Five novel supramolecular assemblies constructed from the thiazolothiazole extended viologen moiety
Yang, Fengyi; Chen, Jiali; Wang, Junwen; Liu, Jinjian; CrystEngComm 25 (2023) 5461–5469; doi:10.1039/D3CE00650F

data_7247403
_publ_section_title
;
 Five novel supramolecular assemblies constructed from the
 thiazolothiazole extended viologen moiety
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              5461
_journal_page_last               5469
_journal_paper_doi               10.1039/D3CE00650F
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C10 H9 N2 O2 S, C5 H2 O4, C3 H7 N O, H2 O'
_chemical_formula_sum            'C18 H20 N3 O8 S'
_chemical_formula_weight         438.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-03-03
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_audit_update_record
;
2023-03-03 deposited with the CCDC.	2023-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                102.279(4)
_cell_angle_beta                 106.083(4)
_cell_angle_gamma                94.691(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4052(13)
_cell_length_b                   9.4814(14)
_cell_length_c                   13.366(2)
_cell_measurement_reflns_used    8481
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.22
_cell_volume                     988.8(3)
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14414
_diffrn_reflns_theta_full        28.40
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         2.22
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6274
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
? was used for absorption correction.
wR2(int) was 0.1391 before and 0.0453 after correction.
The Ratio of minimum to maximum transmission is 0.8414.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             458
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+0.3552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1327
_reflns_number_gt                4055
_reflns_number_total             4940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3ce00650f2.cif
_cod_data_source_block           a_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7247401--7247405.cif.'
_cod_database_code               7247403
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H5 of C5, {H2A,H2B} of C2, H4 of C4, H7 of C7, H18 of C18, {H3A,H3B} of C3,
  H6 of C6, H13 of C13
 At 1.5 times of:
  H1 of O1, {H17A,H17B,H17C} of C17, {H16A,H16B,H16C} of C16, {H8A,H8B} of O8
2.a Free rotating group:
 O8(H8A,H8B)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C13(H13), C6(H6), C4(H4), C18(H18), C7(H7)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;