Assembly of ZnII-coordination polymers constructed from benzothiadiazole functionalized bipyridines and V-shaped dicarboxylic acids: topology variety, photochemical and visible-light-driven photocatalytic properties
Song, Wei-Chao; Liang, Ling; Cui, Xun-Zhe; Wang, Xiu-Guang; Yang, En-Cui; Zhao, Xiao-Jun; CrystEngComm 20 (2018) 668–; doi:10.1039/C7CE01933E

data_7229827
_publ_section_title
;
 Assembly of ZnII-coordination polymers constructed from benzothiadiazole
 functionalized bipyridines and V-shaped dicarboxylic acids: topology
 variety, photochemical and visible-light-driven photocatalytic properties
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              668
_journal_paper_doi               10.1039/C7CE01933E
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         '0.25(C192 H128 N24 O32 S4 Zn8)'
_chemical_formula_sum            'C48 H32 N6 O8 S Zn2'
_chemical_formula_weight         983.59
_space_group_crystal_system      tetragonal
_space_group_IT_number           98
_space_group_name_Hall           'I 4bw 2bw'
_space_group_name_H-M_alt        'I 41 2 2'
_symmetry_space_group_name_Hall  'I 4bw 2bw'
_symmetry_space_group_name_H-M   'I 41 2 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-11-02 deposited with the CCDC.
2017-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.25176(16)
_cell_length_b                   16.25176(16)
_cell_length_c                   16.6475(3)
_cell_measurement_reflns_used    3074
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      73.7380
_cell_measurement_theta_min      5.4190
_cell_volume                     4396.93(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     36.00 120.00   1.00    1.00    --  107.08-125.00  30.00   84
  2  \w     83.00 159.00   1.00    1.00    --  107.08  30.00-120.00   76
  3  \w    108.00 145.00   1.00    1.00    --  107.08 125.00-120.00   37
  4  \w     85.00 115.00   1.00    1.00    --   41.49  38.00-120.00   30
  5  \w     17.00  44.00   1.00    1.00    --   41.49  38.00-120.00   27
  6  \w    -83.00  -4.00   1.00    1.00    --  -41.49 125.00 -90.00   79
  7  \w    113.00 139.00   1.00    1.00    --  107.08 106.00 133.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0912864000
_diffrn_orient_matrix_UB_12      -0.0239973000
_diffrn_orient_matrix_UB_13      -0.0086323000
_diffrn_orient_matrix_UB_21      0.0142936000
_diffrn_orient_matrix_UB_22      -0.0207811000
_diffrn_orient_matrix_UB_23      -0.0892172000
_diffrn_orient_matrix_UB_31      0.0211804000
_diffrn_orient_matrix_UB_32      -0.0893053000
_diffrn_orient_matrix_UB_33      0.0230586000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4515
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.048
_diffrn_reflns_theta_max         67.048
_diffrn_reflns_theta_min         3.801
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.307
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 750 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(3)
_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     236
_refine_ls_number_reflns         1970
_refine_ls_number_restraints     311
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+10.6617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.715
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                1871
_reflns_number_total             1970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01933e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7229827--7229830.cif.'
_cod_original_cell_volume        4396.93(12)
_cod_database_code               7229827
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 S1-N2 = S1-N3 = S1'-N2' = S1'-N3'
 1.61 with sigma of 0.01
 N2-N3 = N2'-N3'
 2.48 with sigma of 0.01
 N2-C14 = N2'-C14' = C15-N3 = C15'-N3'
 1.34 with sigma of 0.01
 S1-C15 = S1-C14 = S1'-C15' = S1'-C14'
 2.39 with sigma of 0.01
 N1-H1
 0.92 with sigma of 0.01
 C10-C11 = C10-C11'
 1.47 with sigma of 0.01
 C12-C13 = C12'-C13'
 1.45 with sigma of 0.01
 C11-C12 = C11'-C12'
 1.34 with sigma of 0.01
3. Restrained planarity
 S1, N2, N3, C12, C13, C14, C15, C16, C17, C18
 with sigma of 0.001
 S1', N2', N3', C12', C13', C14', C15', C16', C17', C18'
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
C11' \\sim S1' \\sim N2' \\sim N3' \\sim C12' \\sim C13' \\sim C14' \\sim C15'
\\sim C16' \\sim C17' \\sim C18': within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C11 \\sim S1 \\sim N2 \\sim N3 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim
C16 \\sim C17 \\sim C18: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C11') \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C12')
\\sim Ueq, Uanis(C13') \\sim Ueq, Uanis(C14') \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(N3') \\sim Ueq, Uanis(C15')
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(N2) \\sim Ueq, Uanis(C18') \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(C17')
\\sim Ueq, Uanis(C16') \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N2') \\sim Ueq,
Uanis(S1') \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C8) = Uanis(C8')
Uanis(C9) = Uanis(C9')
Uanis(N3) = Uanis(N3')
Uanis(N2) = Uanis(N2')
Uanis(S1) = Uanis(S1')
Uanis(C18) = Uanis(C18')
Uanis(C17) = Uanis(C17')
Uanis(C16) = Uanis(C16')
Uanis(C15) = Uanis(C15')
Uanis(C14) = Uanis(C14')
Uanis(C13) = Uanis(C13')
Uanis(C11) = Uanis(C11')
Uanis(C12) = Uanis(C12')
5. Others
 Sof(C9')=Sof(H9')=Sof(C8')=Sof(H8')=1-FVAR(1)
 Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=FVAR(1)
 Sof(C11')=Sof(H11')=Sof(C12')=Sof(H12')=0.5*(1-FVAR(3))
 Sof(S1')=Sof(N2')=Sof(N3')=Sof(C13')=Sof(C14')=Sof(C15')=Sof(C16')=Sof(C17')=
 Sof(H17')=Sof(C18')=Sof(H18')=0.25*(1-FVAR(3))
 Sof(S1)=Sof(N2)=Sof(N3)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=Sof(H17)=
 Sof(C18)=Sof(H18)=0.25*FVAR(3)
 Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=0.5*FVAR(3)
6.a Riding coordinates:
 C11(H11), C12(H12), C17(H17), C18(H18), C11'(H11'), C12'(H12'), C17'(H17'),
 C18'(H18')
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C6(H6), C4(H4), C9'(H9'), C8'(H8'), C8(H8), C9(H9)
6.c Fitted hexagon refined as free rotating group:
 C13(C14,C15,C16,C17,C18), C13'(C14',C15',C16',C17',C18')
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-12-02
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.255
_oxdiff_exptl_absorpt_empirical_full_min 0.848