Crystal structure of (3<i>E</i>,5<i>E</i>)-3,5-bis[4-(diethylazaniumyl)benzylidene]-1-methyl-4-oxopiperidin-1-ium trichloride dihydrate: a potential biophotonic material
Nesterov, Volodymyr V.; Zakharov, Lev N.; Nesterov, Vladimir N.; Shulaev, Vladimir; Acta Crystallographica Section E 71 (2015) 1513–1515; doi:10.1107/S2056989015020952

data_2241339
_publ_section_title
;
 Crystal structure of
 (3<i>E</i>,5<i>E</i>)-3,5-bis[4-(diethylazaniumyl)benzylidene]-1-methyl-4-oxopiperidin-1-ium
 trichloride dihydrate: a potential biophotonic material
;
_journal_coeditor_code           HB7503
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1513
_journal_page_last               1515
_journal_paper_doi               10.1107/S2056989015020952
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C28 H40 N3 O 3+, 3Cl -, 2H2 O'
_chemical_formula_moiety         'C28 H40 N3 O 3+, 3(Cl -), 2(H2 O)'
_chemical_formula_sum            'C28 H44 Cl3 N3 O3'
_chemical_formula_weight         577.01
_chemical_name_systematic
;(3<i>E</i>,5<i>E</i>)-3,5-Bis[4-(diethylazaniumyl)benzylidene]-1-methyl-
4-oxopiperidin-1-ium
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.7590(10)
_cell_angle_beta                 110.7950(10)
_cell_angle_gamma                102.7330(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0933(5)
_cell_length_b                   12.0661(6)
_cell_length_c                   13.7576(6)
_cell_measurement_reflns_used    4567
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.47
_cell_volume                     1485.46(12)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11768
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  0.9666
_exptl_absorpt_correction_T_min  0.9410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2007)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.620
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5787
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0910P)^2^+1.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                5056
_reflns_number_total             5787
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7503sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-11-23
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_cod_database_code               2241339
_cod_database_fobs_code          2241339