#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:30:31 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180397 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/66/7206665.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_7206665
loop_
_publ_author_name
'Calderón-Casado, Ainhoa'
'Barandika, Gotzone'
'Bazán, Begoña'
'Urtiaga, Miren-Karmele'
'Vallcorba, Oriol'
'Rius, Jordi'
'Miravittles, Carles'
'Arriortua, María-Isabel'
_publ_section_title
;
 Solid-state transformation of the MOF
 [Ni2(bipy)1.5(PDC)2(H2O)2]·3.5H2O
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              6831
_journal_paper_doi               10.1039/c1ce05594a
_journal_volume                  13
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'2(C29 H18 N5 Ni2 O10),6(O0.50), 2(O0.50),2(O0.50)'
_chemical_formula_sum            'C58 H36 N10 Ni4 O27'
_chemical_formula_weight         1539.81
_chemical_name_systematic
;
?
;
_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      2.3
_audit_creation_date             2010-07-26T12:56:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 116.141(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.6280(16)
_cell_length_b                   11.6031(11)
_cell_length_c                   22.004(3)
_cell_measurement_reflns_used    1482
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9699
_cell_measurement_theta_min      2.6225
_cell_volume                     3352.7(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, 1997)'
_computing_structure_solution    DIRDIF2008
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3504
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire2 (l'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0416381487
_diffrn_orient_matrix_UB_12      0.0259668046
_diffrn_orient_matrix_UB_13      0.0049848225
_diffrn_orient_matrix_UB_21      -0.0114686578
_diffrn_orient_matrix_UB_22      -0.051726881
_diffrn_orient_matrix_UB_23      0.0146535631
_diffrn_orient_matrix_UB_31      0.02503812
_diffrn_orient_matrix_UB_32      0.0195365085
_diffrn_orient_matrix_UB_33      0.0324202271
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1321
_diffrn_reflns_av_unetI/netI     0.2954
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11305
_diffrn_reflns_theta_full        22.98
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
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_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.1337
_exptl_crystal_size_mid          0.0615
_exptl_crystal_size_min          0.0321
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.75
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.744
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4624
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.743
_refine_ls_R_factor_all          0.1572
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0200P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                1934
_reflns_number_total             4624
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05594a.txt
_cod_data_source_block           '[ni2(4,4-bipy)1.5(2,5-PDC)2(H2O)2]3.5H2O'
_cod_database_code               7206665
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
C1 C -0.1899(6) -0.3588(6) -0.0706(4) 0.0160(6) Uani 1 1 d .
H1 H -0.1273 -0.3708 -0.073 0.019 Uiso 1 1 calc R
C2 C -0.1894(6) -0.3514(6) -0.0079(4) 0.0160(6) Uani 1 1 d .
H2 H -0.1275 -0.3611 0.0319 0.019 Uiso 1 1 calc R
C3 C -0.2794(5) -0.3297(6) -0.0028(4) 0.0160(6) Uani 1 1 d .
C4 C -0.3695(5) -0.3261(6) -0.0624(3) 0.0160(6) Uani 1 1 d .
H4 H -0.4327 -0.3162 -0.0605 0.019 Uiso 1 1 calc R
C5 C -0.3674(6) -0.3369(6) -0.1240(4) 0.0160(6) Uani 1 1 d .
H5 H -0.4299 -0.3356 -0.164 0.019 Uiso 1 1 calc R
C6 C -0.1962(6) -0.2460(6) 0.1796(4) 0.0160(6) Uani 1 1 d .
H6 H -0.1348 -0.2236 0.2171 0.019 Uiso 1 1 calc R
C7 C -0.1924(6) -0.2767(6) 0.1193(3) 0.0160(6) Uani 1 1 d .
H7 H -0.1293 -0.276 0.1167 0.019 Uiso 1 1 calc R
C8 C -0.2810(5) -0.3084(6) 0.0633(3) 0.0160(6) Uani 1 1 d .
C9 C -0.3702(5) -0.3107(6) 0.0711(4) 0.0160(6) Uani 1 1 d .
H9 H -0.4329 -0.3323 0.0344 0.019 Uiso 1 1 calc R
C10 C -0.3663(5) -0.2810(6) 0.1334(3) 0.0160(6) Uani 1 1 d .
