Copper(ii) complexes based on levofloxacin and 2N-donor ligands: synthesis, crystal structures and in vitro biological evaluation
Kumar, Manish; Kumar, Gyanendra; Dadure, Kanhaiya M.; Masram, Dhanraj T.; New Journal of Chemistry 43 (2019) 15462–; doi:10.1039/C9NJ03178B

data_7058845
_publ_section_title
;
 Copper(ii) complexes based on levofloxacin and 2N-donor ligands:
 synthesis, crystal structures and in vitro biological evaluation
;
_journal_issue                   38
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15462
_journal_paper_doi               10.1039/C9NJ03178B
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C28 H29 Cl Cu F N6 O4, 2(Cl)'
_chemical_formula_sum            'C28 H29 Cl3 Cu F N6 O4'
_chemical_formula_weight         702.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-08-13 deposited with the CCDC.    2019-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.078(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1992(16)
_cell_length_b                   13.4765(11)
_cell_length_c                   15.5358(17)
_cell_measurement_reflns_used    6281
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.3200
_cell_measurement_theta_min      3.4490
_cell_volume                     3099.7(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9853
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -84.00   5.00   1.00    4.50    --  -15.17 -77.00 -60.00   89
  2  \w    -13.00  21.00   1.00    4.50    --  -15.17 -99.00   0.00   34
  3  \w    -84.00  10.00   1.00    4.50    --  -15.17 -77.00 120.00   94
  4  \w     23.00  87.00   1.00    4.50    --   19.00  57.00  30.00   64
  5  \w    -24.00  59.00   1.00    4.50    --   19.00 -99.00-180.00   83
  6  \w    -49.00  37.00   1.00    4.50    --   19.00 -57.00  60.00   86
  7  \w    -49.00  37.00   1.00    4.50    --   19.00 -57.00-120.00   86
  8  \w     22.00  87.00   1.00    4.50    --   19.00  57.00-150.00   65
  9  \w    -18.00  64.00   1.00    4.50    --   19.00-107.00  17.49   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0141435000
_diffrn_orient_matrix_UB_12      0.0127335000
_diffrn_orient_matrix_UB_13      -0.0391075000
_diffrn_orient_matrix_UB_21      -0.0048922000
_diffrn_orient_matrix_UB_22      -0.0502483000
_diffrn_orient_matrix_UB_23      -0.0138941000
_diffrn_orient_matrix_UB_31      -0.0455075000
_diffrn_orient_matrix_UB_32      0.0090631000
_diffrn_orient_matrix_UB_33      -0.0217966000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41879
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.310
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         6335
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0589P)^2^+3.9256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4140
_reflns_number_total             6335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03178b2.cif
_cod_data_source_block           levobipyamr-3
_cod_depositor_comments
'Adding full bibliography for 7058845--7058846.cif.'
_cod_database_code               7058845
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C28 H28 Cl Cu F N6 O4'
_chemical_oxdiff_usercomment     17-05-2018
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.914
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 N3-H3
 0.94 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C1) \\sim
Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 N4, C21, O4, C30A, C23, C15, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O4, N4, C15, C30B, C29, C22, C16, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: C30B(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C23(0.5) H23(0.5) C29(0.5)
 H29(0.5) C21(0.5) H21A(0.5) H21B(0.5) C22(0.5) H22A(0.5) H22B(0.5) C30A(0.5)
 H30D(0.5) H30E(0.5) H30F(0.5) Cl5(0.6666) Cl6(0.3333)
6.a Ternary CH refined with riding coordinates:
 N6(H6), C23(H23), C29(H29)
6.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C24(H24A,H24B), C27(H27A,H27B), C21(H21A,
 H21B), C22(H22A,H22B)
6.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C16(H16), C10(H10), C7(H7), C4(H4), C8(H8), C9(H9), C1(H1), C2(H2),
 C3(H3A)
6.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30B(H30A,H30B,H30C), C30A(H30D,H30E,H30F)
;
_shelx_res_checksum              30106
_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 1.276
_oxdiff_exptl_absorpt_empirical_full_min 0.852