Synthesis and characterization a series of Norfloxacin-transition metal complexes
Huang, Yan-Ju; Zhang, Jun; Inorganica Chimica Acta 501 (2020) 119244–; doi:10.1016/j.ica.2019.119244

data_1565611
_publ_section_title
;
 Synthesis and characterization a series of Norfloxacin-transition metal
 complexes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119244
_journal_paper_doi               10.1016/j.ica.2019.119244
_journal_volume                  501
_journal_year                    2020
_chemical_formula_moiety         '4(C32 H40 F2 Fe N6 O8), 4(O4 S), 21(H2 O)'
_chemical_formula_sum            'C128 H202 F8 Fe4 N24 O69 S4'
_chemical_formula_weight         3684.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 101.727(3)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   12.612(2)
_cell_length_b                   24.924(5)
_cell_length_c                   13.540(2)
_cell_measurement_reflns_used    15733
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.271
_cell_measurement_theta_min      3.172
_cell_volume                     4167.3(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1481
_diffrn_reflns_av_unetI/netI     0.2038
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15689
_diffrn_reflns_point_group_measured_fraction_full 0.733
_diffrn_reflns_point_group_measured_fraction_max 0.698
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.271
_diffrn_reflns_theta_min         3.172
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs,bruker(2008)
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1930
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.64(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         7190
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.2147
_refine_ls_R_factor_gt           0.0822
_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^)+(0.1060P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.2326
_reflns_Friedel_coverage         0.442
_reflns_Friedel_fraction_full    0.470
_reflns_Friedel_fraction_max     0.428
_reflns_number_gt                3016
_reflns_number_total             7190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-501-119244.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_cell_volume        4167.3(13)
_cod_original_sg_symbol_H-M      'C  c '
_cod_database_code               1565611
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.36(8)
 0.64(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C15)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O19(0.5) H19A(0.5) H19B(0.5) O18(0.5) H18A(0.5) H18B(0.5) O16(0.5)
 H16C(0.5) H16D(0.5) O13(0.75) H13C(0.75) H13D(0.75)
5.a Riding coordinates:
 N6(H6A,H6B), O7(H7A,H7B), N3(H3A,H3B), C14(H14A,H14B), C30(H30A,H30B),
 O17(H17A,H17B), O14(H14C,H14D), O15(H15C,H15D), O19(H19A,H19B), O18(H18A,H18B),
  O16(H16C,H16D), O13(H13C,H13D)
5.b Rotating group:
 O8(H8A,H8B)
5.c Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C23(H23A,H23B), C29(H29A,H29B), C15(H15A,H15B), C31(H31A,
 H31B), C7(H7C,H7D), C13(H13A,H13B), C32(H32A,H32B)
5.d Aromatic/amide H refined with riding coordinates:
 C28(H28), C22(H22), C25(H25), C9(H9), C12(H12), C6(H6)
5.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C8(H8C,H8D,H8E)
;
_shelx_res_checksum              20198
_shelx_hkl_checksum              85409
_olex2_submission_special_instructions 'No special instructions were received'