Crystal structures of sulfonamide protected bicyclic guanidines: (<i>S</i>)-8-{[(<i>tert</i>-butyl-dimethyl-sil-yl)-oxy]meth-yl}-1-[(2,2,4,6,7-penta-methyl-2,3-di-hydro-benzo-furan-5-yl)sulfon-yl]-1,3,4,6,7,8-hexa-hydro-2<i>H</i>-pyrimido[1,2-<i>a</i>]pyrimidin-1-ium tri-fluoro-methane-sulfonate and (<i>S</i>)-8-(iodo-meth-yl)-1-tosyl-1,3,4,6,7,8-hexa-hydro-2<i>H</i>-pyrimido[1,2-<i>a</i>]pyrimidin-1-ium iodide.
Alaboosh, Jamal M. H.; Hill, Steven P.; Kariuki, Benson M.; Redman, James E.; Acta crystallographica. Section E, Crystallographic communications 80 (2024) 305–309; doi:10.1107/S2056989024001129

data_2023041
_publ_section_title
;
 Crystal structures of sulfonamide protected bicyclic guanidines:
 (<i>S</i>)-8-{[(<i>tert</i>-butyl-dimethyl-sil-yl)-oxy]meth-yl}-1-[(2,2,4,6,7-penta-methyl-2,3-di-hydro-benzo-furan-5-yl)sulfon-yl]-1,3,4,6,7,8-hexa-hydro-2<i>H</i>-pyrimido[1,2-<i>a</i>]pyrimidin-1-ium
 tri-fluoro-methane-sulfonate and
 (<i>S</i>)-8-(iodo-meth-yl)-1-tosyl-1,3,4,6,7,8-hexa-hydro-2<i>H</i>-pyrimido[1,2-<i>a</i>]pyrimidin-1-ium
 iodide.
;
_journal_coeditor_code           DJ2073
_journal_issue                   'Pt 3'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              305
_journal_page_last               309
_journal_paper_doi               10.1107/S2056989024001129
_journal_volume                  80
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C27 H46 N3 O4 S Si +, C F3 O3 S -'
_chemical_formula_moiety         'C27 H46 N3 O4 S Si +, C F3 O3 S -'
_chemical_formula_sum            'C28 H46 F3 N3 O7 S2 Si'
_chemical_formula_weight         685.89
_chemical_name_common
'(<i>S</i>)-8-{[(<i>tert</i>-Butyldimethylsilyl)oxy]methyl}-1-[(2,2,4,6,7-pentamethyl-2,3-dihydrobenzofuran-5-yl)sulfonyl]-1,3,4,6,7,8-hexahydro-2<i>H</i>-pyrimido[1,2-<i>a</i>]pyrimidin-1-ium triflate'
_chemical_name_systematic
'(<i>S</i>)-8-{[(<i>tert</i>-Butyldimethylsilyl)oxy]methyl}-1-[(2,2,4,6,7-pentamethyl-2,3-dihydrobenzofuran-5-yl)sulfonyl]-1,3,4,6,7,8-hexahydro-2<i>H</i>-pyrimido[1,2-<i>a</i>]pyrimidin-1-ium trifluoromethanesulfonate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 96.052(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5784(3)
_cell_length_b                   14.4797(5)
_cell_length_c                   13.6961(5)
_cell_measurement_reflns_used    3508
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.7650
_cell_measurement_theta_min      4.4120
_cell_volume                     1691.75(10)
_computing_cell_refinement
;
CrysAlisPro (Agilent, 2014)
;
_computing_data_collection
;
CrysAlisPro (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlisPro (Agilent, 2014)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
<i>SHELXL2018/1</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10136
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.830
_diffrn_reflns_theta_min         4.457
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.317
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Agilent,2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.475
_refine_ls_abs_structure_details
;
 Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.39(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5593
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0537P)^2^+0.4930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                5350
_reflns_number_total             5593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dj2073sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 2023041--2023042.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2023041
_cod_database_fobs_code          2023041
_shelx_estimated_absorpt_t_min   0.515
_shelx_estimated_absorpt_t_max   0.919
_shelx_hkl_checksum              53901
_shelx_res_checksum              52580