Schiff Base Driven Denticity-Fluctuated Structural Assortment of Zinc-pseudohalide Complexes: Synthesis, Structures and Electrical Transport Properties
Mudi, Prafullya Kumar; Singla, Labhini; Chamuah, Anil; Bhattacharya, Sanjib; Roychoudhury, Angshuman; Biswas, Bhaskar; CrystEngComm  (2022) –; doi:10.1039/D1CE01646F

data_7244474
_publ_section_title
;
 Schiff Base Driven Denticity-Fluctuated Structural Assortment of
 Zinc-pseudohalide Complexes: Synthesis, Structures and Electrical
 Transport Properties
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01646F
_journal_year                    2022
_chemical_formula_moiety         'C32 H30 N4 O6 S2 Zn'
_chemical_formula_sum            'C32 H30 N4 O6 S2 Zn'
_chemical_formula_weight         696.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-05 deposited with the CCDC.	2022-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.591(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.3897(8)
_cell_length_b                   10.8311(4)
_cell_length_c                   18.4897(7)
_cell_measurement_reflns_used    8657
_cell_measurement_temperature    296.0(2)
_cell_measurement_theta_max      23.6430
_cell_measurement_theta_min      2.5150
_cell_volume                     6486.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_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_temperature      296.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.945
_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    -69.00 118.20   0.30   11.00    --   29.89  54.00 -30.00  624
  2  \w    -69.00 118.20   0.30   11.00    --   29.89  54.00  30.00  624
  3  \w    -69.00 113.10   0.30   11.00    --   29.89  54.00 150.00  607
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0214536000
_diffrn_orient_matrix_UB_12      0.0032900000
_diffrn_orient_matrix_UB_13      -0.0078484000
_diffrn_orient_matrix_UB_21      -0.0040384000
_diffrn_orient_matrix_UB_22      -0.0400977000
_diffrn_orient_matrix_UB_23      0.0294418000
_diffrn_orient_matrix_UB_31      -0.0017564000
_diffrn_orient_matrix_UB_32      0.0516657000
_diffrn_orient_matrix_UB_33      0.0233115000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            45356
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.774
_diffrn_reflns_theta_min         2.548
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         11348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0775P)^2^+2.4387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5927
_reflns_number_total             11348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01646f2.cif
_cod_data_source_block           zn-p11-nscn_rt
_cod_database_code               7244474
_shelx_shelxl_version_number     2018/1
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C23(H23), C8(H8), C14(H14), C29(H29), C20(H20), C7(H7),
 C13(H13), C22(H22), C11(H11), C28(H28), C21(H21), C12(H12), C26(H26), C6(H6),
 C27(H27), C5(H5)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C30(H30A,H30B,H30C), C1(H1A,H1B,H1C), C15(H15A,H15B,H15C)
;
_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 1.064
_oxdiff_exptl_absorpt_empirical_full_min 0.954