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_7049928
_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 H98 N2 P2 Th'
_chemical_formula_sum            'C63 H98 N2 P2 Th'
_chemical_formula_weight         1177.41
_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             2018-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-25 deposited with the CCDC.    2019-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.5600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.52240(10)
_cell_length_b                   24.7325(2)
_cell_length_c                   20.3311(2)
_cell_measurement_reflns_used    13083
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.9540
_cell_measurement_theta_min      4.1510
_cell_volume                     6094.53(10)
_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 0.975
_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    -62.00  30.00   1.00    2.15    --  -41.49  37.00 150.00   92
  2  \w   -113.00 -18.00   1.00    2.15    --  -41.49 -37.00 -30.00   95
  3  \w    -27.00  -2.00   1.00    2.15    --  -41.49 125.00-150.00   25
  4  \w     37.00  75.00   1.00    2.15    --   41.49-125.00-180.00   38
  5  \w     76.00 103.00   1.00    3.00    --  104.69  61.00-180.00   27
  6  \w     84.00 176.00   1.00    3.00    --  104.69  45.00 120.00   92
  7  \w    100.00 132.00   1.00    3.00    --  104.69 125.00-180.00   32
  8  \w     30.00 134.00   1.00    3.00    --  104.69 -77.00  30.00  104
  9  \w     95.00 178.00   1.00    3.00    --  104.69 125.00  60.00   83
 10  \w     79.00 168.00   1.00    3.00    --  104.69  61.00 150.00   89
;
_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      -0.0036343000
_diffrn_orient_matrix_UB_12      -0.0034247000
_diffrn_orient_matrix_UB_13      0.0750623000
_diffrn_orient_matrix_UB_21      -0.0359001000
_diffrn_orient_matrix_UB_22      0.0596768000
_diffrn_orient_matrix_UB_23      -0.0021570000
_diffrn_orient_matrix_UB_31      -0.1218951000
_diffrn_orient_matrix_UB_32      -0.0174935000
_diffrn_orient_matrix_UB_33      -0.0221354000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24544
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.993
_diffrn_reflns_theta_min         4.062
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.653
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81294
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       prism
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.088
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         11679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10289
_reflns_number_total             11679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01160a2.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 7049925--7049929.cif.'
_cod_database_code               7049928
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1P1Th1
_shelx_estimated_absorpt_t_max   0.478
_shelx_estimated_absorpt_t_min   0.276
_reflns_odcompleteness_completeness 99.87
_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:
 C33(H33), C36(H36), C39(H39), C48(H48), C51(H51), C54(H54)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C15(H15), C17(H17), C18(H18), C29(H29), C31(H31),
 C44(H44), C46(H46), C57(H57), C58(H58), C60(H60), C61(H61)
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), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C55(H55A,
 H55B,H55C), C56(H56A,H56B,H56C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              94066
_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 1.625
_oxdiff_exptl_absorpt_empirical_full_min 0.833