Preparation of a potassium chloride bridged thorium phosphinidiide complex and its reactivity towards small organic molecules
Wang, Yongsong; Zhang, Congcong; Zi, Guofu; Ding, Wanjian; Walter, Marc D.; New Journal of Chemistry 43 (2019) 9527–; doi:10.1039/C9NJ02269D

data_7058440
_publ_section_title
;
 Preparation of a potassium chloride bridged thorium phosphinidiide
 complex and its reactivity towards small organic molecules
;
_journal_issue                   24
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9527
_journal_paper_doi               10.1039/C9NJ02269D
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C55 H81 P Th'
_chemical_formula_sum            'C55 H81 P Th'
_chemical_formula_weight         1005.20
_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   geom
_audit_creation_date             2018-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2019-03-21 deposited with the CCDC.    2019-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3699(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9426(2)
_cell_length_b                   23.0388(5)
_cell_length_c                   19.9010(4)
_cell_measurement_reflns_used    16998
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.1770
_cell_measurement_theta_min      4.4170
_cell_volume                     5017.02(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)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.987
_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   -108.00 -21.00   1.00    1.00    --  -41.49 -37.00 -90.00   87
  2  \w    -78.00 -17.00   1.00    1.00    --  -41.49 125.00-150.00   61
  3  \w      2.00  68.00   1.00    1.00    --   41.49 -99.00-180.00   66
  4  \w     57.00 103.00   1.00    1.00    --   41.49  37.00  90.00   46
  5  \w     77.00 103.00   1.00    1.00    --  107.19  77.00-120.00   26
  6  \w    117.00 169.00   1.00    1.00    --  107.19  77.00-120.00   52
  7  \w     35.00 128.00   1.00    1.00    --  107.19 -45.00  90.00   93
  8  \w     81.00 123.00   1.00    1.00    --  107.19  45.00 -90.00   42
  9  \w     27.00 107.00   1.00    1.00    --  107.19 -94.00 -30.00   80
 10  \w     26.00  68.00   1.00    1.00    --  107.19 -94.00 -60.00   42
 11  \w     70.00 177.00   1.00    1.00    --  107.19   0.00-180.00  107
 12  \w    -27.00  -2.00   1.00    1.00    --  -41.74 125.00  90.00   25
 13  \w    -73.00 -45.00   1.00    1.00    --  -41.74 125.00  90.00   28
 14  \w   -111.00 -19.00   1.00    1.00    --  -41.74 -37.00   0.00   92
 15  \w     16.00  42.00   1.00    1.00    --   41.74 -99.00-150.00   26
 16  \w     46.00  95.00   1.00    1.00    --   41.74-125.00   0.00   49
 17  \w     73.00 121.00   1.00    1.00    --  107.19-125.00-150.00   48
 18  \w     48.00  74.00   1.00    1.00    --  107.19 -77.00-180.00   26
 19  \w    117.00 174.00   1.00    1.00    --  107.19  45.00-150.00   57
 20  \w     77.00 105.00   1.00    1.00    --  107.19 -94.00  30.00   28
 21  \w     59.00 130.00   1.00    1.00    --  107.19 -45.00 -90.00   71
 22  \w     36.00  85.00   1.00    1.00    --  107.19 -94.00 120.00   49
 23  \w    126.00 166.00   1.00    1.00    --  107.19 125.00-180.00   40
 24  \w    112.00 138.00   1.00    1.00    --  107.19 -77.00-180.00   26
 25  \w     32.00 109.00   1.00    1.00    --  107.19 -94.00-120.00   77
;
_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      -0.0179630000
_diffrn_orient_matrix_UB_12      -0.0482079000
_diffrn_orient_matrix_UB_13      0.0526389000
_diffrn_orient_matrix_UB_21      0.1202375000
_diffrn_orient_matrix_UB_22      -0.0286656000
_diffrn_orient_matrix_UB_23      -0.0222557000
_diffrn_orient_matrix_UB_31      0.0708876000
_diffrn_orient_matrix_UB_32      0.0364240000
_diffrn_orient_matrix_UB_33      0.0522523000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37967
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.389
_diffrn_reflns_theta_min         3.837
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.116
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50075
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.960
_refine_diff_density_min         -2.763
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0639P)^2^+9.6666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8952
_reflns_number_total             9973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02269d2.cif
_cod_data_source_block           compound5a
_cod_depositor_comments
'Adding full bibliography for 7058431--7058443.cif.'
_cod_database_code               7058440
_chemical_oxdiff_formula         C1H1P1Th1
_reflns_odcompleteness_completeness 99.97
_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.a Ternary CH refined with riding coordinates:
 C35(H35), C47(H47), C50(H50), C53(H53)
2.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C15(H15), C17(H17), C18(H18), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34), C43(H43), C45(H45)
2.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), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              91306
_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 1.661
_oxdiff_exptl_absorpt_empirical_full_min 0.606