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_7247401
_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         'C12 H7 O4, C10 H9 N2 O2 S, 2(H2 O)'
_chemical_formula_sum            'C22 H20 N2 O8 S'
_chemical_formula_weight         472.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-03-02
_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                90.00
_cell_angle_beta                 101.670(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.989(3)
_cell_length_b                   7.8780(19)
_cell_length_c                   19.624(5)
_cell_measurement_reflns_used    9429
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.79
_cell_volume                     2118.0(9)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0592
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37149
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.33
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6599
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
? was used for absorption correction.
wR2(int) was 0.1431 before and 0.0598 after correction.
The Ratio of minimum to maximum transmission is 0.8849.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         5265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0544P)^2^+1.5502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1466
_reflns_number_gt                3537
_reflns_number_total             5265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3ce00650f2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7247401--7247405.cif.'
_cod_database_code               7247401
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H21 of C21, {H3A,H3B} of C3, H6 of C6, {H2A,H2B} of C2, H20 of C20, H4 of
  C4, H19 of C19, H14 of C14, H5 of C5, H7 of C7, H13 of C13, H22 of C22
 At 1.5 times of:
  H5A of O5, {H8A,H8B} of O8, H1 of O1, {H7A,H7B} of O7
2.a Free rotating group:
 O8(H8A,H8B), O7(H7A,H7B)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C5(H5), C7(H7), C13(H13), C22(H22), C6(H6), C19(H19), C4(H4),
 C21(H21), C20(H20)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O5(H5A)
;