Synthesis and crystal growth of thienyl-substituted pyridinium derivatives for second-order nonlinear optics
Dai, Yiqiang; Tan, Jifeng; Ye, Ning; Yang, Zhou; CrystEngComm 16 (2014) 636–; doi:10.1039/c3ce41938j

data_7213605
_publ_section_title
;
 Synthesis and crystal growth of thienyl-substituted pyridinium
 derivatives for second-order nonlinear optics
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              636
_journal_paper_doi               10.1039/c3ce41938j
_journal_volume                  16
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C14 H17 N2 S, C6 H4 N O5 S, H2 O'
_chemical_formula_sum            'C20 H23 N3 O6 S2'
_chemical_formula_weight         465.53
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-20
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                104.448(5)
_cell_angle_beta                 108.242(5)
_cell_angle_gamma                96.225(4)
_cell_formula_units_Z            1
_cell_length_a                   7.5719(4)
_cell_length_b                   7.8718(4)
_cell_length_c                   9.8803(6)
_cell_measurement_reflns_used    3200
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.2651
_cell_measurement_theta_min      2.8868
_cell_volume                     530.37(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9877
_diffrn_measurement_details
;
  1 omega   69.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       13.7753  178.0000  120.0000 35

  2 omega   72.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       13.7753  178.0000  -30.0000 32

  3 omega  -23.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566   19.0000 -150.0000 89

  4 omega  -92.00  -56.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  178.0000 -150.0000 36

  5 omega  -19.00   26.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000   90.0000 45

  6 omega  -93.00    6.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -19.0000   30.0000 99
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0579319000
_diffrn_orient_matrix_UB_12      -0.0619317000
_diffrn_orient_matrix_UB_13      0.0181835000
_diffrn_orient_matrix_UB_21      0.0161700000
_diffrn_orient_matrix_UB_22      0.0389528000
_diffrn_orient_matrix_UB_23      0.0768564000
_diffrn_orient_matrix_UB_31      -0.0807971000
_diffrn_orient_matrix_UB_32      -0.0606355000
_diffrn_orient_matrix_UB_33      -0.0064808000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3739
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         2616
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0336P)^2^+0.1354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0687
_reflns_number_gt                2554
_reflns_number_total             2616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41938j.txt
_cod_data_source_block           exp_425
_cod_original_cell_volume        530.37(5)
_cod_database_code               7213605
_chemical_oxdiff_formula         C20H20N3O5S2
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42