Water-induced phase transformation of a CuIIcoordination framework with pyridine-2,5-dicarboxylate and di-2-pyridyl ketone: synchrotron radiation analysis
Llano-Tomé, Francisco; Bazán, Begoña; Urtiaga, M. Karmele; Barandika, Gotzone; Fidalgo-Marijuan, Arkaitz; Fernández de Luis, Roberto; Arriortua, María I.; CrystEngComm 17 (2015) 6346–; doi:10.1039/C5CE01033K

data_7221148
_publ_section_title
;
 Water-induced phase transformation of a CuIIcoordination framework with
 pyridine-2,5-dicarboxylate and di-2-pyridyl ketone: synchrotron radiation
 analysis
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              6346
_journal_paper_doi               10.1039/C5CE01033K
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C18 H15 Cu N3 O7'
_chemical_formula_sum            'C18 H15 Cu N3 O7'
_chemical_formula_weight         448.87
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-09-20T13:17:28-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-04-14 deposited with the CCDC.
2015-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.2953(2)
_cell_length_b                   17.2658(5)
_cell_length_c                   28.4236(7)
_cell_measurement_reflns_used    6323
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.2676
_cell_measurement_theta_min      2.557
_cell_volume                     3580.21(17)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    DIRDIF2008
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4023
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0517108
_diffrn_orient_matrix_UB_12      -0.0748877
_diffrn_orient_matrix_UB_13      0.0263172
_diffrn_orient_matrix_UB_21      0.0535302
_diffrn_orient_matrix_UB_22      -0.0381677
_diffrn_orient_matrix_UB_23      -0.0470545
_diffrn_orient_matrix_UB_31      0.1975231
_diffrn_orient_matrix_UB_32      0.0298886
_diffrn_orient_matrix_UB_33      0.0058811
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            19752
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    2.178
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.7996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_meas      1.65(2)
_exptl_crystal_density_method    Flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.0333
_exptl_crystal_size_mid          0.0329
_exptl_crystal_size_min          0.0195
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.855
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3272
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.855
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0918P)^2^+0.2767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                2699
_reflns_number_total             3272
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5ce01033k2.cif
_cod_data_source_block           fll129_2
_cod_depositor_comments
'Adding full bibliography for 7221148--7221149.cif.'
_cod_database_code               7221148