Synthesis, structure, and stereospecific cross-[2+2] photocycloaddition of pseudodimeric complexes based on ammonioalkyl derivatives of styryl dyes
Gromov, Sergey P.; Vedernikov, Artem I.; Sazonov, Sergey K.; Kuz’mina, Lyudmila G.; Lobova, Natalia A.; Strelenko, Yuri A.; Howard, Judith A. K.; New J. Chem. 40 (2016) 7542–; doi:10.1039/C5NJ03500G

data_7055664
_publ_section_title
;
 Synthesis, structure, and stereospecific cross-[2+2] photocycloaddition
 of pseudodimeric complexes based on ammonioalkyl derivatives of styryl
 dyes
;
_journal_issue                   9
_journal_name_full               'New J. Chem.'
_journal_page_first              7542
_journal_paper_doi               10.1039/C5NJ03500G
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety
'6(Cl O4), 2(C25 H34 N O6), 2(C17 H22 N2 S), 1.4(C6 H6), 1.4(H2 O)'
_chemical_formula_sum            'C46.2 H61.6 Cl3 N3 O18.7 S'
_chemical_formula_weight         1096.59
_chemical_name_systematic
'complex between 1-(3-ammoniopropyl)-4-{(E)-2-[4-(methylthio)-phenyl]vinyl}pyridinium diperchlorate and 4-[(E)-2-(2,3,5,6,8,9,11,12,14,15-decahydro-1,4,7,10,13,16-benzohexaoxacyclooctadecin-18-yl)vinyl]-1-ethylpyridiniumperchlorate, benzene and water solvate'
_chemical_properties_physical    ', Air-sensitive,Light-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-15 deposited with the CCDC.
2016-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.404(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   37.878(8)
_cell_length_b                   16.492(3)
_cell_length_c                   35.710(7)
_cell_measurement_reflns_used    4167
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      18.000
_cell_measurement_theta_min      2.111
_cell_volume                     21399(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       /W
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2225
_diffrn_reflns_av_unetI/netI     0.2262
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            100229
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.035
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             9222
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.285
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         23352
_refine_ls_number_restraints     3580
_refine_ls_restrained_S_all      1.520
_refine_ls_R_factor_all          0.3957
_refine_ls_R_factor_gt           0.1843
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4584
_refine_ls_wR_factor_ref         0.5145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6415
_reflns_number_total             23352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03500g2.cif
_cod_data_source_block           complex_1d-2a
_cod_depositor_comments
'Adding full bibliography for 7055662--7055666.cif.'
_cod_original_cell_volume        21399(8)
_cod_original_formula_sum        'C46.20 H61.60 Cl3 N3 O18.70 S'
_cod_database_code               7055664
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.895
_shelx_estimated_absorpt_t_max   0.956
_shelx_res_checksum              89443
_solvent_exptl_crystal_recrystallization_method 'MeCN, benzene'