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_7049929
_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         'C63 H93 N P2 Th, C6 H6, 0.5(C6 H14)'
_chemical_formula_sum            'C72 H106 N P2 Th'
_chemical_formula_weight         1279.55
_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
_audit_creation_date             2018-08-16
_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                90
_cell_angle_beta                 102.5700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9693(3)
_cell_length_b                   18.0772(2)
_cell_length_c                   18.9897(3)
_cell_measurement_reflns_used    15394
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.1220
_cell_measurement_theta_min      4.5260
_cell_volume                     6690.76(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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      100.00(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 0.976
_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    -47.00  33.00   1.00    1.00    --  -41.49  37.00  90.00   80
  2  \w     25.00  93.00   1.00    1.00    --   41.49-125.00-150.00   68
  3  \w     73.00 108.00   1.00    1.00    --   41.49  37.00-180.00   35
  4  \w     24.00  91.00   1.00    1.00    --   41.49-125.00  60.00   67
  5  \w     81.00 150.00   1.00    1.00    --  107.19  45.00-150.00   69
  6  \w     34.00 140.00   1.00    1.00    --  107.19 -77.00-150.00  106
  7  \w     97.00 135.00   1.00    1.00    --  107.19 -61.00 -30.00   38
  8  \w     35.00 107.00   1.00    1.00    --  107.19 -94.00 120.00   72
  9  \w     34.00 115.00   1.00    1.00    --  107.19-125.00  90.00   81
 10  \w     89.00 169.00   1.00    1.00    --  107.19  45.00 -30.00   80
 11  \w     93.00 118.00   1.00    1.00    --  107.19  45.00   0.00   25
;
_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      0.0735065000
_diffrn_orient_matrix_UB_12      0.0031887000
_diffrn_orient_matrix_UB_13      -0.0128445000
_diffrn_orient_matrix_UB_21      -0.0141855000
_diffrn_orient_matrix_UB_22      0.0779958000
_diffrn_orient_matrix_UB_23      -0.0324830000
_diffrn_orient_matrix_UB_31      0.0253750000
_diffrn_orient_matrix_UB_32      0.0342857000
_diffrn_orient_matrix_UB_33      0.0753765000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27849
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.227
_diffrn_reflns_theta_min         3.802
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             2660
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.453
_refine_diff_density_min         -1.804
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         13109
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+11.6778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11539
_reflns_number_total             13109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01160a2.cif
_cod_data_source_block           compound6
_cod_depositor_comments
'Adding full bibliography for 7049925--7049929.cif.'
_cod_database_code               7049929
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1P1Th1
_reflns_odcompleteness_completeness 99.88
_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
 C64-C69
 1.39 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C40(H40), C43(H43), C46(H46), C55(H55), C58(H58), C61(H61)
3.b Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C72(H72A,H72B)
3.c Aromatic/amide H refined with riding coordinates:
 C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C2(H2), C4(H4),
 C5(H5), C15(H15), C17(H17), C18(H18), C29(H29), C30(H30), C31(H31), C32(H32),
 C33(H33), C36(H36), C38(H38), C51(H51), C53(H53)
3.d Fitted hexagon refined as free rotating group:
 C64(C65,C66,C67,C68,C69)
3.e 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), C70(H70A,H70B,H70C)
;
_shelx_res_checksum              38380
_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 1.422
_oxdiff_exptl_absorpt_empirical_full_min 0.763