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_7055662
_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         '2(Cl O4), C16 H19 N3 O2, 0.25(H2 O)'
_chemical_formula_sum            'C16 H19.5 Cl2 N3 O10.25'
_chemical_formula_weight         488.74
_chemical_name_systematic
'1-(3-ammoniopropyl)-4-[(E)-2-(4-nitrophenyl)vinyl]pyridinium diperchlorate, hydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.3977(5)
_cell_length_b                   8.3891(3)
_cell_length_c                   29.1772(9)
_cell_measurement_reflns_used    1623
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.55
_cell_measurement_theta_min      3.25
_cell_volume                     4013.7(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Bruker PROTEUM-2'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.907
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11130
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        57.296
_diffrn_reflns_theta_max         57.295
_diffrn_reflns_theta_min         3.029
_exptl_absorpt_coefficient_mu    3.501
_exptl_absorpt_correction_T_max  0.9658
_exptl_absorpt_correction_T_min  0.6787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       plate
_exptl_crystal_F_000             2020
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         2475
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0588
_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^)+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1891
_reflns_number_total             2475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03500g2.cif
_cod_data_source_block           dye_1f
_cod_depositor_comments
'Adding full bibliography for 7055662--7055666.cif.'
_cod_original_formula_sum        'C16 H19.50 Cl2 N3 O10.25'
_cod_database_code               7055662
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.679
_shelx_estimated_absorpt_t_max   0.966
_shelx_res_checksum              79327
_solvent_exptl_crystal_recrystallization_method 'MeCN, benzene'