#------------------------------------------------------------------------------
#$Date: 2012-02-24 17:13:23 +0000 (Fri, 24 Feb 2012) $
#$Revision: 34330 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/00/4000028.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_4000028
_journal_name_full 'Chemistry of Materials'
_journal_year    2000
_chemical_formula_weight        950.16
_chemical_formula_sum            'C4 H68 N6 O22 P4 Zr3'
_[local]_cod_chemical_formula_sum_orig 'C4 H68 N6 O22 P4 Zr3 '
_chemical_formula_moiety        'C4 H68 N6 O22 P4 Zr3 '
_chemical_formula_structural    (NH4)2[H3NCH2CH2NH3]2[Zr3(OH)6(PO4)4]
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number       2
_cell_length_a                         9.383(3)
_cell_length_b                         9.923(3)
_cell_length_c                         8.342(2)
_cell_angle_alpha                      97.85(2)
_cell_angle_beta                       111.75(2)
_cell_angle_gamma                      113.01(2)
_cell_volume                           627.0(5)
_cell_formula_units_Z                  1
_cell_measurement_temperature          296.2
_cell_measurement_reflns_used          20
_cell_measurement_theta_min            10.3
_cell_measurement_theta_max            14.5
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'-x,-y,-z'
_exptl_crystal_description            'prismatic'
_exptl_crystal_colour                 'colorless'
_exptl_crystal_size_max                0.200
_exptl_crystal_size_mid                0.100
_exptl_crystal_size_min                0.080
_exptl_crystal_density_diffrn          2.425
_exptl_crystal_density_meas            'not measured'
_exptl_crystal_F_000                   980.00
_exptl_absorpt_coefficient_mu          15.6
_exptl_absorpt_correction_type        none
_diffrn_ambient_temperature            296.2
_diffrn_radiation_wavelength           0.7107
_diffrn_radiation_type                'Mo K\a'
_diffrn_radiation_source              'Rigaku rotating anode'
_diffrn_radiation_monochromator        graphite
_diffrn_radiation_detector            'scintillation counter'
_diffrn_measurement_device            'Rigaku AFC7R'
_diffrn_measurement_method             \w-2\q
_diffrn_standards_number              3
_diffrn_standards_interval_count      500
_diffrn_standards_decay_%             0.51
_diffrn_reflns_number                  10755
_reflns_number_total                   10337
_reflns_number_observed                4242
_reflns_observed_criterion             >3.0sigma(I)
_diffrn_reflns_av_R_equivalents        0.066
_diffrn_reflns_av_sigmaI/netI          0.191
_diffrn_reflns_limit_h_min             0
_diffrn_reflns_limit_h_max             18
_diffrn_reflns_limit_k_min             -19
_diffrn_reflns_limit_k_max             18
_diffrn_reflns_limit_l_min             -16
_diffrn_reflns_limit_l_max             15
_diffrn_reflns_theta_min               2.58
_diffrn_reflns_theta_max               45.02
_diffrn_reflns_reduction_process      'Lp corrections applied'
_diffrn_orient_matrix_UB_11            0.06251
_diffrn_orient_matrix_UB_12            0.08037
_diffrn_orient_matrix_UB_13            0.12319
_diffrn_orient_matrix_UB_21           -0.02863
_diffrn_orient_matrix_UB_22           -0.08356
_diffrn_orient_matrix_UB_23            0.05577
_diffrn_orient_matrix_UB_31            0.11125
_diffrn_orient_matrix_UB_32           -0.00127
_diffrn_orient_matrix_UB_33            0.01983
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_refinement_flags
Zr(1)  1.0000      0.0000      1.0000      0.0096(1)   Uani d . 0.50 S
Zr(2)  0.77767(6)  0.49472(5)  1.12717(6)  0.00990(10) Uani d . 1.00 .
P(1)   0.3909(2)   0.3180(1)   1.1368(2)   0.0128(3)   Uani d . 1.00 .
P(2)   0.8277(2)   0.2397(1)   0.8354(2)   0.0119(2)   Uani d . 1.00 .
O(1)   0.3194(5)   0.4318(4)   1.0909(5)   0.0191(9)   Uani d . 1.00 .
O(2)   0.5245(5)   0.3370(4)   1.0629(5)   0.0211(9)   Uani d . 1.00 .
O(3)   1.0822(4)   0.1026(4)   1.2661(4)   0.0139(7)   Uani d . 1.00 .
O(4)   1.2386(5)   0.1519(4)   1.0263(5)   0.0210(9)   Uani d . 1.00 .
O(5)   0.9076(6)   0.1538(5)   0.9470(6)   0.030(1)    Uani d . 1.00 .
O(6)   0.9633(5)   0.3510(5)   0.7897(6)   0.0252(10)  Uani d . 1.00 .
O(7)   0.4688(5)   0.3440(5)   1.3382(5)   0.0238(9)   Uani d . 1.00 .
O(8)   0.6617(5)   0.1279(5)   0.6616(6)   0.0292(10)  Uani d . 1.00 .
O(9)   0.2288(5)   0.3515(4)   0.6999(5)   0.0158(8)   Uani d . 1.00 .
O(10)  0.1421(5)   0.5939(4)   0.6750(5)   0.0150(8)   Uani d . 1.00 .
O(11)  0.2152(6)   0.6653(5)   1.0471(6)   0.028(1)    Uani d . 1.00 .
N(1)   0.3713(7)   1.1717(6)   0.6065(7)   0.028(1)    Uani d . 1.00 .
N(2)   0.3854(7)   0.8760(6)   0.6815(7)   0.027(1)    Uani d . 1.00 .
N(3)   0.2025(6)   0.4422(6)   0.3800(6)   0.024(1)    Uani d . 1.00 .
C(1)   0.322(1)    0.9707(8)   0.7613(10)  0.036(2)    Uani d . 1.00 .
C(2)   0.2391(8)   1.0391(8)   0.6273(9)   0.031(2)    Uani d . 1.00 .
_cod_database_code 4000028