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_7058435
_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         'C52 H79 P Si Th'
_chemical_formula_sum            'C52 H79 P Si Th'
_chemical_formula_weight         995.25
_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             2018-10-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-03-21 deposited with the CCDC.    2019-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.3700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.44450(10)
_cell_length_b                   16.9931(2)
_cell_length_c                   20.9732(2)
_cell_measurement_reflns_used    10642
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.9100
_cell_measurement_theta_min      4.0910
_cell_volume                     4939.32(9)
_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 0.979
_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    -34.00  -2.00   1.00    2.56    --  -41.49 125.00 120.00   32
  2  \w   -116.00 -23.00   1.00    2.56    --  -41.49 -37.00  30.00   93
  3  \w    -17.00  19.00   1.00    2.56    --  -41.49  37.00 -30.00   36
  4  \w    -93.00 -57.00   1.00    2.56    --  -41.49 125.00 120.00   36
  5  \w     55.00  81.00   1.00    2.56    --   41.49 -99.00 -90.00   26
  6  \w      1.00  34.00   1.00    2.56    --   41.49 -99.00 -90.00   33
  7  \w     22.00  88.00   1.00    3.00    --  104.69 -94.00  60.00   66
  8  \w     32.00  95.00   1.00    3.00    --  104.69 -45.00 -60.00   63
  9  \w     32.00 106.00   1.00    3.00    --  104.69 -94.00 -30.00   74
 10  \w    103.00 174.00   1.00    3.00    --  104.69  45.00-120.00   71
 11  \w    110.00 163.00   1.00    3.00    --  104.69  77.00  90.00   53
 12  \w     57.00 126.00   1.00    3.00    --  104.69 -45.00  30.00   69
 13  \w    104.00 172.00   1.00    3.00    --  104.69  61.00   0.00   68
;
_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      0.0020119000
_diffrn_orient_matrix_UB_12      0.0856071000
_diffrn_orient_matrix_UB_13      0.0245884000
_diffrn_orient_matrix_UB_21      -0.0842482000
_diffrn_orient_matrix_UB_22      0.0206397000
_diffrn_orient_matrix_UB_23      -0.0612564000
_diffrn_orient_matrix_UB_31      -0.0724710000
_diffrn_orient_matrix_UB_32      -0.0215952000
_diffrn_orient_matrix_UB_33      0.0387864000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21029
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.034
_diffrn_reflns_theta_min         3.404
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.493
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88563
_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    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         6.801
_refine_diff_density_min         -2.943
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         9510
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0689P)^2^+62.5112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8231
_reflns_number_total             9510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02269d2.cif
_cod_data_source_block           compound6b
_cod_depositor_comments
'Adding full bibliography for 7058431--7058443.cif.'
_cod_database_code               7058435
_shelx_shelxl_version_number     2014/7
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(P1) = Uanis(C42)
Uanis(C42) = Uanis(C43) = Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47) =
Uanis(C48) = Uanis(C49) = Uanis(C50) = Uanis(C51) = Uanis(C52)
Uanis(Si1) = Uanis(C49)
3. Others
 Sof(C24')=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25')=Sof(H25D)=Sof(H25E)=
 Sof(H25F)=Sof(C26')=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C33(H33), C36(H36), C39(H39)
4.b Me refined with riding coordinates:
 C20(H20A,H20B,H20C), C50(H50A,H50B,H50C)
4.c 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), C45(H45), C46(H46), C47(H47), C48(H48)
4.d Fitted hexagon refined as free rotating group:
 C43(C44,C45,C46,C47,C48)
4.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), 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), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C24'(H24D,H24E,H24F), C25'(H25D,H25E,H25F), C26'(H26D,H26E,H26F)
;
_shelx_res_checksum              6934
_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 1.186
_oxdiff_exptl_absorpt_empirical_full_min 0.860