H10 H -0.4276 -0.2854 0.1382 0.019 Uiso 1 1 calc R
C11 C -0.2556(5) -0.0722(6) -0.1762(3) 0.0147(5) Uani 1 1 d .
C12 C -0.2746(5) 0.0373(6) -0.1598(3) 0.0147(5) Uani 1 1 d .
H12 H -0.2203 0.089 -0.1355 0.018 Uiso 1 1 calc R
C13 C -0.3749(5) 0.0696(6) -0.1798(3) 0.0147(5) Uani 1 1 d .
H13 H -0.3905 0.1452 -0.1706 0.018 Uiso 1 1 calc R
C14 C -0.4512(5) -0.0077(6) -0.2127(3) 0.0147(5) Uani 1 1 d .
C15 C -0.4263(6) -0.1149(6) -0.2292(4) 0.0147(5) Uani 1 1 d .
H15 H -0.4794 -0.1669 -0.255 0.018 Uiso 1 1 calc R
C16 C -0.5625(5) 0.0208(7) -0.2323(3) 0.0147(5) Uani 1 1 d .
C17 C -0.1494(6) -0.1174(6) -0.1540(4) 0.0147(5) Uani 1 1 d .
C18 C 0.2752(5) -0.0183(6) -0.1029(4) 0.0203(9) Uani 1 1 d .
H18 H 0.2339 -0.0279 -0.1501 0.024 Uiso 1 1 calc R
C19 C 0.3795(5) -0.0158(6) -0.0801(4) 0.0203(9) Uani 1 1 d .
H19 H 0.4074 -0.0237 -0.1116 0.024 Uiso 1 1 calc R
C20 C 0.4428(5) -0.0023(6) -0.0135(4) 0.0203(9) Uani 1 1 d .
C21 C 0.3957(5) 0.0112(6) 0.0280(4) 0.0203(9) Uani 1 1 d .
H21 H 0.4358 0.0221 0.0752 0.024 Uiso 1 1 calc R
C22 C 0.2913(5) 0.0091(6) 0.0020(3) 0.0203(9) Uani 1 1 d .
H22 H 0.2622 0.0205 0.0326 0.024 Uiso 1 1 calc R
C23 C 0.0262(6) -0.3715(7) -0.2883(4) 0.0196(5) Uani 1 1 d .
C24 C 0.0678(5) -0.2285(7) -0.1943(4) 0.0196(5) Uani 1 1 d .
H24 H 0.0646 -0.1702 -0.2255 0.024 Uiso 1 1 calc R
C25 C 0.0567(5) -0.3449(7) -0.2156(4) 0.0196(5) Uani 1 1 d .
C26 C 0.0942(5) -0.2814(7) -0.0868(4) 0.0196(5) Uani 1 1 d .
C27 C 0.0657(5) -0.4274(7) -0.1689(3) 0.0196(5) Uani 1 1 d .
H27 H 0.0562 -0.5062 -0.1819 0.024 Uiso 1 1 calc R
C28 C 0.0883(5) -0.3979(7) -0.1034(4) 0.0196(5) Uani 1 1 d .
H28 H 0.0995 -0.4555 -0.0702 0.024 Uiso 1 1 calc R
C29 C 0.1129(6) -0.2404(7) -0.0177(4) 0.0196(5) Uani 1 1 d .
N1 N -0.2779(4) -0.3495(5) -0.1296(3) 0.0160(6) Uani 1 1 d .
N2 N -0.2821(5) -0.2467(5) 0.1870(3) 0.0160(6) Uani 1 1 d .
N3 N -0.3307(4) -0.1465(5) -0.2100(3) 0.0147(5) Uani 1 1 d .
N4 N 0.2286(4) -0.0079(5) -0.0626(3) 0.0203(9) Uani 1 1 d .
N5 N 0.0826(4) -0.1970(5) -0.1327(3) 0.0196(5) Uani 1 1 d .
O1 O -0.1408(3) -0.2207(4) -0.1704(2) 0.0147(5) Uani 1 1 d .
O2 O -0.0779(3) -0.0513(4) -0.1197(2) 0.0147(5) Uani 1 1 d .
O1W O 0.3416(4) -0.1562(5) -0.3807(3) 0.0431(17) Uiso 1 1 d .
O3 O -0.6241(3) -0.0624(4) -0.2499(2) 0.0147(5) Uani 1 1 d .
