Dithionite and sulfinate complexes from the reaction of SO2with decamethylsamarocene
Klementyeva, Svetlana V.; Arleth, Nicholas; Meyer, Karsten; Konchenko, Sergey N.; Roesky, Peter W.; New J. Chem. 39 (2015) 7589–; doi:10.1039/C5NJ00318K

data_7054806
_publ_section_title
;
 Dithionite and sulfinate complexes from the reaction of SO2with
 decamethylsamarocene
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              7589
_journal_paper_doi               10.1039/C5NJ00318K
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C20 H30 O2 S Sm'
_chemical_formula_sum            'C20 H30 O2 S Sm'
_chemical_formula_weight         484.85
_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             2015-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_audit_update_record
;
2015-02-05 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.794(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5615(3)
_cell_length_b                   20.6022(9)
_cell_length_c                   11.7388(6)
_cell_measurement_temperature    100(2)
_cell_volume                     2033.92(16)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED & LANA, 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-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Dectris 100K Pilatus'
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'STOE STADI VARI'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_laue_measured_fraction_full 0.991
_diffrn_reflns_laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9662
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.120
_diffrn_reflns_theta_min         1.977
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_type              'Xenocs Genix3D Microfocus'
_exptl_absorpt_coefficient_mu    2.998
_exptl_absorpt_correction_T_max  0.8637
_exptl_absorpt_correction_T_min  0.7264
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-Red, X-Shape & LANA'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.054
_refine_diff_density_max         1.114
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3985
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0786P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3066
_reflns_number_total             3985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00318k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7054804--7054807.cif.'
_cod_database_code               7054806
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim C9A \\sim
C10A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C7A: within 1A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C11) = Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C16) =
Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C18A) = Uanis(C16A) =
Uanis(C20A) = Uanis(C17A) = Uanis(C19A) = Uanis(C11A) = Uanis(C15A) =
Uanis(C14A) = Uanis(C13A) = Uanis(C12A)
4. Others
 Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(C4A)=Sof(C5A)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=FVAR(1)
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(2)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(2)
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C17A)=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(3)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(3)
 Sof(C11A)=Sof(C15A)=Sof(C14A)=Sof(C13A)=Sof(C12A)=1-FVAR(4)
 Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=FVAR(4)
 Fixed Sof: S1(0.5) S2(0.5)
5.a Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,
 H7AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F),
 C18A(H18D,H18E,H18F), C16A(H16D,H16E,H16F), C20A(H20D,H20E,H20F), C17A(H17D,
 H17E,H17F), C19A(H19D,H19E,H19F)
;
_shelx_res_checksum              73640
_olex2_submission_special_instructions 'No special instructions were received'