Synthesis and structures of 5-Nitro-salicylaldehyde thiosemicarbazonates of Copper(II) : molecular spectroscopy, ESI-mass, antimicrobial activity and cytotoxicity
Lobana, Tarlok Singh; Indoria, Shikha Indoria; Kaur, Harpreet; Arora, Daljit; Jassal, Amanpreet K.; Jasinski, Jerry P.; RSC Adv.  (2015) –; doi:10.1039/C4RA15006F

data_7219355
_publ_section_title
;
 Synthesis and structures of 5-Nitro-salicylaldehyde thiosemicarbazonates
 of Copper(II) : molecular spectroscopy, ESI-mass, antimicrobial activity
 and cytotoxicity
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA15006F
_journal_year                    2015
_chemical_formula_moiety         'C22 H18 Cu N6 O3 S'
_chemical_formula_sum            'C22 H18 Cu N6 O3 S'
_chemical_formula_weight         510.02
_chemical_name_systematic        'Compound 6'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/cc13ht6m
_audit_creation_date             2014-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2015-01-15 deposited with the CCDC.
2015-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                104.034(5)
_cell_angle_beta                 104.217(5)
_cell_angle_gamma                100.871(5)
_cell_formula_units_Z            2
_cell_length_a                   7.9073(4)
_cell_length_b                   11.5507(6)
_cell_length_c                   14.2629(8)
_cell_measurement_reflns_used    3286
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.4630
_cell_measurement_theta_min      4.0880
_cell_volume                     1181.69(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0416
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0000816000
_diffrn_orient_matrix_UB_12      -0.1168386000
_diffrn_orient_matrix_UB_13      -0.0798962000
_diffrn_orient_matrix_UB_21      -0.0158326000
_diffrn_orient_matrix_UB_22      0.0694086000
_diffrn_orient_matrix_UB_23      -0.0800425000
_diffrn_orient_matrix_UB_31      0.2077660000
_diffrn_orient_matrix_UB_32      0.0429606000
_diffrn_orient_matrix_UB_33      0.0297292000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7648
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.944
_diffrn_reflns_theta_min         3.355
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.434
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       plate
_exptl_crystal_F_000             522
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+0.8792P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3830
_reflns_number_total             4471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra15006f2.cif
_cod_data_source_block           jpl-89
_cod_database_code               7219355
_shelxl_version_number           2012-9
_chemical_oxdiff_formula         'C22 H26 N6 S O3 Cu'
_chemical_oxdiff_usercomment     'Lobana's JPL-89'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C2(H2), C4(H4), C6(H6), C7(H7), C13(H13), C14(H14), C15(H15),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;