Samarocene oxide: from an undesired decomposition product to a new reagent
Christoph Schoo; Svetlana V. Klementyeva; Michael T. Gamer; Sergey N. Konchenko; Peter W. Roesky; Chem.Commun. 52 (2016) 6654–; doi:

data_7119116
_publ_section_title
;
 Samarocene oxide: from an undesired decomposition product to a new
 reagent
;
_journal_name_full               Chem.Commun.
_journal_page_first              6654
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C45 H68 O2 S2 Sm2'
_chemical_formula_sum            'C45 H68 O2 S2 Sm2'
_chemical_formula_weight         1005.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-02-26 deposited with the CCDC.
2016-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.26(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.588(4)
_cell_length_b                   23.602(5)
_cell_length_c                   21.654(4)
_cell_measurement_reflns_used    19591
_cell_measurement_temperature    195(2)
_cell_measurement_theta_max      29.69
_cell_measurement_theta_min      1.73
_cell_volume                     9072(4)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2009)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction
'STOE X-RED & X-SHAPE, PLATON (A.L.Spek, 2009)'
_computing_molecular_graphics    'Diamond 2/3, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'MS Word, Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2008)'
_diffrn_ambient_temperature      195.15
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'two-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5mm monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.1188
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39419
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.924
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    2.689
_exptl_absorpt_correction_T_max  0.6500
_exptl_absorpt_correction_T_min  0.5731
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed & XShape'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       block
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.471
_exptl_crystal_size_mid          0.466
_exptl_crystal_size_min          0.392
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.704
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         17571
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.704
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0230P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7215
_reflns_number_total             17571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc02450e2.cif
_cod_data_source_block           3
_cod_original_cell_volume        9072(3)
_cod_database_code               7119116
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C5 \\sim C10A \\sim C10B: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
Uanis(C5) \\sim Ueq: with sigma of 0.7 and sigma for terminal atoms of 0.6
3. Others
 Fixed Sof: H44A(0.5) H44B(0.5) H44C(0.5) H44D(0.5) H41C(0.5) H41D(0.5)
 H41A(0.5) H41B(0.5) C27A(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C43A(0.5)
 H43A(0.5) H43B(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) H6AC(0.5) C28A(0.5) H28A(0.5)
 H28B(0.5) H28C(0.5) C10A(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C30A(0.5)
 H30A(0.5) H30B(0.5) H30C(0.5) C42A(0.5) H42A(0.5) H42B(0.5) C26A(0.5)
 H26A(0.5) H26B(0.5) H26C(0.5) C19B(0.5) H19A(0.5) H19B(0.5) H19C(0.5)
 C29B(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C11B(0.5) C16B(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5) C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5) C15B(0.5) C18B(0.5)
 H18A(0.5) H18B(0.5) H18C(0.5) C20B(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
 C17B(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C8B(0.5) H8BA(0.5) H8BB(0.5) H8BC(0.5)
 C12B(0.5) C9B(0.5) H9BA(0.5) H9BB(0.5) H9BC(0.5) C13B(0.5) C14B(0.5) H82A(0.5)
 H82B(0.5) H82C(0.5) H82D(0.5) C59A(0.5) H59A(0.5) H59B(0.5) H59C(0.5)
 C60A(0.5) H60A(0.5) H60B(0.5) H60C(0.5) C84B(0.5) H84A(0.5) H84B(0.5)
 C63B(0.5) C62B(0.5) C66B(0.5) C65B(0.5) C64B(0.5) C68B(0.5) H68A(0.5)
 H68B(0.5) H68C(0.5) C67B(0.5) H67A(0.5) H67B(0.5) H67C(0.5) C71B(0.5)
 H71A(0.5) H71B(0.5) H71C(0.5) C70B(0.5) H70A(0.5) H70B(0.5) H70C(0.5)
 C69B(0.5) H69A(0.5) H69B(0.5) H69C(0.5) C61B(0.5) H61A(0.5) H61B(0.5)
