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_7119115
_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 O3 S Sm2'
_chemical_formula_sum            'C45 H68 O3 S Sm2'
_chemical_formula_weight         989.75
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-02-26 deposited with the CCDC.
2016-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.381(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7989(9)
_cell_length_b                   23.324(2)
_cell_length_c                   18.5920(16)
_cell_measurement_reflns_used    26000
_cell_measurement_temperature    150
_cell_measurement_theta_max      1.44
_cell_measurement_theta_min      26.20
_cell_volume                     4492.7(7)
_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      150
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.980
_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  0.0845
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34784
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.217
_diffrn_reflns_theta_min         1.437
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    2.670
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       prism
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.343
_exptl_crystal_size_min          0.285
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         8859
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0528
_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^)+(0.1004P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1579
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6391
_reflns_number_total             8859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc02450e2.cif
_cod_data_source_block           2
_cod_original_cell_volume        4492.8(7)
_cod_database_code               7119115
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C25-S1A
 1.8 with sigma of 0.02
 C25-S1B
 1.8 with sigma of 0.02
 C25-O3A
 1.36 with sigma of 0.005
 C25-O3B
 1.36 with sigma of 0.005
 C22A-C23A
 1.5 with sigma of 0.02
 C21B-C22B
 1.5 with sigma of 0.02
 C22B-C23B
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O3A \\sim C25 \\sim O3B: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
4. Others
 Fixed Sof: S1A(0.5) S1B(0.5) O3A(0.5) O3B(0.5) C1A(0.5) C2A(0.5) C3A(0.5)
 C4A(0.5) C5A(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) H6AC(0.5) C7A(0.5) H7AA(0.5)
 H7AB(0.5) H7AC(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5) C9A(0.5) H9AA(0.5)
 H9AB(0.5) H9AC(0.5) C10A(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C1B(0.5) C2B(0.5)
 C3B(0.5) C4B(0.5) C5B(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) H6BC(0.5) C7B(0.5)
 H7BA(0.5) H7BB(0.5) H7BC(0.5) C8B(0.5) H8BA(0.5) H8BB(0.5) H8BC(0.5) C9B(0.5)
 H9BA(0.5) H9BB(0.5) H9BC(0.5) C10B(0.5) H10D(0.5) H10E(0.5) H10F(0.5)
 C11A(0.5) C12A(0.5) C13A(0.5) C14A(0.5) C15A(0.5) C16A(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5) C17A(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C18A(0.5)
 H18A(0.5) H18B(0.5) H18C(0.5) C19A(0.5) H19A(0.5) H19B(0.5) H19C(0.5)
 C20A(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C11B(0.5) C12B(0.5) C13B(0.5)
