A base-free terminal thorium phosphinidene metallocene and its reactivity toward selected organic molecules.
Zhang, Congcong; Hou, Guohua; Zi, Guofu; Walter, Marc D.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2377–2387; doi:10.1039/c9dt00012g

data_7048793
_publ_section_title
;
 A base-free terminal thorium phosphinidene metallocene and its reactivity
 toward selected organic molecules.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2377
_journal_page_last               2387
_journal_paper_doi               10.1039/c9dt00012g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C67 H102 N P Th, C3 H7'
_chemical_formula_sum            'C70 H109 N P Th'
_chemical_formula_weight         1227.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-02-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-12-06 deposited with the CCDC.
2019-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                68.243(4)
_cell_angle_beta                 82.483(4)
_cell_angle_gamma                80.226(4)
_cell_formula_units_Z            2
_cell_length_a                   12.0224(5)
_cell_length_b                   14.9397(6)
_cell_length_c                   19.8170(8)
_cell_measurement_reflns_used    11403
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.0700
_cell_measurement_theta_min      4.4620
_cell_volume                     3248.8(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 0.999
_diffrn_measured_fraction_theta_max 0.970
_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   -109.00 -15.00   1.00    1.00    --  -41.49 -57.00 -30.00   94
  2  \w    -70.00  32.00   1.00    1.00    --  -41.49  57.00-150.00  102
  3  \w   -115.00 -27.00   1.00    1.00    --  -41.49 -37.00  60.00   88
  4  \w     13.00  63.00   1.00    1.00    --   41.49 -99.00 -90.00   50
  5  \w     35.00  93.00   1.00    1.00    --   41.49-125.00  60.00   58
  6  \w     81.00 178.00   1.00    1.00    --  107.19  45.00   0.00   97
  7  \w     35.00 135.00   1.00    1.00    --  107.19 -61.00  30.00  100
  8  \w     31.00 133.00   1.00    1.00    --  107.19 -77.00-180.00  102
  9  \w    146.00 178.00   1.00    1.00    --  107.19  45.00-180.00   32
 10  \w     82.00 121.00   1.00    1.00    --  107.19  45.00-180.00   39
 11  \w     40.00 134.00   1.00    1.00    --  107.19 -30.00-180.00   94
 12  \w     84.00 109.00   1.00    1.00    --  107.19 -94.00-180.00   25
 13  \w     35.00  88.00   1.00    1.00    --  107.19 -61.00 -30.00   53
 14  \w     78.00 117.00   1.00    1.00    --  107.19-125.00-180.00   39
 15  \w     81.00 178.00   1.00    1.00    --  107.19  30.00 120.00   97
 16  \w     50.00 119.00   1.00    1.00    --  107.19-125.00   0.00   69
 17  \w     73.00 109.00   1.00    1.00    --  107.19 -94.00  30.00   36
 18  \w     53.00  90.00   1.00    1.00    --  107.19   0.00 150.00   37
;
_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      0.0209367000
_diffrn_orient_matrix_UB_12      0.0581657000
_diffrn_orient_matrix_UB_13      0.0460446000
_diffrn_orient_matrix_UB_21      -0.1194265000
_diffrn_orient_matrix_UB_22      -0.0118268000
_diffrn_orient_matrix_UB_23      0.0384357000
_diffrn_orient_matrix_UB_31      0.0479459000
_diffrn_orient_matrix_UB_32      -0.0949847000
_diffrn_orient_matrix_UB_33      0.0587145000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23582
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.328
_diffrn_reflns_theta_min         3.741
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80534
_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    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             1282
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.224
_refine_diff_density_min         -2.256
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         12661
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0406P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11432
_reflns_number_total             12661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00012g2.cif
_cod_data_source_block           compound6
_cod_depositor_comments
'Adding full bibliography for 7048788--7048794.cif.'
_cod_database_code               7048793
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1P1Th1
_reflns_odcompleteness_completeness 99.92
_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. Restrained distances
 P1-H1
 1.1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C68(H68A,H68B), C69(H69A,H69B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22), C37(H37), C39(H39), C55(H55), C56(H56),
 C58(H58), C59(H59), C62(H62), C63(H63), C65(H65), C66(H66)
3.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), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C), C60(H60A,H60B,H60C), C67(H67A,H67B,H67C), C70(H70A,H70B,
 H70C)
;
_shelx_res_checksum              79544
_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 1.469
_oxdiff_exptl_absorpt_empirical_full_min 0.678