#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/03/4000361.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4000361
_publ_section_title
;
Crystal structures and magnetic properties of the new alkaline
zinc oxovanadium phosphates MZn(H2O)(VO)2(PO4)2(H2PO4)
with M = K+, Rb+ and Cs+.
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/cm031090k
_journal_year                    2004
_chemical_formula_moiety         'H2 K0.50 O7.50 P1.50 V Zn0.50'
_chemical_formula_sum            'H2 K0.5 O7.5 P1.5 V Zn0.5'
_chemical_formula_weight         271.65
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 104.281(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4459(1)
_cell_length_b                   9.2160(1)
_cell_length_c                   9.3199(2)
_cell_measurement_reflns_used    2591
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.972
_cell_measurement_theta_min      2.910
_cell_volume                     619.78(2)
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       'omega-phi 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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6248
_diffrn_reflns_theta_max         37.05
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    4.205
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.911
_exptl_crystal_density_meas      2.88
_exptl_crystal_density_method    'Archimede's principle in CH2Cl2'
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_ls_extinction_coef       0.0217(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   2.103
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         3318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.103
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0946
_reflns_number_gt                2639
_reflns_number_total             3318
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'H2 K0.50 O7.50 P1.50 V Zn0.50'
_cod_database_code               4000361
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K K 0.17803(18) 0.46586(12) -0.28118(13) 0.0311(3) Uani 0.50 1 d P . .
Zn Zn 0.32949(6) 0.7500 0.38242(4) 0.01900(11) Uani 1 2 d S . .
V1 V 0.55178(7) 0.2500 0.02638(6) 0.01335(11) Uani 1 2 d S . .
V2 V 0.03905(7) 0.7500 -0.02190(6) 0.01428(12) Uani 1 2 d S . .
P1 P 0.29673(7) 0.49026(5) 0.15043(6) 0.01223(12) Uani 1 1 d . . .
P2 P 0.12789(16) 0.66193(11) -0.36731(12) 0.0150(2) Uani 0.50 1 d P . .
O1 O 0.4019(3) 0.2500 -0.1279(2) 0.0234(5) Uani 1 2 d S . .
O2 O 0.4672(2) 0.40379(16) 0.14086(17) 0.0199(3) Uani 1 1 d . . .
O3 O 0.26093(18) 0.60822(15) 0.02580(16) 0.0153(3) Uani 1 1 d . . .
O4 O 0.3364(3) 0.56088(18) 0.30204(18) 0.0311(4) Uani 1 1 d . . .
O5 O 0.1234(2) 0.39978(16) 0.1316(2) 0.0249(4) Uani 1 1 d . . .
O6 O 0.1734(3) 0.7500 -0.2192(2) 0.0183(4) Uani 1 2 d S . .
O7 O 0.0011(3) 0.7500 0.1388(3) 0.0339(6) Uani 1 2 d S . .
O8 O -0.0826(4) 0.6161(3) -0.4169(3) 0.0221(7) Uani 0.50 1 d P . .
O9 O 0.1591(4) 0.7500 0.5089(3) 0.0259(5) Uani 1 2 d S . .
O10 O 0.5828(5) 0.7865(3) 0.5293(4) 0.0337(9) Uani 0.50 1 d P . .
O11 O 0.2367(5) 0.5160(4) -0.3564(5) 0.0347(9) Uani 0.50 1 d P . .
