Synthesis, Structure, and Magnetic Ordering of Layered (2-D) V-Based Tris(oxalato)metalates
Kil Sik Min; Arnold L. Rhinegold; Joel S. Miller; Inorganic Chemistry 44 (2005) 8433–8441; doi:10.1021/ic051373+

data_4327362
_publ_section_title
;
 Synthesis, Structure, and Magnetic Ordering of Layered (2-D) V-Based
 Tris(oxalato)metalates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8433
_journal_page_last               8441
_journal_paper_doi               10.1021/ic051373+
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C6 H6 K3 O15 V'
_chemical_formula_weight         486.35
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.6710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7303(6)
_cell_length_b                   19.9435(16)
_cell_length_c                   10.2616(8)
_cell_measurement_reflns_used    7471
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.77
_cell_volume                     1507.4(2)
_computing_cell_refinement       'Bruker SMART'
_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      213(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11651
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    1.568
_exptl_absorpt_correction_T_max  0.8589
_exptl_absorpt_correction_T_min  0.6505
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_density_meas      0
_exptl_crystal_description       blade
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.343
_refine_ls_shift/su_mean         0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                3044
_reflns_number_total             3461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0513732Bsi20050811_013211.cif
_cod_data_source_block           jsm88
_cod_database_code               4327362