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_7055663
_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         'Cl O4, C27 H34 N O6 S, C4 H8 O2, 3(H2 O)'
_chemical_formula_sum            'C31 H48 Cl N O15 S'
_chemical_formula_weight         742.21
_chemical_name_systematic
'2-[(E)-2-(2,3,5,6,8,9,11,12,14,15-decahydro-1,4,7,10,13,16-benzohexaoxacyclooctadecin-18-yl)vinyl]-3-ethyl-1,3-benzothiazol-3-ium perchlorate, dioxane and water solvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_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                100.100(2)
_cell_angle_beta                 100.108(2)
_cell_angle_gamma                93.581(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9257(5)
_cell_length_b                   11.4270(7)
_cell_length_c                   19.6257(10)
_cell_measurement_reflns_used    894
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.886
_cell_measurement_theta_min      2.266
_cell_volume                     1714.75(18)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART-6K'
_diffrn_measurement_method       /W
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.1229
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10164
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.499
_diffrn_reflns_theta_min         1.819
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         8476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0520P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4386
_reflns_number_total             8476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03500g2.cif
_cod_data_source_block           dye_2c
_cod_depositor_comments
'Adding full bibliography for 7055662--7055666.cif.'
_cod_original_cell_volume        1714.74(17)
_cod_database_code               7055663
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              24946
_solvent_exptl_crystal_recrystallization_method 'MeCN, benzene, dioxane'