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_7054805
_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         'C80 H120 O12 S6 Sm4, 2(C7 H8)'
_chemical_formula_sum            'C94 H136 O12 S6 Sm4'
_chemical_formula_weight         2251.78
_chemical_name_systematic
;
 ?
;
_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
;
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                97.595(16)
_cell_angle_beta                 101.297(15)
_cell_angle_gamma                112.448(15)
_cell_formula_units_Z            1
_cell_length_a                   12.415(2)
_cell_length_b                   12.471(3)
_cell_length_c                   17.870(3)
_cell_measurement_temperature    100
_cell_volume                     2441.3(9)
_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                 'image plate (34 cm diameter)'
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1539
_diffrn_reflns_av_unetI/netI     0.1583
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28810
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.815
_diffrn_source                   'sealed X-ray tube, 12x0.4mm LFF'
_exptl_absorpt_coefficient_mu    2.554
_exptl_absorpt_correction_T_max  0.7880
_exptl_absorpt_correction_T_min  0.4968
_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    1.532
_exptl_crystal_description       prism
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.073
_refine_diff_density_max         4.480
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.335
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9596
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0867
_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^)+(0.1192P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2163
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5647
_reflns_number_total             9596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00318k2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7054804--7054807.cif.'
_cod_database_code               7054805
_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
 C47-C41
 1.4 with sigma of 0.02
3. Rigid bond restraints
 C41
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Aromatic/amide H refined with riding coordinates:
 C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
6.b Fitted hexagon refined as free rotating group:
 C41(C42,C43,C44,C45,C46)
6.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C), C36(H36A,H36B,
 H36C), C40(H40A,H40B,H40C), C28(H28A,H28B,H28C), C16(H16A,H16B,H16C), C39(H39A,
 H39B,H39C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C19(H19A,H19B,H19C),
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C37(H37A,H37B,H37C), C1A(H1AA,H1AB,H1AC), C2(H2A,H2B,H2C), C18(H18A,H18B,H18C),
  C6(H6A,H6B,H6C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              40948
_olex2_submission_special_instructions 'No special instructions were received'