#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:31:59 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180438 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/07/7210796.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7210796
loop_
_publ_author_name
'Calderón-Casado, Ainhoa'
'Barandika, Gotzone'
'Bazán, Begoña'
'Urtiaga, Miren-Karmele'
'Arriortua, María-Isabel'
_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
_chemical_name_systematic
;
?
;
_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       'ω 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/[σ²(Fo²)+(0.1093P)²+0.0000P] where P=(Fo²+2Fc²)/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     >2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.03946(9) 0.15483(6) 0.32681(5) 0.0330(3) Uani 1 1 d .
O5 O 0.2287(5) 0.2649(3) 0.2536(3) 0.0370(9) Uani 1 1 d D
O3 O -0.1673(6) -0.1771(3) -0.0661(3) 0.0504(12) Uani 1 1 d .
O1 O -0.1273(6) 0.0775(4) 0.4103(3) 0.0455(11) Uani 1 1 d .
O4 O -0.2948(6) -0.3920(3) -0.0478(3) 0.0504(12) Uani 1 1 d .
O7 O 0.2147(7) 0.0656(5) 0.3870(3) 0.0581(13) Uani 1 1 d D
O2 O -0.3275(5) -0.1214(4) 0.4222(3) 0.0469(11) Uani 1 1 d .
O6 O 0.3245(7) 0.4935(4) 0.2327(4) 0.0689(16) Uani 1 1 d D
N3 N 0.1715(6) 0.3422(4) 0.4237(3) 0.0361(11) Uani 1 1 d U
N1 N -0.1168(6) -0.0309(4) 0.2313(3) 0.0338(11) Uani 1 1 d .
N2 N -0.0967(6) 0.2611(4) 0.2510(3) 0.0382(12) Uani 1 1 d U
C4 C -0.2338(7) -0.2122(4) 0.0859(4) 0.0296(12) Uani 1 1 d .
C5 C -0.1206(7) -0.0799(5) 0.1381(4) 0.0324(13) Uani 1 1 d .
H5 H -0.0444 -0.0233 0.1064 0.039 Uiso 1 1 calc R
C3 C -0.3518(4) -0.2932(2) 0.1323(2) 0.0381(14) Uani 1 1 d .
H3 H -0.4285 -0.3817 0.1006 0.046 Uiso 1 1 calc R
C14 C 0.2437(4) 0.4440(2) 0.3800(2) 0.0408(15) Uani 1 1 d RU
C1 C -0.2342(4) -0.1118(2) 0.2746(2) 0.0350(13) Uani 1 1 d R
C15 C 0.3313(4) 0.5792(2) 0.4293(2) 0.066(2) Uani 1 1 d RU
H15 H 0.3781 0.6482 0.3958 0.079 Uiso 1 1 d R
C18 C 0.3479(4) 0.6097(2) 0.5300(2) 0.078(3) Uani 1 1 d RU
H18 H 0.4091 0.6992 0.5655 0.094 Uiso 1 1 d R
C7 C -0.2310(7) -0.2647(5) -0.0174(4) 0.0341(13) Uani 1 1 d .
C8 C -0.2737(9) 0.2290(7) 0.2183(5) 0.0557(17) Uani 1 1 d U
H8 H -0.3515 0.1529 0.235 0.067 Uiso 1 1 calc R
C12 C 0.0124(9) 0.3711(5) 0.2252(4) 0.0447(16) Uani 1 1 d U
C13 C 0.2077(8) 0.3965(5) 0.2695(4) 0.0403(15) Uani 1 1 d .
C2 C -0.3540(8) -0.2404(5) 0.2267(4) 0.0394(14) Uani 1 1 d .
H2 H -0.4364 -0.2918 0.2578 0.047 Uiso 1 1 calc R
C6 C -0.2314(7) -0.0474(5) 0.3766(4) 0.0343(13) Uani 1 1 d .
C11 C -0.0491(6) 0.4499(4) 0.1674(3) 0.066(2) Uani 1 1 d U
H11 H 0.0299 0.5255 0.1509 0.079 Uiso 1 1 calc R
C17 C 0.2702(6) 0.5051(4) 0.5754(3) 0.067(2) Uani 1 1 d RU
H17 H 0.2767 0.523 0.6424 0.081 Uiso 1 1 d R
C16 C 0.1837(6) 0.3721(4) 0.5202(3) 0.0513(17) Uani 1 1 d RU
H16 H 0.1336 0.3012 0.5514 0.062 Uiso 1 1 d R
C10 C -0.2315(14) 0.4132(8) 0.1348(6) 0.084(3) Uani 1 1 d U
H10 H -0.2764 0.4632 0.0951 0.101 Uiso 1 1 calc R
C9 C -0.3438(12) 0.3028(9) 0.1620(6) 0.075(2) Uani 1 1 d U
H9 H -0.4661 0.2781 0.1424 0.09 Uiso 1 1 calc R
C19 C 0.2654(15) -0.0395(11) 0.3496(7) 0.121(4) Uani 1 1 d .
