Inorganic−Organic Hybrid Materials with Novel Framework Structures: Synthesis, Structure, and Magnetic Properties of [Ni(py)4]2V10O29and [Ni2(py)5(H2O)3]V4O12
Khan, M. Ishaque; Nome, Renata C.; Deb, Sangita; McNeely, James H.; Cage, Brant; Doedens, Robert J.; Crystal Growth & Design 9 (2009) 2848–; doi:10.1021/cg9001237

data_4509470
_publ_section_title
;
 Inorganic&#x2212;Organic Hybrid Materials with Novel Framework
 Structures: Synthesis, Structure, and Magnetic Properties of
 [Ni(py)4]2V10O29and [Ni2(py)5(H2O)3]V4O12
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2848
_journal_paper_doi               10.1021/cg9001237
_journal_volume                  9
_journal_year                    2009
_chemical_formula_sum            'C25 H31 N5 Ni2 O15 V4'
_chemical_formula_weight         962.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.480(4)
_cell_length_b                   11.444(3)
_cell_length_c                   17.450(5)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    169(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      3.56
_cell_volume                     3490.7(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      169(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '25s frames at 0.3 deg omega increments'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35401
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        o
_exptl_absorpt_coefficient_mu    2.158
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   'semi-empirical from equivalents'
_exptl_absorpt_process_details   'computed via SADABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          .23
_exptl_crystal_size_mid          .19
_exptl_crystal_size_min          .14
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.025(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8366
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0188
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0469
_refine_ls_wR_factor_ref         0.0477
_reflns_number_gt                7977
_reflns_number_total             8366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg9001237sup1.cif
_cod_data_source_block           isk117
_cod_original_cell_volume        3490.9(5)
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               4509470