The method for synthesis of 2-sulfonium closo-decaborate anions derivatives with exo-polyhedral aminogroups
Kubasov, A.S.; Turishev, E.S.; Golubev, A.V.; Bykov, A.Yu.; Zhizhin, K.Yu.; Kuznetsov, N.T.; Inorganica Chimica Acta 507 (2020) 119589–; doi:10.1016/j.ica.2020.119589

data_1564728
_publ_section_title
;
 The method for synthesis of 2-sulfonium closo-decaborate anions
 derivatives with exo-polyhedral aminogroups
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119589
_journal_paper_doi               10.1016/j.ica.2020.119589
_journal_volume                  507
_journal_year                    2020
_chemical_formula_moiety         '2(C24 H20 P), C9 H15 B10 N O2 S'
_chemical_formula_sum            'C57 H55 B10 N O2 P2 S'
_chemical_formula_weight         988.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 95.879(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.087(6)
_cell_length_b                   14.334(4)
_cell_length_c                   18.695(5)
_cell_measurement_reflns_used    2679
_cell_measurement_temperature    296
_cell_measurement_theta_max      25.546
_cell_measurement_theta_min      2.485
_cell_volume                     5354(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            93770
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.221
_diffrn_reflns_theta_min         2.007
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0402 before and 0.0332 after correction. The Ratio of minimum to maximum transmission is 0.9087. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       plate
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         11891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0887P)^2^+0.9967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1579
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8601
_reflns_number_total             11891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            19kub12_0m_a.cif
_cod_data_source_block           19kub12_0m_a
_cod_original_cell_volume        5355(3)
_cod_database_code               1564728
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.867
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C57(H57), C39(H39), C55(H55), C56(H56), C53(H53), C38(H38), C51(H51),
 C42(H42), C54(H54), C47(H47), C41(H41), C48(H48), C35(H35), C45(H45), C49(H49),
  C29(H29), C44(H44), C43(H43), C11(H11), C36(H36), C50(H50), C37(H37),
 C33(H33), C23(H23), C27(H27), C15(H15), C26(H26), C17(H17), C30(H30), C25(H25),
  C12(H12), C21(H21), C14(H14), C24(H24), C32(H32), C20(H20), C31(H31),
 C13(H13), C19(H19), C18(H18)
;