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_7054807
_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         'C60 H90 O8 S4 Sm2, C7 H8'
_chemical_formula_sum            'C67 H98 O8 S4 Sm2'
_chemical_formula_weight         1460.39
_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             2015-01-20
_audit_creation_method
;
 ?
;
_audit_update_record
;
2015-02-05 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                76.608(2)
_cell_angle_beta                 72.242(2)
_cell_angle_gamma                74.217(2)
_cell_formula_units_Z            1
_cell_length_a                   11.8154(4)
_cell_length_b                   12.3472(4)
_cell_length_c                   12.4497(4)
_cell_measurement_temperature    100
_cell_volume                     1642.46(10)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'STOE STADI VARI'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17852
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.043
_diffrn_reflns_theta_min         1.741
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.949
_exptl_absorpt_correction_T_max  0.8300
_exptl_absorpt_correction_T_min  0.6834
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-Red, X-Shape'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       rod
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.104
_refine_diff_density_max         1.907
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6440
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0522P)^2^+2.0957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6131
_reflns_number_total             6440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00318k2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7054804--7054807.cif.'
_cod_database_code               7054807
_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. Restrained distances
 C32-C34
 1.4 with sigma of 0.02
 C34-C31
 2 with sigma of 0.02
 C33-C34 \\sim C34-C31
 with sigma of 0.02
 C33-C32 \\sim C32-C31
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C32) = Uanis(C34) = Uanis(C31)
4. Others
 Fixed Sof: C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C31(H31), C33(H33)
5.b 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), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C34(H34A,
 H34B,H34C)
;
_shelx_res_checksum              4672
_olex2_submission_special_instructions 'No special instructions were received'