 H61C(0.5) C85B(0.5) H85A(0.5) H85B(0.5) C83B(0.5) H83A(0.5) H83B(0.5)
 C72B(0.5) C73B(0.5) C74B(0.5) C75B(0.5) C76B(0.5) C77B(0.5) H77A(0.5)
 H77B(0.5) H77C(0.5) C78B(0.5) H78A(0.5) H78B(0.5) H78C(0.5) C79B(0.5)
 H79A(0.5) H79B(0.5) H79C(0.5) C80B(0.5) H80A(0.5) H80B(0.5) H80C(0.5)
 C81B(0.5) H81A(0.5) H81B(0.5) H81C(0.5) C57B(0.5) H57A(0.5) H57B(0.5)
 H57C(0.5) C58B(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C61A(0.5) H61D(0.5)
 H61E(0.5) H61F(0.5) C10B(0.5) H10D(0.5) H10E(0.5) H10F(0.5) C85A(0.5)
 H85C(0.5) H85D(0.5) C57A(0.5) H57D(0.5) H57E(0.5) H57F(0.5) C58A(0.5)
 H58D(0.5) H58E(0.5) H58F(0.5) C27B(0.5) H27D(0.5) H27E(0.5) H27F(0.5)
 C83A(0.5) H83C(0.5) H83D(0.5) C84A(0.5) H84C(0.5) H84D(0.5) C75A(0.5)
 C76A(0.5) C72A(0.5) C73A(0.5) C74A(0.5) C80A(0.5) H80D(0.5) H80E(0.5)
 H80F(0.5) C81A(0.5) H81D(0.5) H81E(0.5) H81F(0.5) C0AA(0.5) H0AA(0.5)
 H0AB(0.5) H0AC(0.5) C78A(0.5) H78D(0.5) H78E(0.5) H78F(0.5) C79A(0.5)
 H79D(0.5) H79E(0.5) H79F(0.5) C12A(0.5) C13A(0.5) C14A(0.5) C15A(0.5)
 C11A(0.5) C17A(0.5) H17D(0.5) H17E(0.5) H17F(0.5) C18A(0.5) H18D(0.5)
 H18E(0.5) H18F(0.5) C19A(0.5) H19D(0.5) H19E(0.5) H19F(0.5) C20A(0.5)
 H20D(0.5) H20E(0.5) H20F(0.5) C16A(0.5) H16D(0.5) H16E(0.5) H16F(0.5)
 C59B(0.5) H59D(0.5) H59E(0.5) H59F(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) H6BC(0.5)
 C42B(0.5) H42C(0.5) H42D(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5) C9A(0.5)
 H9AA(0.5) H9AB(0.5) H9AC(0.5) C63A(0.5) C62A(0.5) C66A(0.5) C65A(0.5)
 C64A(0.5) C68A(0.5) H68D(0.5) H68E(0.5) H68F(0.5) C67A(0.5) H67D(0.5)
 H67E(0.5) H67F(0.5) C71A(0.5) H71D(0.5) H71E(0.5) H71F(0.5) C70A(0.5)
 H70D(0.5) H70E(0.5) H70F(0.5) C69A(0.5) H69D(0.5) H69E(0.5) H69F(0.5) C8A(0.5)
 H8AA(0.5) H8AB(0.5) H8AC(0.5) C29A(0.5) H29D(0.5) H29E(0.5) H29F(0.5)
 C43B(0.5) H43C(0.5) H43D(0.5) C30B(0.5) H30D(0.5) H30E(0.5) H30F(0.5)
 C26B(0.5) H26D(0.5) H26E(0.5) H26F(0.5) C60B(0.5) H60D(0.5) H60E(0.5)
 H60F(0.5) C28B(0.5) H28D(0.5) H28E(0.5) H28F(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C44(H44C,H44D), C41(H41C,H41D), C41(H41A,H41B), C43A(H43A,
 H43B), C42A(H42A,H42B), C82(H82A,H82B), C82(H82C,H82D), C84B(H84A,H84B),
 C85B(H85A,H85B), C83B(H83A,H83B), C85A(H85C,H85D), C83A(H83C,H83D), C84A(H84C,
 H84D), C42B(H42C,H42D), C43B(H43C,H43D)
4.b Cp* refined as free rotating group:
 C63B(C62B,C66B,C65B,C64B,C68B,C67B,C71B,C70B,C69B), C72B(C73B,C74B,C75B,C76B,
 C77B,C78B,C79B,C80B,C81B), C75A(C76A,C72A,C73A,C74A,C80A,C81A,C0AA,C78A,C79A),
 C12A(C13A,C14A,C15A,C11A,C17A,C18A,C19A,C20A,C16A), C63A(C62A,C66A,C65A,C64A,
 C68A,C67A,C71A,C70A,C69A)
4.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C36(H36A,H36B,
 H36C), C39(H39A,H39B,H39C), C27A(H27A,H27B,H27C), C6A(H6AA,H6AB,H6AC),
 C28A(H28A,H28B,H28C), C10A(H10A,H10B,H10C), C30A(H30A,H30B,H30C), C26A(H26A,
 H26B,H26C), C19B(H19A,H19B,H19C), C29B(H29A,H29B,H29C), C16B(H16A,H16B,H16C),
 C7B(H7BA,H7BB,H7BC), C18B(H18A,H18B,H18C), C20B(H20A,H20B,H20C), C17B(H17A,
 H17B,H17C), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C52(H52A,H52B,H52C),
 C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C53(H53A,H53B,H53C), C55(H55A,H55B,
 H55C), C59A(H59A,H59B,H59C), C60A(H60A,H60B,H60C), C68B(H68A,H68B,H68C),
 C67B(H67A,H67B,H67C), C71B(H71A,H71B,H71C), C70B(H70A,H70B,H70C), C69B(H69A,
 H69B,H69C), C61B(H61A,H61B,H61C), C77B(H77A,H77B,H77C), C78B(H78A,H78B,H78C),
 C79B(H79A,H79B,H79C), C80B(H80A,H80B,H80C), C81B(H81A,H81B,H81C), C57B(H57A,
 H57B,H57C), C58B(H58A,H58B,H58C), C61A(H61D,H61E,H61F), C10B(H10D,H10E,H10F),
 C57A(H57D,H57E,H57F), C58A(H58D,H58E,H58F), C27B(H27D,H27E,H27F), C80A(H80D,
 H80E,H80F), C81A(H81D,H81E,H81F), C0AA(H0AA,H0AB,H0AC), C78A(H78D,H78E,H78F),
 C79A(H79D,H79E,H79F), C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F), C19A(H19D,
 H19E,H19F), C20A(H20D,H20E,H20F), C16A(H16D,H16E,H16F), C59B(H59D,H59E,H59F),
 C6B(H6BA,H6BB,H6BC), C7A(H7AA,H7AB,H7AC), C9A(H9AA,H9AB,H9AC), C68A(H68D,H68E,
 H68F), C67A(H67D,H67E,H67F), C71A(H71D,H71E,H71F), C70A(H70D,H70E,H70F),
 C69A(H69D,H69E,H69F), C8A(H8AA,H8AB,H8AC), C29A(H29D,H29E,H29F), C30B(H30D,
 H30E,H30F), C26B(H26D,H26E,H26F), C60B(H60D,H60E,H60F), C28B(H28D,H28E,H28F)
;
_shelx_res_checksum              62896
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'