 C14B(0.5) C15B(0.5) C16B(0.5) H16D(0.5) H16E(0.5) H16F(0.5) C17B(0.5)
 H17D(0.5) H17E(0.5) H17F(0.5) C18B(0.5) H18D(0.5) H18E(0.5) H18F(0.5)
 C19B(0.5) H19D(0.5) H19E(0.5) H19F(0.5) C20B(0.5) H20D(0.5) H20E(0.5)
 H20F(0.5) C21A(0.5) H21A(0.5) H21B(0.5) C21B(0.5) H21C(0.5) H21D(0.5)
 C22A(0.5) H22A(0.5) H22B(0.5) C22B(0.5) H22C(0.5) H22D(0.5) C23A(0.5)
 H23A(0.5) H23B(0.5) C23B(0.5) H23C(0.5) H23D(0.5) C24A(0.5) H24A(0.5)
 H24B(0.5) C24B(0.5) H24C(0.5) H24D(0.5) C26A(0.66667) C27A(0.66667)
 C28A(0.66667) C29A(0.66667) C30A(0.66667) C31A(0.66667) H31A(0.66667)
 H31B(0.66667) H31C(0.66667) C32A(0.66667) H32A(0.66667) H32B(0.66667)
 H32C(0.66667) C33A(0.66667) H33A(0.66667) H33B(0.66667) H33C(0.66667)
 C34A(0.66667) H34A(0.66667) H34B(0.66667) H34C(0.66667) C35A(0.66667)
 H35A(0.66667) H35B(0.66667) H35C(0.66667) C26B(0.33333) C27B(0.33333)
 C28B(0.33333) C29B(0.33333) C30B(0.33333) C31B(0.33333) H31D(0.33333)
 H31E(0.33333) H31F(0.33333) C32B(0.33333) H32D(0.33333) H32E(0.33333)
 H32F(0.33333) C33B(0.33333) H33D(0.33333) H33E(0.33333) H33F(0.33333)
 C34B(0.33333) H34D(0.33333) H34E(0.33333) H34F(0.33333) C35B(0.33333)
 H35D(0.33333) H35E(0.33333) H35F(0.33333) C36A(0.5) C37A(0.5) C38A(0.5)
 C39A(0.5) C40A(0.5) C41A(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C42A(0.5)
 H42A(0.5) H42B(0.5) H42C(0.5) C43A(0.5) H43A(0.5) H43B(0.5) H43C(0.5)
 C44A(0.5) H44A(0.5) H44B(0.5) H44C(0.5) C45A(0.5) H45A(0.5) H45B(0.5)
 H45C(0.5) C36B(0.5) C37B(0.5) C38B(0.5) C39B(0.5) C40B(0.5) C41B(0.5)
 H41D(0.5) H41E(0.5) H41F(0.5) C42B(0.5) H42D(0.5) H42E(0.5) H42F(0.5)
 C43B(0.5) H43D(0.5) H43E(0.5) H43F(0.5) C44B(0.5) H44D(0.5) H44E(0.5)
 H44F(0.5) C45B(0.5) H45D(0.5) H45E(0.5) H45F(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C21A(H21A,H21B), C21B(H21C,H21D), C22A(H22A,H22B), C22B(H22C,H22D), C23A(H23A,
 H23B), C23B(H23C,H23D), C24A(H24A,H24B), C24B(H24C,H24D)
5.b Cp* refined as free rotating group:
 C1A(C2A,C3A,C4A,C5A,C6A,C7A,C8A,C9A,C10A), C11A(C12A,C13A,C14A,C15A,C16A,C17A,
 C18A,C19A,C20A), C26A(C27A,C28A,C29A,C30A,C31A,C32A,C33A,C34A,C35A), C26B(C27B,
 C28B,C29B,C30B,C31B,C32B,C33B,C34B,C35B), C36A(C37A,C38A,C39A,C40A,C41A,C42A,
 C43A,C44A,C45A)
5.c Idealised Me refined as rotating group:
 C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,
 H9AC), C10A(H10A,H10B,H10C), C6B(H6BA,H6BB,H6BC), C7B(H7BA,H7BB,H7BC),
 C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F), C16A(H16A,H16B,
 H16C), C17A(H17A,H17B,H17C), C18A(H18A,H18B,H18C), C19A(H19A,H19B,H19C),
 C20A(H20A,H20B,H20C), C16B(H16D,H16E,H16F), C17B(H17D,H17E,H17F), C18B(H18D,
 H18E,H18F), C19B(H19D,H19E,H19F), C20B(H20D,H20E,H20F), C31A(H31A,H31B,H31C),
 C32A(H32A,H32B,H32C), C33A(H33A,H33B,H33C), C34A(H34A,H34B,H34C), C35A(H35A,
 H35B,H35C), C31B(H31D,H31E,H31F), C32B(H32D,H32E,H32F), C33B(H33D,H33E,H33F),
 C34B(H34D,H34E,H34F), C35B(H35D,H35E,H35F), C41A(H41A,H41B,H41C), C42A(H42A,
 H42B,H42C), C43A(H43A,H43B,H43C), C44A(H44A,H44B,H44C), C45A(H45A,H45B,H45C),
 C41B(H41D,H41E,H41F), C42B(H42D,H42E,H42F), C43B(H43D,H43E,H43F), C44B(H44D,
 H44E,H44F), C45B(H45D,H45E,H45F)
;
_shelx_res_checksum              30333
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'