00 -90.00   95
  4  \w     54.00  91.00   1.00    1.00    --   41.49-125.00   0.00   37
  5  \w     38.00  72.00   1.00    1.00    --   41.49-125.00  90.00   34
  6  \w     37.00  67.00   1.00    1.00    --  104.69-125.00-120.00   30
  7  \w     52.00 125.00   1.00    1.00    --  104.69  15.00 -90.00   73
  8  \w    106.00 173.00   1.00    1.00    --  104.69 125.00  30.00   67
  9  \w     37.00  63.00   1.00    1.00    --  104.69 -61.00 -90.00   26
 10  \w     84.00 109.00   1.00    1.00    --  104.69 -94.00 -30.00   25
 11  \w     81.00 128.00   1.00    1.00    --  104.69 -61.00 -90.00   47
 12  \w     79.00 152.00   1.00    1.00    --  104.69  45.00 150.00   73
 13  \w     35.00 109.00   1.00    1.00    --  104.69 -94.00  60.00   74
 14  \w     70.00 114.00   1.00    1.00    --  104.69-125.00-120.00   44
 15  \w     80.00 177.00   1.00    1.00    --  104.69  45.00  90.00   97
 16  \w     45.00  79.00   1.00    1.00    --  104.69-125.00 -90.00   34
 17  \w     40.00 126.00   1.00    1.00    --  104.69 -30.00 -90.00   86
 18  \w     60.00 118.00   1.00    1.00    --  104.69-125.00   0.00   58
 19  \w     40.00 133.00   1.00    1.00    --  104.69 -61.00  60.00   93
;
_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      0.0320889000
_diffrn_orient_matrix_UB_12      0.1061078000
_diffrn_orient_matrix_UB_13      -0.0098355000
_diffrn_orient_matrix_UB_21      -0.0877409000
_diffrn_orient_matrix_UB_22      0.0274748000
_diffrn_orient_matrix_UB_23      0.0580432000
_diffrn_orient_matrix_UB_31      0.0973392000
_diffrn_orient_matrix_UB_32      -0.0243794000
_diffrn_orient_matrix_UB_33      0.0439093000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24342
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.138
_diffrn_reflns_theta_min         3.737
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.735
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       block
_exptl_crystal_F_000             1418
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.385
_refine_diff_density_min         -1.536
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         12761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0303P)^2^+2.6753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12309
_reflns_number_total             12761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01160a2.cif
_cod_data_source_block           compound7
_cod_depositor_comments
'Adding full bibliography for 7049925--7049929.cif.'
_cod_database_code               7049925
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1O1Cl1P1Th1
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C27(H27), C40(H40), C43(H43), C46(H46), C55(H55), C58(H58), C61(H61), C64(H64)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C15(H15), C17(H17), C18(H18), C29(H29), C30(H30),
 C32(H32), C33(H33), C36(H36), C38(H38), C51(H51), C53(H53), C66(H66), C67(H67),
  C69(H69), C70(H70), C71(H71), C72(H72), C73(H73)
2.c 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), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,
 H62B,H62C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              2867
_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 1.445
_oxdiff_exptl_absorpt_empirical_full_min 0.775