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_7119117
_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         'C44 H68 O4 S Sm2'
_chemical_formula_sum            'C44 H68 O4 S Sm2'
_chemical_formula_weight         993.74
_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
_audit_creation_date             2015-11-24
_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                 108.56(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.824(4)
_cell_length_b                   16.299(3)
_cell_length_c                   16.056(3)
_cell_measurement_reflns_used    7571
_cell_measurement_temperature    195
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      1.74
_cell_volume                     4421.9(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      195.0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.1738
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18573
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.999
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.736
_exptl_absorpt_coefficient_mu    2.715
_exptl_absorpt_correction_T_max  0.8115
_exptl_absorpt_correction_T_min  0.6772
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed & XShape'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.201
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.731
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         8591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.731
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.099
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0220P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4297
_reflns_number_total             8591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc02450e2.cif
_cod_data_source_block           4
_cod_database_code               7119117
_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, All C(H,H,H,H,H,H) groups
2. Others
 Fixed Sof: C35B(0.5) C34B(0.5) C33B(0.5) C32B(0.5) C31B(0.5) C40B(0.5)
 H40A(0.5) H40B(0.5) H40C(0.5) C39B(0.5) H39A(0.5) H39B(0.5) H39C(0.5)
 C38B(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C37B(0.5) H37A(0.5) H37B(0.5)
 H37C(0.5) H41A(0.5) H41B(0.5) H41C(0.5) H41D(0.5) C42B(0.5) H42A(0.5)
 H42B(0.5) C43B(0.5) H43A(0.5) H43B(0.5) C44B(0.5) H44A(0.5) H44B(0.5)
 C14B(0.5) C13B(0.5) C12B(0.5) C11B(0.5) C15B(0.5) C19B(0.5) H19A(0.5)
 H19B(0.5) H19C(0.5) C18B(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C17B(0.5)
 H17A(0.5) H17B(0.5) H17C(0.5) C16B(0.5) H16A(0.5) H16B(0.5) H16C(0.5)
 C20B(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C42A(0.5) H42C(0.5) H42D(0.5)
 C44A(0.5) H44C(0.5) H44D(0.5) C43A(0.5) H43C(0.5) H43D(0.5) C35A(0.5)
 C34A(0.5) C33A(0.5) C32A(0.5) C31A(0.5) C40A(0.5) H40D(0.5) H40E(0.5)
 H40F(0.5) C39A(0.5) H39D(0.5) H39E(0.5) H39F(0.5) C38A(0.5) H38D(0.5)
 H38E(0.5) H38F(0.5) C37A(0.5) H37D(0.5) H37E(0.5) H37F(0.5) C15A(0.5)
 C14A(0.5) C13A(0.5) C12A(0.5) C11A(0.5) C20A(0.5) H20D(0.5) H20E(0.5)
 H20F(0.5) C19A(0.5) H19D(0.5) H19E(0.5) H19F(0.5) C18A(0.5) H18D(0.5)
 H18E(0.5) H18F(0.5) C17A(0.5) H17D(0.5) H17E(0.5) H17F(0.5) C16A(0.5)
 H16D(0.5) H16E(0.5) H16F(0.5) H0AD(0.5) H0AE(0.5) H0AF(0.5) H0AA(0.5)
 H0AB(0.5) H0AC(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C41(H41C,H41D), C42B(H42A,H42B), C43B(H43A,H43B), C44B(H44A,
 H44B), C42A(H42C,H42D), C44A(H44C,H44D), C43A(H43C,H43D)
3.b Cp* refined as free rotating group:
 C14B(C13B,C12B,C11B,C15B,C19B,C18B,C17B,C16B,C20B), C15A(C14A,C13A,C12A,C11A,
 C20A,C19A,C18A,C17A,C16A)
3.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C40B(H40A,H40B,H40C), C39B(H39A,H39B,H39C), C38B(H38A,
 H38B,H38C), C37B(H37A,H37B,H37C), C7(H7A,H7B,H7C), C28(H28A,H28B,H28C), C8(H8A,
 H8B,H8C), C6(H6A,H6B,H6C), C29(H29A,H29B,H29C), C9(H9A,H9B,H9C), C27(H27A,H27B,
 H27C), C30(H30A,H30B,H30C), C10(H10A,H10B,H10C), C19B(H19A,H19B,H19C),
 C18B(H18A,H18B,H18C), C17B(H17A,H17B,H17C), C16B(H16A,H16B,H16C), C20B(H20A,
 H20B,H20C), C40A(H40D,H40E,H40F), C39A(H39D,H39E,H39F), C38A(H38D,H38E,H38F),
 C37A(H37D,H37E,H37F), C20A(H20D,H20E,H20F), C19A(H19D,H19E,H19F), C18A(H18D,
 H18E,H18F), C17A(H17D,H17E,H17F), C16A(H16D,H16E,H16F), C0AA(H0AD,H0AE,H0AF),
 C0AA(H0AA,H0AB,H0AC)
;
_shelx_res_checksum              8743
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'