H19A H 0.3501 -0.0518 0.3999 0.182 Uiso 1 1 calc R
H19B H 0.3182 -0.0163 0.2956 0.182 Uiso 1 1 calc R
H19C H 0.1632 -0.1233 0.3273 0.182 Uiso 1 1 calc R
O8 O 0.345(2) -0.0347(15) 0.0952(12) 0.258(6) Uiso 1 1 d .
C30 C 0.274(2) -0.1597(16) 0.0636(12) 0.169(6) Uiso 1 1 d .
H5H H 0.23(2) 0.238(14) 0.196(5) 0.253 Uiso 1 1 d D
H7H H 0.264(19) 0.088(15) 0.447(3) 0.253 Uiso 1 1 d D
H6H H 0.319(16) 0.456(10) 0.174(4) 0.16(5) Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 Ni1 N3 94.53(15)
O1 Ni1 N1 81.60(15)
N3 Ni1 N1 174.21(17)
O1 Ni1 O7 91.45(19)
N3 Ni1 O7 93.9(2)
N1 Ni1 O7 90.53(19)
O1 Ni1 N2 100.18(18)
N3 Ni1 N2 84.67(18)
N1 Ni1 N2 91.76(18)
O7 Ni1 N2 168.35(17)
O1 Ni1 O5 171.45(14)
N3 Ni1 O5 77.00(15)
N1 Ni1 O5 106.77(14)
O7 Ni1 O5 90.28(18)
N2 Ni1 O5 78.13(16)
C13 O5 Ni1 99.5(3)
C6 O1 Ni1 114.5(3)
C19 O7 Ni1 133.4(5)
C14 N3 C16 118.3(4)
C14 N3 Ni1 113.0(3)
C16 N3 Ni1 128.6(3)
C5 N1 C1 117.5(4)
C5 N1 Ni1 131.7(3)
C1 N1 Ni1 110.8(3)
C12 N2 C8 117.0(5)
C12 N2 Ni1 112.8(4)
C8 N2 Ni1 130.0(4)
C3 C4 C5 117.8(4)
C3 C4 C7 120.3(4)
C5 C4 C7 121.9(4)
N1 C5 C4 123.4(4)
C4 C3 C2 118.8(3)
N3 C14 C15 123.2(2)
N3 C14 C13 112.3(3)
C15 C14 C13 124.32(18)
N1 C1 C2 122.2(3)
N1 C1 C6 114.9(3)
C2 C1 C6 122.8(3)
C14 C15 C18 118.6
C17 C18 C15 118.49(19)
O4 C7 O3 125.6(5)
O4 C7 C4 117.2(4)
O3 C7 C4 117.2(4)
N2 C8 C9 123.5(6)
N2 C12 C11 122.7(6)
N2 C12 C13 111.0(5)
C11 C12 C13 126.3(4)
O6 C13 O5 112.3(5)
O6 C13 C14 109.2(4)
O5 C13 C14 106.5(4)
O6 C13 C12 113.0(5)
O5 C13 C12 107.4(4)
C14 C13 C12 108.1(4)
C1 C2 C3 120.1(3)
O2 C6 O1 125.2(5)
O2 C6 C1 117.2(4)
O1 C6 C1 117.6(3)
C12 C11 C10 118.6(5)
C18 C17 C16 119.15(18)
N3 C16 C17 122.3(2)
C9 C10 C11 119.1(7)
C10 C9 C8 119.1(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ni1 O1 1.999(3)
Ni1 N3 2.072(4)
Ni1 N1 2.080(4)
Ni1 O7 2.094(5)
Ni1 N2 2.098(5)
Ni1 O5 2.121(3)
O5 C13 1.448(7)
O3 C7 1.251(5)
O1 C6 1.276(6)
O4 C7 1.248(6)
O7 C19 1.385(10)
O2 C6 1.242(5)
O6 C13 1.374(5)
N3 C14 1.324(4)
N3 C16 1.338(5)
N1 C5 1.343(6)
N1 C1 1.349(4)
N2 C12 1.343(6)
N2 C8 1.358(8)
C4 C3 1.381(5)
C4 C5 1.406(7)
C4 C7 1.500(7)
C3 C2 1.384(6)
C14 C15 1.3823
C14 C13 1.522(6)
C1 C2 1.377(6)
C1 C6 1.505(6)
C15 C18 1.39
C18 C17 1.375(4)
C8 C9 1.370(11)
C12 C11 1.389(8)
C12 C13 1.538(10)
C11 C10 1.392(11)
C17 C16 1.39
C10 C9 1.367(11)
O8 C30 1.230(17)
