Multiply Engaged Molecular Gear composed of Cerium (IV) Double-Decker of a triptycene-functionalized Porphyrin
Nishino, Toshio; Fukumura, Masafumi; Katao, Shohei; Yasuhara, Kazuma; Rapenne, Gwenael; Dalton Transactions  (2023) –; doi:10.1039/D3DT02443A

data_7713723
_publ_section_title
;
 Multiply Engaged Molecular Gear composed of Cerium (IV) Double-Decker of
 a triptycene-functionalized Porphyrin
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02443A
_journal_year                    2023
_chemical_formula_moiety         'C184 H152 Ce N8 O8, 2(C H Cl3)'
_chemical_formula_sum            'C186 H154 Ce Cl6 N8 O8'
_chemical_formula_weight         2981.98
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-04-24 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120.0000(13)
_cell_formula_units_Z            18
_cell_length_a                   41.9814(5)
_cell_length_b                   41.9814(8)
_cell_length_c                   53.6321(10)
_cell_measurement_reflns_used    238784
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.375
_cell_measurement_theta_min      1.89
_cell_volume                     81860(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      103.15
_diffrn_detector                 'Rigaku curved IP area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'Imaging plate area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku VariMax RAPID'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            391865
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.351
_diffrn_reflns_theta_min         1.887
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              'MicroMax 007'
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_description       block
_exptl_crystal_F_000             27900
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform, methanol'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.768
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1926
_refine_ls_number_reflns         33301
_refine_ls_number_restraints     239
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0860
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2678
_refine_ls_wR_factor_ref         0.2866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25547
_reflns_number_total             33301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02443a2.cif
_cod_data_source_block           CeL2
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7713723
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.926
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O8-C145 = O2-C151
 1.43 with sigma of 0.02
 C153-C154
 1.52 with sigma of 0.02
 O2-C187
 1.43 with sigma of 0.02
 C187-C191 = C152-C153
 1.52 with sigma of 0.02
 C151-C152 = C191-C153
 1.52 with sigma of 0.02
 O4-C190
 1.43 with sigma of 0.02
 C159-C161 = C190-C183
 1.52 with sigma of 0.02
 O4-C159
 1.43 with sigma of 0.02
 O4-C95
 1.43 with sigma of 0.02
 C171-C172 = C173-C174
 1.52 with sigma of 0.02
 C172-C173
 1.52 with sigma of 0.02
 C160-C161
 1.52 with sigma of 0.02
 C162-C160
 1.52 with sigma of 0.02
 C160-C183
 1.52 with sigma of 0.02
 C155-C156 = C157-C158
 1.52 with sigma of 0.02
 C156-C157
 1.52 with sigma of 0.02
 O3-C155
 1.43 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C171 \\sim C172 \\sim C174 \\sim C173: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
C43 \\sim C44 \\sim C49 \\sim C48 \\sim C47 \\sim C46 \\sim C45 \\sim C58 \\sim
C50 \\sim C61 \\sim C60 \\sim C59 \\sim C62 \\sim C57 \\sim C56 \\sim C55 \\sim
C54 \\sim C51 \\sim C52 \\sim C53: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
4. Rigid body (RIGU) restrains
 C152, C153, C154, C151
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C162, C160, C161, C159
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C155, C156, C157, C158
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C187, C191, C153
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C159(0.5) H15F(0.5) H15G(0.5) H16P(0.5) H16Q(0.5) H16R(0.5)
 H16S(0.5) C161(0.5) H16T(0.5) H16U(0.5) H15L(0.5) H15M(0.5) H15N(0.5)
 H15O(0.5) C152(0.5) H15P(0.5) H15Q(0.5) C151(0.5) H15U(0.5) H15V(0.5)
 C183(0.5) H18A(0.5) H18B(0.5) C190(0.5) H19A(0.5) H19B(0.5) C187(0.5)
 H18C(0.5) H18D(0.5) C191(0.5) H19C(0.5) H19D(0.5)
6.a Ternary CH refined with riding coordinates:
 C106(H106), C78(H78), C128(H128), C50(H50), C179(H179), C180(H180)
6.b Secondary CH2 refined with riding coordinates:
 C163(H16A,H16B), C171(H17A,H17B), C147(H14A,H14B), C164(H16C,H16D), C155(H15A,
 H15B), C165(H16E,H16F), C168(H16G,H16H), C167(H16I,H16J), C159(H15F,H15G),
 C175(H17C,H17D), C149(H14C,H14D), C156(H15H,H15I), C169(H16N,H16O), C160(H16P,
 H16Q), C160(H16R,H16S), C161(H16T,H16U), C172(H17H,H17I), C173(H17J,H17K),
 C176(H17L,H17M), C177(H17N,H17O), C148(H14E,H14F), C157(H15J,H15K), C153(H15L,
 H15M), C153(H15N,H15O), C152(H15P,H15Q), C151(H15U,H15V), C183(H18A,H18B),
 C190(H19A,H19B), C187(H18C,H18D), C191(H19C,H19D)
6.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C14(H14), C13(H13), C28(H28), C32(H32), C8(H8), C37(H37), C27(H27),
 C19(H19), C38(H38), C9(H9), C89(H89), C92(H92), C96(H96), C18(H18), C108(H108),
  C3(H3), C22(H22), C4(H4), C73(H73), C123(H123), C23(H23), C80(H80),
 C114(H114), C86(H86), C88(H88), C76(H76), C118(H118), C101(H101), C87(H87),
 C94(H94), C109(H109), C102(H102), C110(H110), C124(H124), C126(H126), C83(H83),
  C133(H133), C111(H111), C82(H82), C74(H74), C125(H125), C104(H104), C75(H75),
 C68(H68), C103(H103), C81(H81), C182(H182), C142(H142), C64(H64), C146(H146),
 C130(H130), C185(H185), C66(H66), C139(H139), C188(H188), C136(H136),
 C116(H116), C132(H132), C186(H186), C131(H131), C137(H137), C138(H138),
 C58(H58), C55(H55), C144(H144), C45(H45), C52(H52), C46(H46), C48(H48),
 C61(H61), C59(H59), C53(H53), C54(H54), C47(H47), C60(H60)
6.d Idealised Me refined as rotating group:
 C150(H15C,H15D,H15E), C166(H16K,H16L,H16M), C170(H17E,H17F,H17G), C162(H16V,
 H16W,H16X), C174(H17P,H17Q,H17R), C178(H17S,H17T,H17U), C158(H15R,H15S,H15T),
 C154(H15W,H15X,H15Y)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              87498
_shelx_fab_checksum              54154
_olex2_submission_special_instructions 'No special instructions were received'