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_7058433
_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_absolute_configuration ad
_chemical_formula_moiety         'C51 H83 P Si2 Th'
_chemical_formula_sum            'C51 H83 P Si2 Th'
_chemical_formula_weight         1015.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-11-07
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4933(3)
_cell_length_b                   20.1773(5)
_cell_length_c                   24.5352(7)
_cell_measurement_reflns_used    11069
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.2530
_cell_measurement_theta_min      3.6760
_cell_volume                     5194.8(2)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.905
_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      1.00  27.00   1.00   10.00    --  -11.20 -99.00 120.00   26
  2  \w     23.00  49.00   1.00   10.00    --   12.45 -99.00-180.00   26
  3  \w    -11.00  86.00   1.00   10.00    --   12.45  37.00-150.00   97
  4  \w     56.00  88.00   1.00   10.00    --   12.45  19.00 120.00   32
  5  \w     -9.00  71.00   1.00   10.00    --   12.45  37.00 -60.00   80
;
_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      -0.0671247000
_diffrn_orient_matrix_UB_12      0.0030335000
_diffrn_orient_matrix_UB_13      -0.0022379000
_diffrn_orient_matrix_UB_21      -0.0065633000
_diffrn_orient_matrix_UB_22      -0.0089722000
_diffrn_orient_matrix_UB_23      0.0278156000
_diffrn_orient_matrix_UB_31      0.0042449000
_diffrn_orient_matrix_UB_32      0.0338639000
_diffrn_orient_matrix_UB_33      0.0075463000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35914
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.836
_diffrn_reflns_theta_min         3.207
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.977
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86010
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Flack x determined using 4362 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         12714
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0072P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0526
_reflns_Friedel_coverage         0.715
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.786
_reflns_number_gt                11608
_reflns_number_total             12714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02269d2.cif
_cod_data_source_block           compound8
_cod_depositor_comments
'Adding full bibliography for 7058431--7058443.cif.'
_cod_database_code               7058433
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1P1Si1Th1
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C34')
\\sim Ueq, Uanis(C35') \\sim Ueq, Uanis(C36') \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C34) = Uanis(C34')
Uanis(C35) = Uanis(C35')
Uanis(C36) = Uanis(C36')
3. Others
 Sof(C34')=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35')=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=Sof(C36')=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C43(H43), C46(H46), C49(H49)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C15(H15), C17(H17), C18(H18), C39(H39), C41(H41)
4.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), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C34'(H34D,H34E,
 H34F), C35'(H35D,H35E,H35F), C36'(H36D,H36E,H36F), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              80679
_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 1.322
_oxdiff_exptl_absorpt_empirical_full_min 0.811