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_7701875
_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         'C14 H16 Cl2 Cu2 N2 O4'
_chemical_formula_sum            'C14 H16 Cl2 Cu2 N2 O4'
_chemical_formula_weight         474.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-08
_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                 95.417(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6181(5)
_cell_length_b                   4.0692(2)
_cell_length_c                   19.2298(9)
_cell_measurement_reflns_used    1344
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.5720
_cell_measurement_theta_min      3.5570
_cell_volume                     827.15(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_details
;
  1 omega  -62.00  -26.00   1.0000   23.5900
omega____ theta____ kappa____ phi______ frames
    -      -19.7470   77.0000   30.0000 36

  2 omega   -2.00  122.00   1.0000   23.5900
omega____ theta____ kappa____ phi______ frames
    -       21.5439   77.0000  -90.0000 124

  3 omega  -21.00   40.00   1.0000   23.5900
omega____ theta____ kappa____ phi______ frames
    -       21.5439   77.0000 -180.0000 61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0159378000
_diffrn_orient_matrix_UB_12      -0.1560832000
_diffrn_orient_matrix_UB_13      0.0129803000
_diffrn_orient_matrix_UB_21      -0.0647195000
_diffrn_orient_matrix_UB_22      0.0298960000
_diffrn_orient_matrix_UB_23      -0.0107664000
_diffrn_orient_matrix_UB_31      0.0077291000
_diffrn_orient_matrix_UB_32      -0.0711847000
_diffrn_orient_matrix_UB_33      -0.0330327000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3121
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.398
_diffrn_reflns_theta_min         2.111
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.915
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_description       needle
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.3014
_exptl_crystal_size_mid          0.0974
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0361P)^2^+0.8501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1417
_reflns_number_total             1840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03822a2.cif
_cod_data_source_block           Compound_7_lam387c
_cod_database_code               7701875
_chemical_oxdiff_formula         'C7 H8 Cl1 Cu1 N1 O2'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2.a Ternary CH refined with riding coordinates:
 C16(H16)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              88604
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'