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_7058846
_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         'C42 H36 Cl Cu F N5 O4, 2(Cl)'
_chemical_formula_sum            'C42 H36 Cl3 Cu F N5 O4'
_chemical_formula_weight         863.65
_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_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                101.577(8)
_cell_angle_beta                 108.055(8)
_cell_angle_gamma                94.122(8)
_cell_formula_units_Z            2
_cell_length_a                   12.5234(11)
_cell_length_b                   13.0688(14)
_cell_length_c                   13.2794(12)
_cell_measurement_reflns_used    4798
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.9380
_cell_measurement_theta_min      3.5090
_cell_volume                     2003.2(4)
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9853
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     -9.00  79.00   1.00    7.50    --   19.00  77.00  90.00   88
  2  \w      1.00  83.00   1.00    7.50    --   19.00  57.00   0.00   82
  3  \w      0.00  87.00   1.00    7.50    --   19.00  57.00 -90.00   87
  4  \w    -24.00  59.00   1.00    7.50    --   19.00 -99.00 -60.00   83
  5  \w    -17.00  61.00   1.00    7.50    --   19.00-102.00  47.00   78
  6  \w    -18.00  64.00   1.00    7.50    --   19.00-107.00 134.89   82
  7  \w    -34.00  53.00   1.00    7.50    --  -15.17  57.00-150.00   87
  8  \w    -84.00   3.00   1.00    7.50    --  -15.17 -38.00 120.00   87
;
_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      -0.0011345000
_diffrn_orient_matrix_UB_12      -0.0081903000
_diffrn_orient_matrix_UB_13      -0.0547839000
_diffrn_orient_matrix_UB_21      0.0259556000
_diffrn_orient_matrix_UB_22      0.0528669000
_diffrn_orient_matrix_UB_23      0.0105986000
_diffrn_orient_matrix_UB_31      0.0542907000
_diffrn_orient_matrix_UB_32      -0.0164939000
_diffrn_orient_matrix_UB_33      0.0150539000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_unetI/netI     0.0911
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25673
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         3.425
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59595
_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            'bluish green'
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.396
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         7574
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1396
_refine_ls_R_factor_gt           0.0998
_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^)+(0.1696P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2569
_refine_ls_wR_factor_ref         0.2935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4854
_reflns_number_total             7574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03178b2.cif
_cod_data_source_block           levocubatho
_cod_depositor_comments
'Adding full bibliography for 7058845--7058846.cif.'
_cod_original_cell_volume        2003.2(3)
_cod_database_code               7058846
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C42 H35 Cl Cu F N5 O4 '
_chemical_oxdiff_usercomment     26-04-2018
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.932
_reflns_odcompleteness_completeness 99.77
_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
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 H33A, C43, H43B, C44, H43A, H44A, H43C, H44B, C33, O4, N3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: H33(0.5) H33A(0.5) C32(0.5) H32A(0.5) H32B(0.5) C34(0.5) H34A(0.5)
 H34B(0.5) H34C(0.5) C44(0.5) H44A(0.5) H44B(0.5) C43(0.5) H43A(0.5) H43B(0.5)
 H43C(0.5) Cl3(0.5) Cl1(0.5)
6.a Ternary CH refined with riding coordinates:
 C33(H33), C33(H33A), N5(H5)
6.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C38(H38A,H38B), C40(H40A,H40B), C39(H39A,H39B), C41(H41A,
 H41B), C44(H44A,H44B)
6.c Me refined with riding coordinates:
 C42(H42A,H42B,H42C)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C30(H30), C18(H18), C7(H7), C11(H11), C35(H35), C12(H12),
 C1(H1), C14(H14), C15(H15), C20(H20), C17(H17), C21(H21), C24(H24), C16(H16),
 C22(H22), C23(H23)
6.e Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              83424
_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 1.320
_oxdiff_exptl_absorpt_empirical_full_min 0.742