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_7119118
_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         'C50 H70 N2 O4 S Sm2'
_chemical_formula_sum            'C50 H70 N2 O4 S Sm2'
_chemical_formula_weight         1095.84
_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             2015-10-02
_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                 90.81(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.952(3)
_cell_length_b                   13.879(3)
_cell_length_c                   20.819(4)
_cell_measurement_reflns_used    10961
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      29.33
_cell_measurement_theta_min      1.76
_cell_volume                     4897.7(17)
_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      210.0
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.1396
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21566
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.998
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.763
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    2.47
_exptl_absorpt_correction_T_max  0.7725
_exptl_absorpt_correction_T_min  0.5783
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            yellow/green
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       plates
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.113
_refine_diff_density_max         1.611
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.840
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         9533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.840
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0472
_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          0.0745
_refine_ls_wR_factor_ref         0.0823
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5516
_reflns_number_total             9533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc02450e2.cif
_cod_data_source_block           5
_cod_database_code               7119118
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C46(H46), C50(H50), C22(H22), C48(H48), C25(H25), C23(H23), C21(H21),
 C24(H24), C47(H47), C49(H49)
2.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C44(H44A,H44B,H44C), C42(H42A,H42B,H42C), C6(H6A,H6B,
 H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C32(H32A,H32B,H32C), C8(H8A,H8B,
 H8C), C19(H19A,H19B,H19C), C43(H43A,H43B,H43C), C17(H17A,H17B,H17C), C41(H41A,
 H41B,H41C), C34(H34A,H34B,H34C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C),
 C35(H35A,H35B,H35C), C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C45(H45A,H45B,H45C),
  C33(H33A,H33B,H33C)
;
_shelx_res_checksum              10699
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'