O2W O 0.0707(4) -0.4017(4) 0.1213(2) 0.0234(14) Uiso 1 1 d .
O4 O -0.5823(3) 0.1239(4) -0.2270(2) 0.0147(5) Uani 1 1 d .
O4W O 0.4232(9) -0.0761(12) -0.4640(6) 0.070(4) Uiso 0.5 1 d P
O5 O 0.0544(3) 0.1139(4) -0.0489(2) 0.0152(9) Uani 1 1 d U
O3W O -0.2857(9) -0.7652(11) -0.2890(6) 0.072(4) Uiso 0.5 1 d P
O6 O -0.2038(3) -0.4593(4) -0.2253(2) 0.0152(9) Uani 1 1 d U
O5W O 0.4075(10) -0.0909(12) -0.5938(7) 0.085(5) Uiso 0.5 1 d P
O7 O 0.1035(4) -0.1336(4) -0.0098(2) 0.0196(5) Uani 1 1 d .
O8 O 0.1305(3) -0.3148(4) 0.0275(2) 0.0196(5) Uani 1 1 d .
O9 O -0.0284(3) -0.4620(4) -0.3119(2) 0.0196(5) Uani 1 1 d .
O10 O 0.0484(3) -0.3046(4) -0.3240(2) 0.0196(5) Uani 1 1 d .
Ni1 Ni -0.27580(7) -0.30598(8) -0.22185(5) 0.0131(3) Uani 1 1 d .
Ni2 Ni 0.07255(7) -0.03851(8) -0.09494(5) 0.0136(3) Uani 1 1 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'
O O 0.0106 0.006 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 C1 C2 122.1(7) . .
C1 C2 C3 120.3(7) . .
C4 C3 C2 117.8(7) . .
C4 C3 C8 120.1(7) . .
C2 C3 C8 122.2(6) . .
C5 C4 C3 120.2(7) . .
C4 C5 N1 122.3(7) . .
N2 C6 C7 123.1(7) . .
C8 C7 C6 119.9(7) . .
C7 C8 C9 117.1(7) . .
C7 C8 C3 120.2(7) . .
C9 C8 C3 122.5(6) . .
C10 C9 C8 118.9(7) . .
N2 C10 C9 124.5(7) . .
N3 C11 C12 121.9(7) . .
N3 C11 C17 115.7(7) . .
C12 C11 C17 122.3(7) . .
C11 C12 C13 118.2(7) . .
C14 C13 C12 119.7(7) . .
C13 C14 C15 118.6(7) . .
C13 C14 C16 122.0(7) . .
C15 C14 C16 119.4(6) . .
N3 C15 C14 121.9(7) . .
O4 C16 O3 126.8(7) . .
O4 C16 C14 116.4(6) . .
O3 C16 C14 116.8(7) . .
O2 C17 O1 126.0(7) . .
O2 C17 C11 117.0(7) . .
O1 C17 C11 117.0(7) . .
N4 C18 C19 124.0(7) . .
C20 C19 C18 121.0(7) . .
C19 C20 C21 115.4(6) . .
C19 C20 C20 122.6(8) . 3_655
C21 C20 C20 121.9(9) . 3_655
C20 C21 C22 120.9(7) . .
N4 C22 C21 124.4(7) . .
O10 C23 O9 122.9(7) . .
O10 C23 C25 120.7(7) . .
O9 C23 C25 116.3(7) . .
N5 C24 C25 122.9(7) . .
C27 C25 C24 117.4(7) . .
C27 C25 C23 123.1(7) . .
C24 C25 C23 119.2(7) . .
N5 C26 C28 121.9(7) . .
N5 C26 C29 115.6(7) . .
C28 C26 C29 122.5(7) . .
C25 C27 C28 120.9(8) . .
C27 C28 C26 118.5(7) . .
O8 C29 O7 124.1(7) . .
O8 C29 C26 117.8(7) . .
O7 C29 C26 117.9(7) . .
C1 N1 C5 117.1(6) . .
C1 N1 Ni1 121.7(5) . .
C5 N1 Ni1 118.7(4) . .
C6 N2 C10 116.4(6) . .
C6 N2 Ni1 118.4(5) . 4_556
C10 N2 Ni1 125.2(5) . 4_556
C15 N3 C11 119.5(7) . .
C15 N3 Ni1 128.3(5) . .
C11 N3 Ni1 112.1(5) . .
