#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/32/2013239.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2013239
loop_
_publ_author_name
'Zhicheng Liu'
'Linhong Weng'
'Zhenxia Chen'
'Dongyuan Zhao'
_publ_section_title
;
 (NH₄)₂ZrGe₃O₉: a new microporous zirconogermanate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i29
_journal_page_last               i31
_journal_paper_doi               10.1107/S0108270103005353
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '(N H4)2 Zr Ge3 O9'
_chemical_formula_moiety         'Ge3 N2 O9 Zr'
_chemical_formula_sum            'Ge3 N2 O9 Zr'
_chemical_formula_weight         481.01
_chemical_name_common            FDZG-2
_chemical_name_systematic
;
diammonium zirconium getmanate
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   7.117(5)
_cell_length_b                   7.117(5)
_cell_length_c                   10.542(9)
_cell_measurement_reflns_used    568
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.02
_cell_measurement_theta_min      5.62
_cell_volume                     462.4(6)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DS Viewerpro (Accelrys, 2002)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCDr'
_diffrn_measurement_method       ω
_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  0.0852
_diffrn_reflns_av_sigmaI/netI    0.0741
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2333
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         3.31
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.789
_exptl_absorpt_correction_T_max  0.6722
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.460
_refine_diff_density_min         -0.840
_refine_ls_extinction_coef       0.009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     28
_refine_ls_number_reflns         367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0524
_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)+(0.0415P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                280
_reflns_number_total             367
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bc1005.cif
_cod_data_source_block           I
_cod_database_code               2013239
_cod_database_fobs_code          2013239
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Zr 1.0000 1.0000 0.0000 0.0112(6) Uani d S 1 . . Zr
Ge 0.8761(2) 0.6230(2) 0.2500 0.0135(5) Uani d S 1 . . Ge
O1 0.9877(12) 0.7564(12) 0.1128(6) 0.0236(17) Uani d . 1 . . O
O2 0.9235(16) 0.4027(16) 0.2500 0.025(3) Uani d S 1 . . O
N 0.3333 0.6667 0.0559(14) 0.025(4) Uani d S 1 . . N
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Zr 0.0120(8) 0.0120(8) 0.0096(12) 0.0060(4) 0.000 0.000
Ge 0.0118(8) 0.0101(8) 0.0182(9) 0.0052(7) 0.000 0.000
O1 0.029(5) 0.027(4) 0.024(4) 0.020(4) 0.004(3) 0.014(3)
O2 0.014(5) 0.013(5) 0.053(7) 0.011(5) 0.000 0.000
N 0.025(5) 0.025(5) 0.026(9) 0.012(3) 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Zr O1 8_565 2_765 180.0 no
O1 Zr O1 8_565 9_655 90.2(3) no
O1 Zr O1 2_765 9_655 89.8(3) no
O1 Zr O1 8_565 . 89.8(3) no
O1 Zr O1 2_765 . 90.2(3) no
O1 Zr O1 9_655 . 89.8(3) no
O1 Zr O1 8_565 7_775 90.2(3) no
O1 Zr O1 2_765 7_775 89.8(3) no
O1 Zr O1 9_655 7_775 90.2(3) no
O1 Zr O1 . 7_775 180.0 no
O1 Zr O1 8_565 3_675 89.8(3) no
O1 Zr O1 2_765 3_675 90.2(3) no
O1 Zr O1 9_655 3_675 180.0 no
O1 Zr O1 . 3_675 90.2(3) yes
O1 Zr O1 7_775 3_675 89.8(3) no
O1 Ge O1 10_556 . 117.2(5) yes
O1 Ge O2 10_556 2_655 110.6(3) no
O1 Ge O2 . 2_655 110.6(3) yes
O1 Ge O2 10_556 . 104.7(3) no
O1 Ge O2 . . 104.7(3) yes
O2 Ge O2 2_655 . 108.3(6) yes
Ge O1 Zr . . 140.5(4) yes
Ge O2 Ge 3_665 . 131.7(6) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zr O1 8_565 2.068(7) no
Zr O1 2_765 2.068(7) no
Zr O1 9_655 2.068(7) no
Zr O1 . 2.068(7) yes
Zr O1 7_775 2.068(7) no
Zr O1 3_675 2.068(7) no
Ge O1 10_556 1.694(7) no
Ge O1 . 1.694(7) yes
Ge O2 2_655 1.738(10) yes
Ge O2 . 1.761(9) yes
O2 Ge 3_665 1.738(10) no
