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_4509471
_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            'C40 H40 N8 Ni2 O14.5 V5'
_chemical_formula_weight         1236.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 107.31(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.306(11)
_cell_length_b                   26.46(3)
_cell_length_c                   16.820(17)
_cell_measurement_reflns_used    1016
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      3.09
_cell_volume                     4804(9)
_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      175(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '20s 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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50476
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.770
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  .68
_exptl_absorpt_correction_type   'semi-empirical from equivalents'
_exptl_absorpt_process_details   'computed via SADABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.454
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         11845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.05P)^2^+17.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                9674
_reflns_number_total             11845
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg9001237sup2.cif
_cod_data_source_block           isk136
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4804(14)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C40 H40 N8 Ni2 O14.50 V5'
_cod_database_code               4509471