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_7058442
_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         'C96 H140 Cl2 K2 N2 P2 Th2'
_chemical_formula_sum            'C96 H140 Cl2 K2 N2 P2 Th2'
_chemical_formula_weight         1997.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-25 deposited with the CCDC.    2019-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.277(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8824(6)
_cell_length_b                   11.6832(3)
_cell_length_c                   32.2158(7)
_cell_measurement_reflns_used    5234
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.1420
_cell_measurement_theta_min      4.1690
_cell_volume                     9357.9(4)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.966
_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    -66.00  17.00   1.00    5.00    --  -41.49  37.00  60.00   83
  2  \w   -115.00 -17.00   1.00    5.00    --  -41.49 -37.00-120.00   98
  3  \w    -43.00  -5.00   1.00    5.00    --  -41.49 125.00 120.00   38
  4  \w     69.00 106.00   1.00    5.00    --   41.49 165.00-134.00   37
  5  \w     26.00  65.00   1.00   10.00    --  107.19 -15.00  60.00   39
  6  \w     84.00 139.00   1.00   10.00    --  107.19 -15.00  60.00   55
  7  \w     36.00  95.00   1.00   10.00    --  107.19 -61.00 -60.00   59
  8  \w    103.00 170.00   1.00   10.00    --  107.19  45.00-120.00   67
  9  \w     35.00 128.00   1.00   10.00    --  107.19 -30.00-150.00   93
 10  \w    137.00 177.00   1.00   10.00    --  107.19  61.00 150.00   40
 11  \w     82.00 126.00   1.00   10.00    --  107.19  61.00 150.00   44
;
_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      0.0235553000
_diffrn_orient_matrix_UB_12      0.0521708000
_diffrn_orient_matrix_UB_13      -0.0392389000
_diffrn_orient_matrix_UB_21      -0.0485743000
_diffrn_orient_matrix_UB_22      -0.0450468000
_diffrn_orient_matrix_UB_23      -0.0262913000
_diffrn_orient_matrix_UB_31      -0.0304012000
_diffrn_orient_matrix_UB_32      0.1124312000
_diffrn_orient_matrix_UB_33      0.0077058000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            17598
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.294
_diffrn_reflns_theta_min         4.181
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.144
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92851
_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    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.176
_refine_diff_density_min         -2.378
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0360P)^2^+15.4731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7259
_reflns_number_total             9078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02269d2.cif
_cod_data_source_block           compound11
_cod_depositor_comments
'Adding full bibliography for 7058431--7058443.cif.'
_cod_database_code               7058442
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1P1Th1
_reflns_odcompleteness_completeness 99.77
_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:
 C40(H40), C43(H43), C46(H46)
2.b Aromatic/amide H refined with riding coordinates:
 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)
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), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              34641
_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 1.338
_oxdiff_exptl_absorpt_empirical_full_min 0.806