Synthesis, characterization, antioxidant and antidiabetic studies of Cu(II) and Zn(II) complexes of tolfenamic acid/mefenamic acid with 1-methylimidazole
Shamle, Nathaniel J.; Tella, Adedibu C.; Obaleye, Joshua A.; Balogun, Fatai O.; Ashafa, Anofi O.T.; Ajibade, Peter A.; Inorganica Chimica Acta 513 (2020) 119942–; doi:10.1016/j.ica.2020.119942

data_1564013
_publ_section_title
;
 Synthesis, characterization, antioxidant and antidiabetic studies of
 Cu(II) and Zn(II) complexes of tolfenamic acid/mefenamic acid with
 1-methylimidazole
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119942
_journal_paper_doi               10.1016/j.ica.2020.119942
_journal_volume                  513
_journal_year                    2020
_chemical_formula_moiety         'C38 H40 Cu N6 O4, H2 O'
_chemical_formula_sum            'C38 H42 Cu N6 O5'
_chemical_formula_weight         726.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                94.595(5)
_cell_angle_beta                 98.726(5)
_cell_angle_gamma                92.552(5)
_cell_formula_units_Z            1
_cell_length_a                   7.7814(9)
_cell_length_b                   7.8017(8)
_cell_length_c                   14.9217(16)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    99.95
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.62
_cell_volume                     891.03(17)
_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-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.95
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15756
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.315
_diffrn_reflns_theta_min         1.386
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1199 before and 0.0281 after correction.
The Ratio of minimum to maximum transmission is 0.8477.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             381
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0635P)^2^+0.7987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4190
_reflns_number_total             4322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mo_pa_ns_143_a_0m.cif
_cod_data_source_block           mo_pa_ns_143_a_0m
_cod_database_code               1564013
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.625
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O3(0.5) H3B(0.5) H3C(0.5)
3.a Free rotating group:
 O3(H3B,H3C)
3.b Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C9(H9), C11(H11), C3(H3A), C2(H2), C10(H10), C14(H14), C8(H8),
 C16(H16), C15(H15)
;
_shelx_res_checksum              38673
_shelx_hkl_checksum              60586
_olex2_submission_special_instructions 'No special instructions were received'