Four nodal self-catenated [{Ni8(Bpy)16}V24O68]·8.5(H2O), combining three dimensional metal‒organic and inorganic frameworks
Fernández de Luis, Roberto; Urtiaga, Miren Karmele; Mesa, José Luis; Aguayo, Andrés Tomás; Rojo, Teófilo; Arriortua, María Isabel; CrystEngComm 12 (2010) 1880–; doi:10.1039/b915539b

data_7211850
_publ_section_title
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 Four nodal self-catenated [{Ni8(Bpy)16}V24O68]&#x00B7;8.5(H2O), combining
 three dimensional metal--organic and inorganic frameworks
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1880
_journal_paper_doi               10.1039/b915539b
_journal_volume                  12
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C160 H128 N32 Ni8 O76.53 V24'
_chemical_formula_sum            'C160 H128 N32 Ni8 O76.53 V24'
_chemical_formula_weight         5415.66
_chemical_name_systematic
;
?
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_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      2.3
_audit_creation_date             2008-03-12T10:03:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                104.626(14)
_cell_angle_beta                 100.215(14)
_cell_angle_gamma                96.241(9)
_cell_formula_units_Z            1
_cell_length_a                   11.2784(13)
_cell_length_b                   22.600(3)
_cell_length_c                   22.521(5)
_cell_measurement_reflns_used    48685
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      73.7892
_cell_measurement_theta_min      3.2927
_cell_measurement_wavelength     1.5418
_cell_volume                     5394.9(16)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_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    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_details
;
1 omega 41.00 91.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 18.7475 45.0000 240.0000 0.0000 0.0000 50

2 omega -2.00 51.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 18.7475 -75.0000 120.0000 0.0000 0.0000 53

3 omega -54.00 -4.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 18.7475 -45.0000 0.0000 0.0000 0.0000 50

4 omega -5.00 46.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 18.7475 -45.0000 120.0000 0.0000 0.0000 51

5 omega -57.00 -4.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 18.7475 -75.0000 120.0000 0.0000 0.0000 53

6 omega -41.00 8.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -18.7475 -45.0000 240.0000 0.0000 0.0000 49

7 omega -39.00 14.00 1.0000 10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -18.7475 -75.0000 0.0000 0.0000 0.0000 53

8 phi 89.00 149.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
-40.0000 -94.7500 0.0000 - 0.0000 0.0000 60

9 omega -72.00 -21.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -94.7500 45.0000 120.0000 0.0000 0.0000 51

10 omega -122.00 -70.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -94.7500 45.0000 240.0000 0.0000 0.0000 52

11 omega -118.00 -67.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -94.7500 -45.0000 120.0000 0.0000 0.0000 51

12 omega -158.00 -100.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -94.7500 -167.0000 180.0000 0.0000 0.0000 58

13 omega -118.00 -67.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -94.7500 -45.0000 0.0000 0.0000 0.0000 51

14 omega -72.00 -21.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -94.7500 45.0000 240.0000 0.0000 0.0000 51

15 omega -127.00 -72.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -94.7500 75.0000 0.0000 0.0000 0.0000 55

16 omega -74.00 -24.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -94.7500 75.0000 0.0000 0.0000 0.0000 50

17 phi -148.00 -95.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
-40.0000 -94.7500 0.0000 - 0.0000 0.0000 53

18 omega -118.00 -66.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -94.7500 -37.0000 263.0000 0.0000 0.0000 52

19 phi -31.00 31.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
-40.0000 -94.7500 0.0000 - 0.0000 0.0000 62

20 omega 82.00 137.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 105.0000 -75.0000 120.0000 0.0000 0.0000 55

21 omega 126.00 154.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 105.0000 45.0000 240.0000 0.0000 0.0000 28

22 omega 78.00 127.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 105.0000 45.0000 120.0000 0.0000 0.0000 49

23 phi 89.00 149.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
40.0000 105.0000 0.0000 - 0.0000 0.0000 60

24 omega 81.00 143.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 105.0000 -91.0000 139.0000 0.0000 0.0000 62

25 omega 25.00 71.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 105.0000 -108.0000 92.0000 0.0000 0.0000 46

26 omega 69.00 114.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 105.0000 -108.0000 92.0000 0.0000 0.0000 45

27 omega 78.00 106.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 105.0000 -107.0000 356.0000 0.0000 0.0000 28

28 omega 124.00 177.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 105.0000 75.0000 120.0000 0.0000 0.0000 53

29 omega 73.00 126.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 105.0000 75.0000 240.0000 0.0000 0.0000 53

_diffrn_reflns_theta_min 3.2927
_diffrn_reflns_theta_max 73.7892
_diffrn_reflns_number 48685
_reflns_number_total 28648
_reflns_number_gt 23238
_reflns_threshold_expression >2sigma(I)

_computing_data_collection

'CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)'
;
_diffrn_measurement_device       'XCalibur Nova'
_diffrn_orient_matrix_UB_11      -0.1297456686
_diffrn_orient_matrix_UB_12      0.0131947694
_diffrn_orient_matrix_UB_13      -0.0018065417
_diffrn_orient_matrix_UB_21      -0.0545213953
_diffrn_orient_matrix_UB_22      -0.0708779919
_diffrn_orient_matrix_UB_23      -0.0269220932
_diffrn_orient_matrix_UB_31      -0.0013977926
_diffrn_orient_matrix_UB_32      -0.0068159569
_diffrn_orient_matrix_UB_33      0.0661382244
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48685
_diffrn_reflns_theta_full        67.5
_diffrn_reflns_theta_max         73.7892
_diffrn_reflns_theta_min         3.2927
_exptl_absorpt_coefficient_mu    9.738
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_meas      1.67(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2700
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.477(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2541
_refine_ls_number_reflns         28651
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1454
_reflns_number_gt                23239
_reflns_number_total             28651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b915539b.txt
_cod_data_source_block           Ni8Bpy16V24O68
_cod_original_cell_volume        5394.9(15)
_cod_database_code               7211850