The effect of halides and coordination mode of 4-amino-2,1,3-benzothiadiazole on the luminescence properties of its Zn complexes
Pylova, Ekaterina Konstantinovna; Khisamov, Radmir M.; Bashirov, Denis Aleksandrovich; Sukhikh, Taisiya Sergeevna; Konchenko, Sergey Nikolaevich; CrystEngComm  (2022) –; doi:10.1039/D2CE01215D

data_7245700
_publ_section_title
;
 The effect of halides and coordination mode of
 4-amino-2,1,3-benzothiadiazole on the luminescence properties of its Zn
 complexes
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01215D
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         '3(C2 H1.667 I0.667 N S0.333 Zn0.333)'
_chemical_formula_sum            'C6 H5 I2 N3 S Zn'
_chemical_formula_weight         470.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-10-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2022-03-23 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.846(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   14.5782(6)
_cell_length_b                   32.4028(12)
_cell_length_c                   7.0488(3)
_cell_measurement_reflns_used    4329
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.35
_cell_volume                     3312.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8493
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.380
_diffrn_reflns_theta_min         1.538
_diffrn_source                   'sealed tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.964
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0931 before and 0.0573 after correction. The Ratio of minimum to maximum transmission is 0.6788. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.830
_exptl_crystal_description       prism
_exptl_crystal_F_000             2568
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.357
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.271
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.37(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5020
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+131.1360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1527
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4320
_reflns_number_total             5020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01215d2.cif
_cod_data_source_block           ts225d_sc
_cod_database_code               7245700
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.503
_shelx_estimated_absorpt_t_min   0.299
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.63(7)
 0.37(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(I221) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(S312) \\sim Ueq, Uanis(N311) \\sim Ueq, Uanis(N313) \\sim Ueq,
Uanis(N314) \\sim Ueq, Uanis(C311) \\sim Ueq, Uanis(C312) \\sim Ueq,
Uanis(C314) \\sim Ueq, Uanis(C315) \\sim Ueq, Uanis(C316) \\sim Ueq,
Uanis(C317) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uiso(C111) = Uiso(C117) = Uiso(C116) = Uiso(C115) = Uiso(C114) = Uiso(C112) =
Uiso(C211) = Uiso(C217) = Uiso(C216) = Uiso(C215) = Uiso(C214) = Uiso(C212) =
Uiso(N221) = Uiso(N223) = Uiso(S222) = Uiso(N111) = Uiso(N113) = Uiso(S112)
Uiso(S122) = Uiso(N121) = Uiso(N123) = Uiso(N124) = Uiso(C121) = Uiso(C122) =
Uiso(C124) = Uiso(C125) = Uiso(C126) = Uiso(C127) = Uiso(S212) = Uiso(N211) =
Uiso(N213) = Uiso(N214) = Uiso(C211) = Uiso(C212) = Uiso(C214) = Uiso(C215) =
Uiso(C216) = Uiso(C217)
4. Rigid body (RIGU) restrains
 S312, N311, N313, C311, C312, C314, C315, C316, C317
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(I211)=Sof(I212)=Sof(I221)=Sof(I222)=Sof(Zn21)=Sof(Zn22)=Sof(S212)=
 Sof(S222)=Sof(N211)=Sof(N213)=Sof(N214)=Sof(H21A)=Sof(H21B)=Sof(N221)=
 Sof(N223)=Sof(N224)=Sof(H22A)=Sof(H22B)=Sof(C211)=Sof(C212)=Sof(C214)=
 Sof(C215)=Sof(H215)=Sof(C216)=Sof(H216)=Sof(C217)=Sof(H217)=Sof(C221)=
 Sof(C222)=Sof(C224)=Sof(C225)=Sof(H225)=Sof(C226)=Sof(H226)=Sof(C227)=
 Sof(H227)=1-FVAR(1)
 Sof(I111)=Sof(I112)=Sof(I121)=Sof(I122)=Sof(Zn11)=Sof(Zn12)=Sof(S112)=
 Sof(S122)=Sof(N111)=Sof(N113)=Sof(N114)=Sof(H11A)=Sof(H11B)=Sof(N121)=
 Sof(N123)=Sof(N124)=Sof(H12A)=Sof(H12B)=Sof(C111)=Sof(C112)=Sof(C114)=
 Sof(C115)=Sof(H115)=Sof(C116)=Sof(H116)=Sof(C117)=Sof(H117)=Sof(C121)=
 Sof(C122)=Sof(C124)=Sof(C125)=Sof(H125)=Sof(C126)=Sof(H126)=Sof(C127)=
 Sof(H127)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 N314(H31A,H31B), N114(H11A,H11B), N124(H12A,H12B), N214(H21A,H21B), N224(H22A,
 H22B)
6.b Aromatic/amide H refined with riding coordinates:
 C315(H315), C316(H316), C317(H317), C115(H115), C116(H116), C117(H117),
 C125(H125), C126(H126), C127(H127), C215(H215), C216(H216), C217(H217),
 C225(H225), C226(H226), C227(H227)
;
_shelx_res_checksum              1547
_shelx_hkl_checksum              42310
_olex2_submission_special_instructions 'No special instructions were received'