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_7210796
_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         'C19 H17 N3 Ni O7, C O'
_chemical_formula_sum            'C20 H17 N3 Ni O8'
_chemical_formula_weight         486.08
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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             2013-04-15T08:55:36-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                97.46(2)
_cell_angle_beta                 99.97(3)
_cell_angle_gamma                109.71(3)
_cell_formula_units_Z            2
_cell_length_a                   8.230(3)
_cell_length_b                   10.540(4)
_cell_length_c                   14.140(3)
_cell_measurement_reflns_used    1662
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.3633
_cell_measurement_theta_min      2.0919
_cell_volume                     1113.6(7)
_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      298(2)
_diffrn_detector_area_resol_mean 16.2439
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0164804
_diffrn_orient_matrix_UB_12      -0.0073683
_diffrn_orient_matrix_UB_13      0.0495217
_diffrn_orient_matrix_UB_21      -0.0737628
_diffrn_orient_matrix_UB_22      -0.0632001
_diffrn_orient_matrix_UB_23      -0.0121663
_diffrn_orient_matrix_UB_31      0.0561113
_diffrn_orient_matrix_UB_32      -0.0357918
_diffrn_orient_matrix_UB_33      -0.0102568
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1091
_diffrn_reflns_av_unetI/netI     0.1244
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5671
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.1
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.33333
_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            purple
_exptl_crystal_density_diffrn    1.45
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.354
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3825
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0717
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1093P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.2121
_reflns_number_gt                2617
_reflns_number_total             3825
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3ce40377g.txt
_cod_data_source_block           '[Ni(dpk)(2,5-PDC)(MeOH)]MeOH'
_cod_original_cell_volume        1113.6(6)
_cod_database_code               7210796