Relationship between solid state structure and solution stability of copper(ii)‒hydroxypyridinecarboxylate complexes
May, Nóra V.; Gál, G. Tamás; Szentendrei, Zsolt; Korecz, László; May, Zoltán; Ferlin, Maria Grazia; Dean, Annalisa; Bombicz, Petra; Di Marco, Valerio B.; New Journal of Chemistry 43 (2019) 10699–; doi:10.1039/C9NJ01469A

data_1551257
_publ_section_title
;
 Relationship between solid state structure and solution stability of
 copper(ii)--hydroxypyridinecarboxylate complexes
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10699
_journal_paper_doi               10.1039/C9NJ01469A
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C54 H60 Cu3 N6 O24, 12(H2 O), 4(H O), 2(O)'
_chemical_formula_sum            'C54 H88 Cu3 N6 O42'
_chemical_formula_weight         1683.92
_chemical_name_systematic
'"'bis(\m2-4-hydroxy-1-(2-hydroxyethyl)-6-methyl-3-pyridinecarboxylato)-bis(\m2-4-hydroxy-1-(2-hydroxyethyl)-6-methyl-3-pyridinecarboxylato)-bis(\m2-4-hydroxy-1-(2-hydroxyethyl)-6-methyl-3-pyridinecarboxylato)-tri-copper(II) nonahydrate'"'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-05-15 deposited with the CCDC.    2019-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                98.9780(10)
_cell_angle_beta                 91.0710(10)
_cell_angle_gamma                113.1190(10)
_cell_formula_units_Z            1
_cell_length_a                   12.1956(4)
_cell_length_b                   12.4877(4)
_cell_length_c                   12.6185(5)
_cell_measurement_reflns_used    47047
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.04
_cell_volume                     1738.97(11)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'Mercury (Macrae, 2006)'
_computing_publication_material  'Spek, A.L. (2015). Acta Cryst. C71, 9-18.'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Sir2014 (Burla, 2015)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
 scan:  N=1,PHI=180.0,CHI=0.0,OMEGA=25.0,195.0,5.0,COUPLE=0.00                 
 scan:  N=2,PHI=270.0,CHI=45.0,OMEGA=26.0,216.0,5.0,COUPLE=0.00                
 scan:  N=3,PHI=90.0,CHI=45.0,OMEGA=25.0,225.0,5.0,COUPLE=0.00                 
 scan:  N=4,PHI=0.0,CHI=45.0,OMEGA=28.0,193.0,5.0,COUPLE=0.00                  
 scan:  N=5,PHI=180.0,CHI=45.0,OMEGA=60.0,200.0,5.0,COUPLE=0.00                
 scan:  N=6,PHI=90.0,CHI=0.0,OMEGA=100.0,200.0,5.0,COUPLE=0.00                 
 Orientation Matrix:
    UB11  0.0834 UB12  0.0623 UB13  0.0078
    UB21 -0.0006 UB22  0.0104 UB23  0.0802
    UB31  0.0325 UB32 -0.0620 UB33  0.0008
    Matrix type: 'd*Trek'
;
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID II.'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       RX
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            70996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.457
_diffrn_reflns_theta_min         3.034
_diffrn_source_current           40.0000
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.8784
_exptl_absorpt_correction_T_min  0.6660
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 T.Higashi, Numerical Absorption Correction, NUMABS, 2002
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             877
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         7929
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0558P)^2^+2.1123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6746
_reflns_number_total             7929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01469a2.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 1551256--1551260.cif.
;
_cod_database_code               1551257
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.785
_shelx_estimated_absorpt_t_max   0.785
_shelx_res_checksum              60148