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_1564727
_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         'C22 H20 B10 Cl9 N2 O4 S, C16 H36 N'
_chemical_formula_sum            'C40 H50 B10 Cl9 N0.5 O0.5 S'
_chemical_formula_weight         1005.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                80.395(2)
_cell_angle_beta                 89.953(2)
_cell_angle_gamma                60.9440(10)
_cell_formula_units_Z            2
_cell_length_a                   12.3454(5)
_cell_length_b                   12.4756(5)
_cell_length_c                   22.0778(9)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.462
_cell_measurement_theta_min      2.192
_cell_volume                     2918.0(2)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43567
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.879
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0843 before and 0.0576 after correction. The Ratio of minimum to maximum transmission is 0.8435. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       plate
_exptl_crystal_F_000             1033
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         13298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0617
_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^)+(0.1158P)^2^+0.6035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.2068
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8539
_reflns_number_total             13298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            19kbub41_0m_a.cif
_cod_data_source_block           19kbub41_0m_a
_cod_original_formula_sum        'C40 H50 B10 Cl9 N0.50 O0.50 S'
_cod_database_code               1564727
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.723
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.085) H1B(0.085) H2A(0.092) H2B(0.092) H3A(0.107) H3B(0.107)
 H6(0.129) H7(0.146) H8(0.153) H9(0.131) H12A(0.089) H12B(0.089) H13A(0.094)
 H13B(0.094) H14A(0.114) H14B(0.114) H17(0.134) H18(0.167) H19(0.19) H20(0.173)
 H23A(0.092) H23B(0.092) H24A(0.117) H24B(0.117) H25A(0.129) H25B(0.129)
 H26A(0.202) H26B(0.202) H26C(0.202) H27A(0.087) H27B(0.087) H28A(0.1)
 H28B(0.1) H29A(0.134) H29B(0.134) H30A(0.222) H30B(0.222) H30C(0.222)
 H31A(0.084) H31B(0.084) H32A(0.104) H32B(0.104) H33A(0.108) H33B(0.108)
 H34A(0.166) H34B(0.166) H34C(0.166) H35A(0.09) H35B(0.09) H36A(0.111)
 H36B(0.111) H37A(0.149) H37B(0.149) H38A(0.266) H38B(0.266) H38C(0.266)
 Fixed X: H1A(0.886875) H1B(0.805177) H2A(0.781254) H2B(0.685444)
 H3A(0.941132) H3B(0.85374) H6(0.90069) H7(0.746377) H8(0.585618) H9(0.553936)
 H12A(0.723723) H12B(0.851733) H13A(0.803481) H13B(0.66816) H14A(0.73815)
 H14B(0.876745) H17(0.633126) H18(0.765092) H19(0.971955) H20(1.06285)
 H23A(0.512644) H23B(0.398634) H24A(0.61125) H24B(0.499145) H25A(0.549101)
 H25B(0.662833) H26A(0.766406) H26B(0.70646) H26C(0.646681) H27A(0.308748)
 H27B(0.401231) H28A(0.17389) H28B(0.265659) H29A(0.13854) H29B(0.235326)
 H30A(0.040754) H30B(0.007825) H30C(0.105392) H31A(0.464086) H31B(0.537107)
 H32A(0.644485) H32B(0.580573) H33A(0.74026) H33B(0.679161) H34A(0.802273)
 H34B(0.891294) H34C(0.840185) H35A(0.260135) H35B(0.364015) H36A(0.186904)
 H36B(0.294027) H37A(0.108609) H37B(0.214389) H38A(0.131346) H38B(0.029716)
 H38C(0.030187)
 Fixed Y: H1A(0.040821) H1B(0.176467) H2A(0.097384) H2B(0.229574)
 H3A(0.146601) H3B(0.27376) H6(0.268034) H7(0.442036) H8(0.599519) H9(0.590499)
 H12A(-0.130377) H12B(-0.136626) H13A(-0.096376) H13B(-0.072872) H14A(-
 0.279105) H14B(-0.308186) H17(-0.225458) H18(-0.314706) H19(-0.420132) H20(-
 0.444657) H23A(0.586597) H23B(0.671235) H24A(0.698805) H24B(0.775402)
 H25A(0.592829) H25B(0.517808) H26A(0.605586) H26B(0.580482) H26C(0.715065)
 H27A(0.768624) H27B(0.631531) H28A(0.78323) H28B(0.643541) H29A(0.72235)
 H29B(0.582908) H30A(0.61238) H30B(0.718688) H30C(0.580183) H31A(0.825373)
 H31B(0.814012) H32A(0.595596) H32B(0.618129) H33A(0.706515) H33B(0.72368)
 H34A(0.483057) H34B(0.531311) H34C(0.559279) H35A(0.877249) H35B(0.91435)
 H36A(0.967203) H36B(1.000019) H37A(1.098649) H37B(1.132584) H38A(1.235391)
 H38B(1.284762) H38C(1.193573)
 Fixed Z: H1A(0.360287) H1B(0.321946) H2A(0.446633) H2B(0.408647) H3A(0.43814)
 H3B(0.393637) H6(0.663464) H7(0.701006) H8(0.637626) H9(0.536186)
 H12A(0.336564) H12B(0.350118) H13A(0.44883) H13B(0.435354) H14A(0.436694)
 H14B(0.435228) H17(0.676102) H18(0.76671) H19(0.76387) H20(0.673123)
 H23A(0.186069) H23B(0.219257) H24A(0.208459) H24B(0.245033) H25A(0.315567)
 H25B(0.279334) H26A(0.309149) H26B(0.368648) H26C(0.328226) H27A(0.057486)
 H27B(0.090197) H28A(0.133896) H28B(0.164054) H29A(0.045358) H29B(0.07254)
 H30A(0.07976) H30B(0.117384) H30C(0.146424) H31A(0.057467) H31B(0.118128)
 H32A(0.124561) H32B(0.058978) H33A(0.08326) H33B(0.017776) H34A(0.056562)
 H34B(0.074846) H34C(0.005742) H35A(0.17684) H35B(0.170631) H36A(0.076834)
 H36B(0.068314) H37A(0.147018) H37B(0.137179) H38A(0.042257) H38B(0.088592)
 H38C(0.047452)
;
_shelx_res_checksum              22394
_shelx_hkl_checksum              6087
_shelx_fab_checksum              13215
_olex2_submission_special_instructions 'No special instructions were received'