C22 N4 C18 114.2(6) . .
C22 N4 Ni2 121.6(5) . .
C18 N4 Ni2 123.7(5) . .
C24 N5 C26 118.1(7) . .
C24 N5 Ni2 130.7(5) . .
C26 N5 Ni2 110.6(5) . .
C17 O1 Ni1 114.8(5) . .
C17 O2 Ni2 136.9(5) . .
C16 O4 Ni1 123.4(5) . 2_454
C29 O7 Ni2 113.3(5) . .
C23 O9 Ni2 128.5(5) . 2_544
O4 Ni1 O1 174.27(19) 2_444 .
O4 Ni1 N2 89.0(2) 2_444 4
O1 Ni1 N2 90.8(2) . 4
O4 Ni1 N3 93.9(2) 2_444 .
O1 Ni1 N3 80.4(2) . .
N2 Ni1 N3 90.3(2) 4 .
O4 Ni1 O6 92.70(18) 2_444 .
O1 Ni1 O6 93.03(18) . .
N2 Ni1 O6 91.4(2) 4 .
N3 Ni1 O6 173.2(2) . .
O4 Ni1 N1 89.6(2) 2_444 .
O1 Ni1 N1 90.2(2) . .
N2 Ni1 N1 175.4(2) 4 .
N3 Ni1 N1 85.5(2) . .
O6 Ni1 N1 93.0(2) . .
O2 Ni2 O7 89.00(19) . .
O2 Ni2 N5 95.1(2) . .
O7 Ni2 N5 82.0(2) . .
O2 Ni2 O9 86.37(18) . 2_554
O7 Ni2 O9 171.9(2) . 2_554
N5 Ni2 O9 91.7(2) . 2_554
O2 Ni2 N4 173.2(2) . .
O7 Ni2 N4 90.7(2) . .
N5 Ni2 N4 91.6(2) . .
O9 Ni2 N4 94.7(2) 2_554 .
O2 Ni2 O5 80.75(19) . .
O7 Ni2 O5 92.09(19) . .
N5 Ni2 O5 172.9(2) . .
O9 Ni2 O5 93.78(18) 2_554 .
N4 Ni2 O5 92.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.373(8) .
C1 C2 1.378(9) .
C2 C3 1.393(9) .
C3 C4 1.392(9) .
C3 C8 1.485(9) .
C4 C5 1.375(8) .
C5 N1 1.376(8) .
C6 N2 1.336(8) .
C6 C7 1.398(8) .
C7 C8 1.388(9) .
C8 C9 1.390(8) .
C9 C10 1.390(8) .
C10 N2 1.337(8) .
C11 N3 1.336(8) .
C11 C12 1.381(9) .
C11 C17 1.503(9) .
C12 C13 1.385(8) .
C13 C14 1.364(9) .
C14 C15 1.389(9) .
C14 C16 1.524(9) .
C15 N3 1.321(8) .
C16 O4 1.248(8) .
C16 O3 1.260(8) .
C17 O2 1.248(7) .
C17 O1 1.274(7) .
C18 N4 1.342(8) .
C18 C19 1.381(9) .
C19 C20 1.354(9) .
C20 C21 1.372(9) .
C20 C20 1.511(13) 3_655
C21 C22 1.375(8) .
C22 N4 1.325(8) .
C23 O10 1.246(8) .
C23 O9 1.282(8) .
C23 C25 1.490(9) .
C24 N5 1.326(8) .
C24 C25 1.416(9) .
C25 C27 1.368(9) .
C26 N5 1.363(8) .
C26 C28 1.393(10) .
C26 C29 1.498(9) .
C27 C28 1.372(9) .
C29 O8 1.255(8) .
C29 O7 1.267(8) .
N1 Ni1 2.104(6) .
N2 Ni1 2.060(6) 4_556
N3 Ni1 2.079(6) .
N4 Ni2 2.100(6) .
N5 Ni2 2.050(6) .
O1 Ni1 2.046(4) .
O2 Ni2 2.026(5) .
O4 Ni1 2.045(5) 2_454
O5 Ni2 2.112(4) .
O6 Ni1 2.085(4) .
O7 Ni2 2.046(5) .
O9 Ni2 2.060(5) 2_544
Ni1 O4 2.045(5) 2_444
Ni1 N2 2.060(6) 4
Ni2 O9 2.060(5) 2_554
