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_1564729
_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         'C20 H25 B10 N2 O4 S, C16 H36 N'
_chemical_formula_sum            'C36 H61 B10 N3 O4 S'
_chemical_formula_weight         740.03
_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   geom
_cell_angle_alpha                90
_cell_angle_beta                 111.673(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9294(12)
_cell_length_b                   17.0837(11)
_cell_length_c                   20.1140(15)
_cell_measurement_reflns_used    2750
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.44
_cell_volume                     4767.4(6)
_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      296.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.970
_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  0.0929
_diffrn_reflns_av_unetI/netI     0.1446
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24187
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.891
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0953 before and 0.0545 after correction. The Ratio of minimum to maximum transmission is 0.8577. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.031
_exptl_crystal_description       plate
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         9086
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.2300
_refine_ls_R_factor_gt           0.1130
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1958P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2983
_refine_ls_wR_factor_ref         0.3731
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3150
_reflns_number_total             9086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            19kub41_0m_a.cif
_cod_data_source_block           19kub41_0m_a
_cod_database_code               1564729
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.921
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-C21B = N3-C33B = N3-C25B = N3-C21 = N3-C25
 1.55 with sigma of 0.02
 N3-C33
 1.5 with sigma of 0.02
 C34-C33
 1.55 with sigma of 0.02
 C34-C35
 1.55 with sigma of 0.02
 C35-C36
 1.55 with sigma of 0.02
 C35B-C36B
 1.55 with sigma of 0.02
 C27B-C26B = C27B-C28B
 1.55 with sigma of 0.02
 C27-C28 = C27-C26
 1.55 with sigma of 0.02
 C26-C25 = C26-C27
 1.55 with sigma of 0.02
 C26B-C27B = C26B-C25B
 1.55 with sigma of 0.02
 C22B-C21B
 1.55 with sigma of 0.02
 C23-C22B = C23-C24
 1.55 with sigma of 0.02
 C22B-C21B = C22B-C23
 1.55 with sigma of 0.02
 C22-C21
 1.55 with sigma of 0.02
 C23B-C24B
 1.55 with sigma of 0.02
 C35B-C34B = C35B-C36B
 1.52 with sigma of 0.02
 C29-N3 = C29-C30B
 1.52 with sigma of 0.02
 C30-C29
 1.52 with sigma of 0.02
 C29-N3 = C29-C30
 1.52 with sigma of 0.02
 C31-C30
 1.52 with sigma of 0.02
 C32-C31
 1.52 with sigma of 0.02
 C31B-C30B
 1.52 with sigma of 0.02
 C29B-N3 = C29B-C30B
 1.52 with sigma of 0.02
 C30B-C29B = C30B-C31B
 1.52 with sigma of 0.02
 C32B-C31B
 1.52 with sigma of 0.02
 C29-C31
 2.48 with sigma of 0.02
 C30-C32
 2.48 with sigma of 0.02
 C29B-C31B
 2.48 with sigma of 0.02
 C30B-C32B
 2.48 with sigma of 0.02
 C26-C28
 2.48 with sigma of 0.02
 C21-C23
 2.48 with sigma of 0.02
 C22-N3
 2.48 with sigma of 0.02
 C22-C24
 2.48 with sigma of 0.02
 C34-C36
 2.48 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C35) = Uanis(C35B)
Uanis(C33B) = Uanis(C33)
Uanis(C36B) = Uanis(C36)
