Development of copper(II)-diimine-iminodiacetate mixed ligand complexes as potential antitumor agents
Alvarez, Natalia; Mendes, Luis F.S.; Kramer, M. Gabriela; Torre, María H.; Costa-Filho, Antonio J.; Ellena, Javier; Facchin, Gianella; Inorganica Chimica Acta 483 (2018) 61–70; doi:10.1016/j.ica.2018.07.052

data_1563796
_publ_section_title
;
 Development of copper(II)-diimine-iminodiacetate mixed ligand complexes
 as potential antitumor agents
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              61
_journal_page_last               70
_journal_paper_doi               10.1016/j.ica.2018.07.052
_journal_volume                  483
_journal_year                    2018
_chemical_formula_sum            'C17 H19 Cu N3 O6'
_chemical_formula_weight         424.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 130.530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.310(7)
_cell_length_b                   17.940(6)
_cell_length_c                   14.663(9)
_cell_measurement_reflns_used    8574
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.9777
_cell_measurement_theta_min      3.6766
_cell_volume                     4261(3)
_computing_cell_refinement       'APEX2 v2014.5-0 (Bruker AXS)'
_computing_data_collection       'APEX2 v2014.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'BRUKER D8 venture diffractometer'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.915
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12630
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.446
_diffrn_reflns_theta_min         3.677
_diffrn_source                   'microfocused sealed tube'
_diffrn_source_type              'INCOATEC ICT-IMSB-HOUSING-L model D21502'
_exptl_absorpt_coefficient_mu    1.756
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.3806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       prism
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.105
_platon_squeeze_details
;
Crystallization was performed in water. 
The resulting electron density was largely uninterpretable, 
so it was removed with SQUEEZE in Platon (Spek, 2009).
Electron count and volume are consistent with 8 water molecules per void,
meaning two extra water molecules per assymetric unit. 
Also consistent with experimental elemental analysis of the sample.
;
_refine_diff_density_max         1.149
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.310
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.310
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2982
_refine_ls_wR_factor_ref         0.3158
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2767
_reflns_number_total             3556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mmc4.cif
_cod_data_source_block           cu_ida_4met_0ma_a_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_cell_volume        4260(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1563796
_shelx_shelxl_version_number     2014/7
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              1747
_shelx_hkl_checksum              59897
_shelx_fab_checksum              3739