Positional isomers of (E)-2-(anthracen-9-ylmethylene)-N-(aryl)hydrazinecarbothioamide, zinc complexes and polymorphic solvates
Nath, Jitendra; Baruah, Jubaraj B.; CrystEngComm 27 (2025) 46–54; doi:10.1039/D4CE00992D

data_7249631
_publ_section_title
;
 Positional isomers of
 (E)-2-(anthracen-9-ylmethylene)-N-(aryl)hydrazinecarbothioamide, zinc
 complexes and polymorphic solvates
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              46
_journal_page_last               54
_journal_paper_doi               10.1039/D4CE00992D
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C44 H28 Cl4 N6 S2 Zn, C H Cl3, 1.2[CHCl3]'
_chemical_formula_sum            'C46.2 H30.2 Cl10.6 N6 S2 Zn'
_chemical_formula_weight         1174.62
_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
_audit_creation_date             2024-07-02
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-09-28 deposited with the CCDC.	2024-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                105.037(19)
_cell_angle_beta                 97.95(2)
_cell_angle_gamma                103.998(19)
_cell_formula_units_Z            2
_cell_length_a                   9.909(5)
_cell_length_b                   15.867(9)
_cell_length_c                   18.059(10)
_cell_measurement_reflns_used    9307
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.23
_cell_measurement_theta_min      2.24
_cell_volume                     2599(2)
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25058
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.793
_diffrn_reflns_theta_max         24.793
_diffrn_reflns_theta_min         1.195
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       block
_exptl_crystal_F_000             1183
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         8862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1445P)^2^+0.5323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2175
_refine_ls_wR_factor_ref         0.2425
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5580
_reflns_number_total             8862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00992d2.cif
_cod_data_source_block           23Cl_ZnATUP1
_cod_depositor_comments
'Adding full bibliography for 7249627--7249635.cif.'
_cod_original_cell_volume        2599(3)
_cod_original_formula_sum        'C46.20 H30.20 Cl10.60 N6 S2 Zn'
_cod_database_code               7249631
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 C45(H45)
2.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N3(H3), C37(H37), C15(H15), C18(H18), C40(H40), C34(H34), C12(H12),
 C20(H20), C31(H31), C24(H24), C33(H33), C29(H29), C42(H42), C7(H7), C32(H32),
 C41(H41), C19(H19), C27(H27), C2(H2), C10(H10), C5(H5), C25(H25), C11(H11),
 C26(H26), C9(H9), C3(H3A), C4(H4)
;
_shelx_res_checksum              67498
_shelx_hkl_checksum              65237
_shelx_fab_checksum              77056
_platon_squeeze_special_details
;
A solvent mask was calculated and 142 electrons were 
found in a volume of 412\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.2[CHCl3] per Asymmetric Unit 
which account for 139 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'