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_7119120
_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 H66 N2 O8 Re2 Sm2'
_chemical_formula_sum            'C44 H66 N2 O8 Re2 Sm2'
_chemical_formula_weight         1424.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2016-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.207(3)
_cell_length_b                   14.000(3)
_cell_length_c                   21.465(4)
_cell_measurement_reflns_used    25670
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      29.42
_cell_measurement_theta_min      1.57
_cell_volume                     4870.4(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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      205.0
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_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  0.0444
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34712
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.137
_diffrn_reflns_theta_min         2.144
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    7.375
_exptl_absorpt_correction_T_max  0.5688
_exptl_absorpt_correction_T_min  0.2354
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed & XShape'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_description       prism
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.111
_refine_diff_density_max         1.454
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0509
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3703
_reflns_number_total             4809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc02450e2.cif
_cod_data_source_block           csp45pbca
_cod_original_cell_volume        4870.5(17)
_cod_database_code               7119120
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C10(H10A,H10B,H10C), C16(H16A,H16B,H16C), C8(H8A,H8B,
 H8C), C19(H19A,H19B,H19C), C6(H6A,H6B,H6C), C20(H20A,H20B,H20C), C9(H9A,H9B,
 H9C), C22(H22B,H22A,H22C), C7(H7A,H7B,H7C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              7740
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'