Flexible and Dynamic Thermal Behavior of Self-Catenated [{Ni3(H2O)3(Bpa)4}(V6O18)].8H2O Constructed from 10-c Heterometallic Inorganic-Organic Clusters
Roberto Fernández de Luis; José L. Mesa; M. Karmele Urtiaga; Edurne S. Larrea; Teófilo Rojo; María I. Arriortua; Inorganic Chemistry 51 (2012) 2130–2139; doi:10.1021/ic201951e

data_4328307
_publ_contact_author
;
   Dra. Miren Karmele Urtiaga Greaves
   Facultad de Ciencia y Tecnolog\'ia
   Dpto. de Mineralog\'ia y Petrolog\'ia 
   Universidad del Pa\'is Vasco
   Apartado 644
   48080 Bilbao
   Spain
;
_publ_contact_author_email       karmele.urtiaga@ehu.es
_publ_contact_author_fax         '34 4 4648500'
_publ_contact_author_phone       '34 4 601000 ext 5372'
_publ_section_title
;
 Flexible and Dynamic Thermal Behavior of Self-Catenated
 [{Ni3(H2O)3(Bpa)4}(V6O18)].8H2O Constructed from 10-c Heterometallic
 Inorganic-Organic Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2130
_journal_page_last               2139
_journal_paper_doi               10.1021/ic201951e
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C48 H54 N8 Ni3 O21 V6'
_chemical_formula_sum            'C48 H54 N8 Ni3 O29 V6'
_chemical_formula_weight         1688.76
_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             2010-03-12T12:04:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 112.3880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5536(2)
_cell_length_b                   19.0463(2)
_cell_length_c                   27.7435(3)
_cell_measurement_reflns_used    20529
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.8607
_cell_measurement_theta_min      2.8851
_cell_volume                     6622.05(15)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
        (compiled Jan 27 2009,14:17:37)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
        (compiled Jan 27 2009,14:17:37)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
        (compiled Jan 27 2009,14:17:37)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.264
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Goniometer Xcalibur, detector: Onyx (Nova)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0589482398
_diffrn_orient_matrix_UB_12      -0.028522269
_diffrn_orient_matrix_UB_13      -0.0501598447
_diffrn_orient_matrix_UB_21      0.0920176443
_diffrn_orient_matrix_UB_22      -0.0416466136
_diffrn_orient_matrix_UB_23      -0.012177554
_diffrn_orient_matrix_UB_31      -0.0339007723
_diffrn_orient_matrix_UB_32      -0.0631307749
_diffrn_orient_matrix_UB_33      0.0306844312
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            50933
_diffrn_reflns_theta_full        74.02
_diffrn_reflns_theta_max         74.02
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    8.446
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.50677
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
X-RED (Stoe & Cie, March 2001 Revision 1.22) and
X-SHAPE (Stoe & Cie, October 1999, Revision 1.06)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.1207
_exptl_crystal_size_mid          0.0533
_exptl_crystal_size_min          0.0269
_refine_diff_density_max         1.176
_refine_diff_density_min         -1.09
_refine_diff_density_rms         0.12
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         13347
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0558
_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^)+(0.1011P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                10278
_reflns_number_total             13347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201951e_si_002.cif
_cod_data_source_block           '[{Ni3(H2O)3(Bpa)4}(V6O18)]_8H2O'
_cod_original_cell_volume        6622.05(14)
_cod_database_code               4328307