Formation of a cyclooctatetraenylsamarium(III) inverse sandwich that ring-opens tetrahydrofuran.
Peedika Paramban, Ramees; Guo, Zhifang; Deacon, Glen B.; Junk, Peter C.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d2dt04164b

data_7712108
_publ_section_title
;
 Formation of a cyclooctatetraenylsamarium(III) inverse sandwich that
 ring-opens tetrahydrofuran.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt04164b
_journal_year                    2023
_chemical_formula_moiety         'C108 H148 N8 Sm2, 4(C6 H6)'
_chemical_formula_sum            'C132 H172 N8 Sm2'
_chemical_formula_weight         2171.47
_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   mixed
_audit_creation_date             2021-11-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-11-15 deposited with the CCDC.	2023-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                95.1820(10)
_cell_angle_beta                 96.0570(10)
_cell_angle_gamma                98.3200(10)
_cell_formula_units_Z            2
_cell_length_a                   15.9605(2)
_cell_length_b                   17.7059(2)
_cell_length_c                   21.0634(3)
_cell_measurement_reflns_used    20432
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     5823.06(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            20432
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.299
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       plate
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.859
_refine_diff_density_min         -1.459
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1284
_refine_ls_number_reflns         20432
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+33.0307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18331
_reflns_number_total             20432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04164b2.cif
_cod_data_source_block           mx132_21_auto_tw
_cod_database_code               7712108
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.806
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.88109
 0.11891
2. Restrained distances
 C116-C117 = C119-C120 = C120-C115
 1.37 with sigma of 0.02
 C116-C115
 1.38 with sigma of 0.02
 C117-C118 = C118-C119
 1.36 with sigma of 0.02
 C109-C110 = C112-C113 = C113-C114
 1.37 with sigma of 0.02
 C109-C114
 1.38 with sigma of 0.02
 C110-C111 = C111-C112
 1.36 with sigma of 0.02
 C116-C120
 2.38 with sigma of 0.04
 C117-C119
 2.36 with sigma of 0.04
 C116-C118 = C118-C120 = C119-C115
 2.37 with sigma of 0.04
 C110-C112
 2.36 with sigma of 0.04
 C109-C113
 2.38 with sigma of 0.04
 C109-C111 = C111-C113 = C112-C114
 2.37 with sigma of 0.04
 C116-C117 \\sim C117-C118 \\sim C118-C119 \\sim C119-C120 \\sim C120-C115
\\sim C115-C116
 with sigma of 0.02
 C116-C120 \\sim C116-C118 \\sim C120-C118 \\sim C119-C117 \\sim C119-C115
\\sim C115-C117
 with sigma of 0.04
 C109-C110 \\sim C110-C111 \\sim C111-C112 \\sim C112-C113 \\sim C113-C114
\\sim C114-C109
 with sigma of 0.02
 C109-C113 \\sim C109-C111 \\sim C113-C111 \\sim C112-C110 \\sim C112-C114
\\sim C114-C110
 with sigma of 0.04
 C12-C10 \\sim C10-C12A
 with sigma of 0.02
 C11-C10 \\sim C10-C11A
 with sigma of 0.02
3. Restrained planarity
 C116, C117, C118, C119, C120, C115
 with sigma of 0.1
 C109, C110, C111, C112, C113, C114
 with sigma of 0.1
4. Rigid bond restraints
 C36, C37, C35
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C12, C12A, C11, C11A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C26, C28, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
C36 \\sim C35 \\sim C37: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01 within 2A
C116 \\sim C117 \\sim C118 \\sim C119 \\sim C120 \\sim C115: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C109 \\sim C110 \\sim C111 \\sim C112 \\sim C113 \\sim C114: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C12 \\sim C12A \\sim C11 \\sim C11A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 2A
C126 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C116 \\sim C120 \\sim C119 \\sim C115 \\sim C118 \\sim C117: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C35 \\sim C37 \\sim C36: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
C26 \\sim C28 \\sim C27: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.001 within 2A
6. Rigid body (RIGU) restrains
 C116, C117, C118, C119, C120, C115
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C109, C110, C111, C112, C113, C114
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(H10A)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(H10)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C11)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=FVAR(1)
8.a Riding coordinates:
 C36(H36A,H36B,H36C)
8.b Ternary CH refined with riding coordinates:
 C86(H86), C81(H81), C106(H106), C3(H3), C93(H93), C68(H68), C20(H20),
 C48(H48), C103(H103), C45(H45), C61(H61), C10(H10), C10(H10A), C74(H74),
 C23(H23), C28(H28), C35(H35)
8.c Aromatic/amide H refined with riding coordinates:
 C53(H53), C54(H54), C51(H51), C55(H55), C52(H52), C58(H58), C56(H56),
 C57(H57), C96(H96), C13(H13), C71(H71), C38(H38), C90(H90), C78(H78), C76(H76),
  C63(H63), C64(H64), C77(H77), C101(H101), C89(H89), C41(H41), C5(H5),
 C88(H88), C43(H43), C65(H65), C100(H100), C30(H30), C16(H16), C42(H42),
 C17(H17), C99(H99), C7(H7), C6(H6), C18(H18), C31(H31), C129(H129), C128(H128),
  C127(H127), C132(H132), C131(H131), C130(H130), C32(H32), C121(H121),
 C126(H126), C125(H125), C124(H124), C123(H123), C122(H122), C120(H120),
 C119(H119), C118(H118), C117(H117), C116(H116), C115(H115), C109(H109),
 C114(H114), C113(H113), C112(H112), C111(H111), C110(H110)
8.d Fitted hexagon refined as free rotating group:
 C129(C128,C127,C132,C131,C130), C121(C126,C125,C124,C123,C122), C120(C119,
 C118,C117,C116,C115), C109(C114,C113,C112,C111,C110)
8.e Idealised Me refined as rotating group:
 C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C84(H84A,H84B,H84C), C1(H1A,H1B,
 H1C), C2(H2A,H2B,H2C), C85(H85A,H85B,H85C), C46(H46A,H46B,H46C), C50(H50A,H50B,
 H50C), C108(H10B,H10C,H10D), C104(H10E,H10F,H10G), C59(H59A,H59B,H59C),
 C47(H47A,H47B,H47C), C73(H73A,H73B,H73C), C24(H24A,H24B,H24C), C70(H70A,H70B,
 H70C), C25(H25A,H25B,H25C), C60(H60A,H60B,H60C), C82(H82A,H82B,H82C), C22(H22A,
 H22B,H22C), C83(H83A,H83B,H83C), C105(H10H,H10I,H10J), C49(H49A,H49B,H49C),
 C107(H10K,H10L,H10M), C21(H21A,H21B,H21C), C69(H69A,H69B,H69C), C72(H72A,H72B,
 H72C), C26(H26A,H26B,H26C), C12(H12A,H12B,H12C), C37(H37A,H37B,H37C), C11(H11A,
 H11B,H11C), C27(H27A,H27B,H27C), C11A(H11D,H11E,H11F), C12A(H12D,H12E,H12F)
;
_shelx_res_checksum              29785
_shelx_hkl_checksum              46434
_olex2_submission_special_instructions 'No special instructions were received'