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_7712109
_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         'C41 H59 N2 O2 Sm'
_chemical_formula_sum            'C41 H59 N2 O2 Sm'
_chemical_formula_weight         762.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-11-15 deposited with the CCDC.	2023-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.842(2)
_cell_length_b                   18.607(4)
_cell_length_c                   18.765(4)
_cell_measurement_reflns_used    7196
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     3785.6(13)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47416
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.687
_diffrn_reflns_theta_min         1.541
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       plate
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.940
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 3009 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7196
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0475P)^2^+1.5365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0767
_reflns_Friedel_coverage         0.788
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6999
_reflns_number_total             7196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04164b2.cif
_cod_data_source_block           2
_cod_database_code               7712109
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.742
_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.a Ternary CH refined with riding coordinates:
 C23(H23), C10(H10), C16(H16), C35(H35), C2(H2), C36(H36), C34(H34), C39(H39),
 C38(H38), C37(H37), C40(H40), C41(H41)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C32(H32A,H32B), C29(H29A,H29B), C33(H33A,H33B), C26(H26A,
 H26B), C31(H31A,H31B), C28(H28A,H28B), C27(H27A,H27B)
2.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C21(H21), C13(H13), C7(H7), C20(H20), C5(H5), C6(H6)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C12(H12A,H12B,H12C), C3(H3A,H3B,
 H3C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C1(H1A,H1B,H1C), C11(H11A,H11B,
 H11C)
;
_shelx_res_checksum              12826
_shelx_hkl_checksum              79843
_olex2_submission_special_instructions 'No special instructions were received'