Cyclopentadienyl capped thorium(IV) porphyrinoid complex.
Mangel, Daniel N.; Brewster, James T.; Juarez, Gabriel J.; Lynch, Vincent M.; Sessler, Jonathan L.; Chemical communications (Cambridge, England) 60 (2024) 1020–1022; doi:10.1039/d3cc05283d

data_7132548
_publ_section_title
;
 Cyclopentadienyl capped thorium(IV) porphyrinoid complex.
;
_journal_issue                   8
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1020
_journal_page_last               1022
_journal_paper_doi               10.1039/d3cc05283d
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C70 H66 N6 O4 Th + 2 C4H8O'
_chemical_formula_sum            'C78 H82 N6 O6 Th'
_chemical_formula_weight         1431.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-12-18
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2023-12-20 deposited with the CCDC.	2023-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                92.412(5)
_cell_angle_beta                 90.923(6)
_cell_angle_gamma                117.468(7)
_cell_formula_units_Z            2
_cell_length_a                   14.3339(12)
_cell_length_b                   14.7275(9)
_cell_length_c                   17.9016(11)
_cell_measurement_reflns_used    2591
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      72.0230
_cell_measurement_theta_min      3.3540
_cell_volume                     3347.4(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.946
_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   -113.00 -16.00   1.00   29.50    --  -42.67 -57.00 -90.00   97
  2  \w    -66.00  27.00   1.00   29.50    --  -42.67  57.00  60.00   93
  3  \w    -70.00  26.00   1.00   29.50    --  -42.67  77.00-180.00   96
  4  \w     35.00 129.00   1.00   97.50    --  106.64 -30.00-150.00   94
  5  \w     58.00  99.00   1.00   97.50    --  106.64-125.00-180.00   41
  6  \w     35.00 127.00   1.00   97.50    --  106.64 -30.00  30.00   92
  7  \w     33.00 129.00   1.00   97.50    --  106.64 -30.00 -60.00   96
  8  \w     40.00 117.00   1.00   97.50    --  106.64-125.00 120.00   77
  9  \w     49.00  99.00   1.00   97.50    --  106.64 -94.00-120.00   50
 10  \w     49.00  95.00   1.00   97.50    --  106.64 -94.00-180.00   46
 11  \w     36.00 130.00   1.00   97.50    --  106.64 -30.00 120.00   94
 12  \w     48.00 138.00   1.00   97.50    --  106.64 -77.00 -90.00   90
;
_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      0.0469067000
_diffrn_orient_matrix_UB_12      0.1065020000
_diffrn_orient_matrix_UB_13      0.0413388000
_diffrn_orient_matrix_UB_21      0.0010339000
_diffrn_orient_matrix_UB_22      0.0490113000
_diffrn_orient_matrix_UB_23      -0.0745337000
_diffrn_orient_matrix_UB_31      -0.1117828000
_diffrn_orient_matrix_UB_32      -0.0140712000
_diffrn_orient_matrix_UB_33      0.0129125000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1307
_diffrn_reflns_av_unetI/netI     0.2079
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20542
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.826
_diffrn_reflns_theta_min         3.388
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.643
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.393
_exptl_absorpt_correction_type   'gaussian and multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.88a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       needle
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.035
_refine_diff_density_max         5.326
_refine_diff_density_min         -2.763
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         12828
_refine_ls_number_restraints     1299
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0994
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1067P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2335
_refine_ls_wR_factor_ref         0.2638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8357
_reflns_number_total             12828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05283d2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7132547--7132548.cif.'
_cod_original_cell_volume        3347.4(4)
_cod_database_code               7132548
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C78H66N6O4ThCl2
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.310
_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
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C31(H31A,H31B), C39(H39A,H39B), C41(H41A,H41B), C43(H43A,
 H43B), C45(H45A,H45B), C53(H53A,H53B), C55(H55A,H55B)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C25(H25), C26(H26), C27(H27), C34(H34),
 C35(H35), C36(H36), C37(H37), C38(H38), C48(H48), C49(H49), C50(H50), C51(H51),
  C52(H52), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C66(H66),
 C67(H67), C68(H68), C69(H69), C70(H70)
4.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C40(H40A,H40B,H40C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C54(H54A,H54B,H54C), C56(H56A,
 H56B,H56C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              6395
_shelx_hkl_checksum              55121
_shelx_fab_checksum              84706
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.388
_oxdiff_exptl_absorpt_empirical_full_min 0.412