Synthesis, crystal structure and NMR investigation of novel Ca(II) complexes with heterocyclic alcohol, aldehyde and carboxylate ligands. Evaluation of Ca(II) and Cd(II) analogues for anticancer activity
Barbara Barszcz; Joanna Masternak; Maciej Hodorowicz; Ewa Matczak-Jon; Agnieszka Jablonska-Wawrzycka; Katarzyna Stadnicka; Malgorzata Zienkiewicz; Karolina Krolewska; Julia Kazmierczak-Baranska; Inorganica Chimica Acta 399 (2013) 85–94; doi:

data_1516861
_publ_section_title
;
 Synthesis, crystal structure and NMR investigation of novel Ca(II)
 complexes with heterocyclic alcohol, aldehyde and carboxylate ligands.
 Evaluation of Ca(II) and Cd(II) analogues for anticancer activity
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              85
_journal_page_last               94
_journal_volume                  399
_journal_year                    2013
_chemical_formula_moiety         '(C5 H6 N2 O)2, (Ca 2+), (N O3 1-)2'
_chemical_formula_sum            'C10 H12 Ca N6 O8'
_chemical_formula_weight         384.34
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                82.762(3)
_cell_angle_beta                 83.740(3)
_cell_angle_gamma                85.249(2)
_cell_formula_units_Z            2
_cell_length_a                   7.0216(4)
_cell_length_b                   7.6611(4)
_cell_length_c                   14.6518(9)
_cell_measurement_reflns_used    1936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     775.31(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep3 (Farrugia, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (ALTOMARE et al., 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f and \o scans to fill Ewald sphere'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4738
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.462
_exptl_absorpt_correction_T_max  0.9174
_exptl_absorpt_correction_T_min  0.8739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.841
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.841
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0999P)^2^+1.8797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1549
_reflns_number_gt                2685
_reflns_number_total             3483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-399-85-94-2.cif
_cod_data_source_block           Ca-4Me
_cod_database_code               1516861