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_7132547
_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         'C61 H61 Cl0.08 F0.92 N6 Th'
_chemical_formula_sum            'C61 H61 Cl0.08 F0.92 N6 Th'
_chemical_formula_weight         1130.51
_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'
_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                90
_cell_angle_beta                 90.9154(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.63492(9)
_cell_length_b                   11.85014(7)
_cell_length_c                   24.83906(14)
_cell_measurement_reflns_used    33312
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      75.6
_cell_measurement_theta_min      3.53
_cell_volume                     4895.80(5)
_computing_cell_refinement
'CrysAlisPro V 1.171.40.53, Rigaku Oxford Diffraction'
_computing_data_collection
'CrysAlisPro V 1.171.40.53, Rigaku Oxford Diffraction'
_computing_data_reduction
'CrysAlisPro V 1.171.40.53, Rigaku Oxford Diffraction'
_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)'
_computing_structure_solution    'SHELXT. (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Agilent SuperNova with an Atlas S2 CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            51244
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.779
_diffrn_reflns_theta_min         3.559
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    10.255
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.234
_exptl_absorpt_correction_type   'gaussian and multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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_density_diffrn    1.534
_exptl_crystal_description       prism
_exptl_crystal_F_000             2275
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.590
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         10134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+9.5763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9783
_reflns_number_total             10134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05283d2.cif
_cod_data_source_block           th-dpam-f
_cod_depositor_comments
'Adding full bibliography for 7132547--7132548.cif.'
_cod_database_code               7132547
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.530
_shelx_estimated_absorpt_t_min   0.234
_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. Others
 Fixed Sof: F1(0.92) Cl7(0.08)
3.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)
3.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), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61)
3.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)
;
_shelx_res_checksum              8145
_shelx_hkl_checksum              10756
_olex2_submission_special_instructions 'No special instructions were received'