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_7119119
_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         'C54 H70 O4 Sm2, 2(C7 H8)'
_chemical_formula_sum            'C68 H86 O4 Sm2'
_chemical_formula_weight         1268.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                110.25(3)
_cell_angle_beta                 97.77(3)
_cell_angle_gamma                98.73(3)
_cell_formula_units_Z            1
_cell_length_a                   10.561(2)
_cell_length_b                   10.700(2)
_cell_length_c                   15.035(3)
_cell_measurement_reflns_used    30792
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.42
_cell_measurement_theta_min      1.99
_cell_volume                     1542.9(7)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0605
_diffrn_reflns_av_unetI/netI     0.0445
_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       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26833
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.999
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.992
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.929
_exptl_absorpt_correction_T_max  0.7587
_exptl_absorpt_correction_T_min  0.4933
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE''
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       prism
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.401
_exptl_crystal_size_mid          0.289
_exptl_crystal_size_min          0.154
_refine_diff_density_max         1.180
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         6049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0522P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5171
_reflns_number_total             6049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc02450e2.cif
_cod_data_source_block           7
_cod_original_cell_volume        1542.9(6)
_cod_database_code               7119119
_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. Others
 Fixed Sof: C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C34(0.5) H34(0.5) C29(0.5)
 C30(0.5) H30(0.5) C31(0.5) H31(0.5) C32(0.5) H32(0.5) C33(0.5) H33(0.5)
 C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C38(0.5) H38(0.5) C37(0.5) H37(0.5)
 C36(0.5) C41(0.5) H41(0.5) C40(0.5) H40(0.5) C39(0.5) H39(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C6(H6), C34(H34), C30(H30), C31(H31),
 C32(H32), C33(H33), C38(H38), C37(H37), C41(H41), C40(H40), C39(H39)
3.b Fitted hexagon refined as free rotating group:
 C34(C29,C30,C31,C32,C33), C38(C37,C36,C41,C40,C39)
3.c Cp* refined as free rotating group:
 C18(C19,C20,C21,C22,C23,C24,C25,C26,C27)
3.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C15(H15A,H15B,H15C), C13(H13A,
 H13B,H13C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C28(H28A,H28B,H28C),
 C35(H35A,H35B,H35C)
;
_shelx_res_checksum              94257
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'