#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/03/4000362.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_4000362
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/cm031090k
_journal_year                    2004
_chemical_formula_moiety         'H4 O15 P3 Rb V2 Zn'
_chemical_formula_sum            'H4 O15 P3 Rb V2 Zn'
_chemical_formula_weight         589.66
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 103.5010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8586(2)
_cell_length_b                   9.1973(2)
_cell_length_c                   13.1673(3)
_cell_measurement_reflns_used    11461
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      37.036
_cell_measurement_theta_min      0.998
_cell_volume                     1278.68(5)
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12339
_diffrn_reflns_theta_max         37.05
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    7.533
_exptl_absorpt_correction_T_max  1.259
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.063
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_ls_extinction_coef       0.0058(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.661
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         6522
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.719
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.001
_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          0.0929
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                4636
_reflns_number_total             6522
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4000362
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Rb Rb 0.05693(3) 0.45258(3) -0.23953(3) 0.02602(10) Uani 0.8630(11) 1 d P . .
Zn Zn 0.14219(3) 0.74876(3) -0.48025(2) 0.01566(8) Uani 1 1 d . . .
V1 V -0.21132(4) 0.75115(4) -0.23625(3) 0.00983(9) Uani 1 1 d . . .
V2 V -0.00744(4) 0.75407(4) -0.03160(3) 0.01082(9) Uani 1 1 d . . .
P1 P -0.27730(6) 0.51069(6) -0.42776(5) 0.00974(13) Uani 1 1 d . . .
P2 P -0.28687(6) 0.99219(6) -0.43297(5) 0.00962(13) Uani 1 1 d . . .
P3 P 0.09745(7) 0.83370(8) -0.25990(5) 0.01161(15) Uani 0.8630(11) 1 d PD . .
O1 O -0.20737(17) 0.90360(17) -0.34235(13) 0.0145(4) Uani 1 1 d . . .
O2 O -0.14398(16) 0.89440(16) -0.11634(12) 0.0119(3) Uani 1 1 d . . .
O3 O -0.1833(2) 0.43996(18) -0.48262(15) 0.0203(4) Uani 1 1 d . . .
O4 O -0.35511(17) 0.7483(2) -0.22730(14) 0.0200(4) Uani 1 1 d . . .
O5 O -0.38068(17) 0.90100(17) -0.51015(13) 0.0163(4) Uani 1 1 d . . .
O6 O 0.19669(19) 0.93638(18) -0.50947(14) 0.0193(4) Uani 1 1 d . . .
O7 O -0.36998(18) 0.60049(18) -0.50873(14) 0.0170(4) Uani 1 1 d . . .
O8 O 0.00872(17) 0.75875(17) -0.20294(13) 0.0148(3) Uani 1 1 d . . .
O9 O -0.13871(16) 0.60954(16) -0.11518(12) 0.0116(3) Uani 1 1 d . . .
O10 O -0.20106(17) 0.59985(18) -0.33735(13) 0.0150(4) Uani 1 1 d . . .
O11 O 0.1450(2) 0.7372(2) -0.33464(15) 0.0287(5) Uani 1 1 d D . .
O12 O -0.4428(2) 0.25671(19) -0.57303(14) 0.0230(4) Uani 1 1 d . . .
O13 O -0.0470(2) 0.7701(3) -0.5533(2) 0.0525(8) Uani 1 1 d . . .
O14 O 0.0334(2) 0.9731(2) -0.3181(2) 0.0266(6) Uani 0.8630(11) 1 d P . .
O15 O 0.2814(2) 0.3902(3) -0.31834(16) 0.0252(5) Uani 0.8630(11) 1 d P . .
Rb2 Rb 0.0547(2) 1.0464(3) -0.2427(2) 0.0365(8) Uani 0.1370(11) 1 d P . .
P3' P 0.0920(5) 0.6600(6) -0.2536(4) 0.0285(15) Uani 0.1370(11) 1 d PD . .
O14' O 0.2193(17) 0.610(2) -0.1773(11) 0.045(5) Uani 0.1370(11) 1 d P . .
O15' O 0.0364(17) 0.5167(19) -0.3207(14) 0.041(5) Uani 0.1370(11) 1 d P . .
