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_7048792
_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         '2(C23 H34 P Th0.5)'
_chemical_formula_sum            'C46 H68 P2 Th'
_chemical_formula_weight         914.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-12-06 deposited with the CCDC.
2019-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.863(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3422(4)
_cell_length_b                   19.3149(5)
_cell_length_c                   21.2672(6)
_cell_measurement_reflns_used    9193
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.2080
_cell_measurement_theta_min      3.7670
_cell_volume                     4141.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.870
_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    -18.00  10.00   1.00   15.00    --   12.45 -37.00 -30.00   28
  2  \w    -20.00  11.00   1.00   15.00    --  -11.20 -99.00   0.00   31
  3  \w     39.00  92.00   1.00   15.00    --   12.45-178.00  30.00   53
  4  \w    -10.00  27.00   1.00   15.00    --  -11.20 -99.00-180.00   37
  5  \w     13.00  75.00   1.00   15.00    --   12.45  37.00-150.00   62
  6  \w     73.00  99.00   1.00   15.00    --   12.45 178.00-180.00   26
  7  \w    -68.00  52.00   1.00   15.00    --   12.45 -19.00  30.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0462126000
_diffrn_orient_matrix_UB_12      0.0057687000
_diffrn_orient_matrix_UB_13      -0.0295833000
_diffrn_orient_matrix_UB_21      0.0442135000
_diffrn_orient_matrix_UB_22      0.0240857000
_diffrn_orient_matrix_UB_23      -0.0092371000
_diffrn_orient_matrix_UB_31      0.0292791000
_diffrn_orient_matrix_UB_32      -0.0271275000
_diffrn_orient_matrix_UB_33      -0.0144703000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38778
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.827
_diffrn_reflns_theta_min         3.290
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41k (Rigaku Oxford Diffraction, 2015)
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    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.599
_refine_diff_density_min         -2.806
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         10352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0056P)^2^+12.0397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7162
_reflns_number_total             10352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00012g2.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 7048788--7048794.cif.'
_cod_database_code               7048792
_chemical_oxdiff_formula         C1H1P1Th1
_reflns_odcompleteness_completeness 99.71
_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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26),
 C28(H28), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
2.b 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), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              99708
_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 1.674
_oxdiff_exptl_absorpt_empirical_full_min 0.657