Host–guest chemistry of NiII coordination compounds with PDC and (py)2CO: reversible crystal-to-amorphous transformations induced by solvent exchange
Calderón-Casado, Ainhoa; Barandika, Gotzone; Bazán, Begoña; Urtiaga, Miren-Karmele; Arriortua, María-Isabel; CrystEngComm 15 (2013) 5134–; doi:10.1039/c3ce40377g

data_7210798
_publ_section_title
;
 Host--guest chemistry of NiII coordination compounds with PDC and
 (py)2CO: reversible crystal-to-amorphous transformations induced by
 solvent exchange
;
_journal_issue                   25
_journal_name_full               CrystEngComm
_journal_page_first              5134
_journal_paper_doi               10.1039/c3ce40377g
_journal_volume                  15
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C18 H15 N3 Ni O7, 2(H2 O)'
_chemical_formula_sum            'C18 H19 N3 Ni O9'
_chemical_formula_weight         480.07
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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             2013-04-09T18:23:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.8410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.82970(10)
_cell_length_b                   7.41380(10)
_cell_length_c                   29.8081(4)
_cell_measurement_reflns_used    9070
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.9007
_cell_measurement_theta_min      2.9838
_cell_volume                     1937.39(4)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2012
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0314461
_diffrn_orient_matrix_UB_12      0.2040851
_diffrn_orient_matrix_UB_13      -0.0019758
_diffrn_orient_matrix_UB_21      -0.0074673
_diffrn_orient_matrix_UB_22      -0.0109523
_diffrn_orient_matrix_UB_23      -0.0518359
_diffrn_orient_matrix_UB_31      -0.1726881
_diffrn_orient_matrix_UB_32      0.0376046
_diffrn_orient_matrix_UB_33      -0.0044425
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            14756
_diffrn_reflns_theta_full        74.07
_diffrn_reflns_theta_max         74.07
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    1.991
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.1172
_exptl_crystal_size_mid          0.0499
_exptl_crystal_size_min          0.0363
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         3879
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0260P)^2^+4.4297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                3741
_reflns_number_total             3879
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3ce40377g.txt
_cod_data_source_block           '[Ni(dpk)(2,5-PDC)(H2O)]H2O'
_cod_database_code               7210798