Uanis(C34B) = Uanis(C34)
Uanis(C25B) = Uanis(C25)
Uanis(C26B) = Uanis(C26)
Uanis(C27B) = Uanis(C27)
Uanis(C28B) = Uanis(C28)
Uanis(C21) = Uanis(C21B)
Uanis(C22B) = Uanis(C22)
Uanis(C24) = Uanis(C23B)
Uanis(C23) = Uanis(C23B)
Uanis(C24) = Uanis(C24B)
Uanis(C32B) = Uanis(C32)
Uanis(C31) = Uanis(C31B)
Uanis(C30) = Uanis(C30B)
Uanis(C23) = Uanis(C27)
Uanis(C23B) = Uanis(C35B)
Uanis(C23) = Uanis(C35)
Uanis(C32) = Uanis(C24)
Uanis(C32B) = Uanis(C24B)
Uanis(C31) = Uanis(C27)
Uanis(C31B) = Uanis(C27B)
Uanis(C30B) = Uanis(C22B)
4. Others
 Fixed Sof: C21B(0.666) H21A(0.666) H21B(0.666) C26B(0.6666) H26A(0.6666)
 H26B(0.6666) C22(0.33333) H22A(0.33333) H22B(0.33333) C27B(0.6666)
 H27A(0.6666) H27B(0.6666) C33B(0.66667) H33A(0.66667) H33B(0.66667)
 C28B(0.6666) H28A(0.6666) H28B(0.6666) H28C(0.6666) C25B(0.6666) H25A(0.6666)
 H25B(0.6666) C21(0.33333) H21C(0.33333) H21D(0.33333) C23B(0.66666)
 H23A(0.66666) H23B(0.66666) C25(0.33333) H25C(0.33333) H25D(0.33333)
 C34B(0.66667) H34A(0.66667) H34B(0.66667) C35B(0.66667) H35A(0.66667)
 H35B(0.66667) C36B(0.66667) H36A(0.66667) H36B(0.66667) H36C(0.66667)
 C33(0.33333) H33C(0.33333) H33D(0.33333) C34(0.33333) H34C(0.33333)
 H34D(0.33333) C35(0.33333) H35C(0.33333) H35D(0.33333) C36(0.33333)
 H36D(0.33333) H36E(0.33333) H36F(0.33333) C28(0.33333) H28D(0.33333)
 H28E(0.33333) H28F(0.33333) C27(0.33333) H27C(0.33333) H27D(0.33333)
 C26(0.33333) H26C(0.33333) H26D(0.33333) C22B(0.6666) H22C(0.6666)
 H22D(0.6666) C24(0.3333) H24A(0.3333) H24B(0.3333) H24C(0.3333) C23(0.3333)
 H23C(0.3333) H23D(0.3333) C24B(0.66666) H24D(0.66666) H24E(0.66666)
 H24F(0.66666) C29B(0.66666) H29A(0.66666) H29B(0.66666) C30B(0.66667)
 H30A(0.66667) H30B(0.66667) C31B(0.66667) H31A(0.66667) H31B(0.66667)
 C29(0.33333) H29C(0.33333) H29D(0.33333) C30(0.33333) H30C(0.33333)
 H30D(0.33333) C31(0.33333) H31C(0.33333) H31D(0.33333) C32B(0.6666)
 H32A(0.6666) H32B(0.6666) H32C(0.6666) C32(0.33333) H32D(0.33333)
 H32E(0.33333) H32F(0.33333)
 Fixed X: C22(0.87501) C23B(0.881961) C22B(0.853001) C24(0.83191) C23(0.90418)
 C24B(0.87739)
 Fixed Y: C22(0.57352) C23B(0.628761) C22B(0.542689) C24(0.661751)
 C23(0.64259) C24B(0.68773)
 Fixed Z: C22(0.739539) C23B(0.71885) C22B(0.703589) C24(0.631921)
 C23(0.709049) C24B(0.661251)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C11(H11A,H11B), C1(H1A,H1B), C12(H12A,H12B), C21B(H21A,H21B),
 C26B(H26A,H26B), C22(H22A,H22B), C27B(H27A,H27B), C33B(H33A,H33B), C25B(H25A,
 H25B), C21(H21C,H21D), C23B(H23A,H23B), C25(H25C,H25D), C34B(H34A,H34B),
 C35B(H35A,H35B), C33(H33C,H33D), C34(H34C,H34D), C35(H35C,H35D), C27(H27C,
 H27D), C26(H26C,H26D), C22B(H22C,H22D), C23(H23C,H23D), C29B(H29A,H29B),
 C30B(H30A,H30B), C31B(H31A,H31B), C29(H29C,H29D), C30(H30C,H30D), C31(H31C,
 H31D)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C5(H5A), C18(H18), C16(H16), C17(H17), C8(H8), C6(H6A), C7(H7A)
5.c Idealised Me refined as rotating group:
 C28B(H28A,H28B,H28C), C36B(H36A,H36B,H36C), C36(H36D,H36E,H36F), C28(H28D,
 H28E,H28F), C24(H24A,H24B,H24C), C24B(H24D,H24E,H24F), C32B(H32A,H32B,H32C),
 C32(H32D,H32E,H32F)
5.d Boron cage BH refined with riding coordinates:
 B9(H9), B5(H5), B6(H6), B1(H1), B7(H7), B3(H3), B8(H8A), B4(H4), B10(H10)
;
_shelx_res_checksum              87768
_shelx_hkl_checksum              70082
_shelx_fab_checksum              21429
_olex2_submission_special_instructions 'No special instructions were received'