Copper complexes for the promotion of iminopyridine ligands derived from β-alanine and self-aldol additions: Relaxivity and cytotoxic properties
Alvarez-Miguel, Lucia; Álvarez-Miguel, Ines; Martín Álvarez, Jose Miguel; Alvarez, Celedonio M.; Rogez, Guillaume; García-Rodríguez, Raúl; Miguel, Daniel; Dalton Transactions  (2019) –; doi:10.1039/C9DT03822A

data_7701882
_publ_section_title
;
 Copper complexes for the promotion of iminopyridine ligands derived from
 \b-alanine and self-aldol additions: Relaxivity and cytotoxic properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03822A
_journal_year                    2019
_chemical_formula_moiety         'C11 H13 Cu N3 O3 S'
_chemical_formula_sum            'C11 H13 Cu N3 O3 S'
_chemical_formula_weight         330.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2019-09-24 deposited with the CCDC.	2019-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.857(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8730(3)
_cell_length_b                   14.0579(6)
_cell_length_c                   12.7811(5)
_cell_measurement_reflns_used    2172
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      28.5994
_cell_measurement_theta_min      2.1519
_cell_volume                     1411.38(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      297.15
_diffrn_detector_area_resol_mean 10.4757
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_details
;
  1 omega   68.00  114.00   1.0000   39.7700
omega____ theta____ kappa____ phi______ frames
    -       21.5439  151.0000  -23.0000 46

  2 omega  -23.00  118.00   1.0000   39.7700
omega____ theta____ kappa____ phi______ frames
    -       21.5439   77.0000    0.0000 141

  3 omega   70.00  108.00   1.0000   39.7700
omega____ theta____ kappa____ phi______ frames
    -       21.5439   77.0000   90.0000 38
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0393148000
_diffrn_orient_matrix_UB_12      -0.0350870000
_diffrn_orient_matrix_UB_13      -0.0332835000
_diffrn_orient_matrix_UB_21      -0.0479785000
_diffrn_orient_matrix_UB_22      0.0358869000
_diffrn_orient_matrix_UB_23      -0.0274830000
_diffrn_orient_matrix_UB_31      0.0654432000
_diffrn_orient_matrix_UB_32      0.0052177000
_diffrn_orient_matrix_UB_33      -0.0351841000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5953
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.662
_diffrn_reflns_theta_min         2.156
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.701
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       prism
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.2069
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.0687
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0406P)^2^+0.3543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2356
_reflns_number_total             3187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03822a2.cif
_cod_data_source_block           Compound_9_dm266a
_cod_database_code               7701882
_chemical_oxdiff_formula         C10H9Cl1Cu1N3O2S1
_reflns_odcompleteness_completeness 99.90
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C16(H16)
2.c Tetrahedral OH refined with riding coordinates:
 O30(H30)
2.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              65686
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'