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_7048794
_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         'C37 H65 O P Th'
_chemical_formula_sum            'C37 H65 O P Th'
_chemical_formula_weight         788.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-03
_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                 92.286(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2839(3)
_cell_length_b                   18.1136(5)
_cell_length_c                   16.7491(5)
_cell_measurement_reflns_used    10469
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.2310
_cell_measurement_theta_min      3.6270
_cell_volume                     3723.80(18)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_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   -110.00 -13.00   1.00    1.00    --  -39.24 -57.00 -60.00   97
  2  \w    -65.00  34.00   1.00    1.00    --  -39.24  57.00  90.00   99
  3  \w    -62.00 -34.00   1.00    1.00    --  -39.24 178.00  90.00   28
  4  \w     17.00 113.00   1.00    1.00    --   39.24  37.00-120.00   96
  5  \w     60.00  97.00   1.00    1.00    --   39.24 178.00 -90.00   37
  6  \w     47.00  74.00   1.00    1.00    --   39.24 -99.00  90.00   27
  7  \w     71.00 128.00   1.00    1.00    --   39.24 178.00 -30.00   57
  8  \w     40.00 137.00   1.00    1.00    --  108.44 -30.00-150.00   97
  9  \w     75.00 119.00   1.00    1.00    --  108.44-125.00 -90.00   44
 10  \w     37.00  79.00   1.00    1.00    --  108.44 -30.00   0.00   42
 11  \w     36.00  64.00   1.00    1.00    --  108.44-125.00 -90.00   28
 12  \w     85.00 177.00   1.00    1.00    --  108.44  45.00  30.00   92
 13  \w     30.00 160.00   1.00    1.00    --  108.44 -15.00  30.00  130
 14  \w     80.00 121.00   1.00    1.00    --  108.44-125.00 120.00   41
 15  \w     82.00 109.00   1.00    1.00    --  108.44 -94.00 -30.00   27
 16  \w     37.00 138.00   1.00    1.00    --  108.44 -61.00  90.00  101
 17  \w    127.00 178.00   1.00    1.00    --  108.44 125.00 -60.00   51
 18  \w     43.00 115.00   1.00    1.00    --  108.44 -61.00   0.00   72
 19  \w     38.00 141.00   1.00    1.00    --  108.44 -77.00-120.00  103
;
_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      -0.1031052000
_diffrn_orient_matrix_UB_12      0.0294571000
_diffrn_orient_matrix_UB_13      0.0384110000
_diffrn_orient_matrix_UB_21      -0.0173638000
_diffrn_orient_matrix_UB_22      -0.0757725000
_diffrn_orient_matrix_UB_23      0.0394659000
_diffrn_orient_matrix_UB_31      0.0692429000
_diffrn_orient_matrix_UB_32      0.0249727000
_diffrn_orient_matrix_UB_33      0.0738670000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24887
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.988
_diffrn_reflns_theta_min         3.596
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.487
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32805
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         6.457
_refine_diff_density_min         -3.423
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7437
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0801P)^2^+60.5077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6176
_reflns_number_total             7437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00012g2.cif
_cod_data_source_block           compound9
_cod_depositor_comments
'Adding full bibliography for 7048788--7048794.cif.'
_cod_original_cell_volume        3723.81(17)
_cod_database_code               7048794
_chemical_oxdiff_formula         C1H1O1P1Th1
_reflns_odcompleteness_completeness 99.97
_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. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C37(H37A,H37B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22)
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), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C)
;
_shelx_res_checksum              75374
_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 2.050
_oxdiff_exptl_absorpt_empirical_full_min 0.484