#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/27/2012741.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_2012741
loop_
_publ_author_name
'Assaaoudi, Hassane'
'Ennaciri, Abdelaziz'
'Harcharras, Mohamed'
'El Bali, Brahim'
'Reinauer, Felix'
'Glaum, Robert'
'Rulmont, André'
'Spirlet, Marie-Rose'
_publ_section_title
;
 KZn(HP₂O₇)·2H₂O and KMn(HP₂O₇)·2H₂O: acid
 pyrophosphate metallates(II) with layer structures
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i79
_journal_page_last               i81
_journal_paper_doi               10.1107/S0108270102007394
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'K Zn (H P2 O7) (H2 O)2'
_chemical_formula_structural     'K Zn (H P2 O7) (H2 O)2'
_chemical_formula_sum            'H5 K O9 P2 Zn'
_chemical_formula_weight         315.45
_chemical_name_systematic
;
potassium zinc hydrogen pyrophosphate dihydrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4727(12)
_cell_length_b                   7.7820(9)
_cell_length_c                   6.5009(7)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.47
_cell_measurement_theta_min      5.27
_cell_volume                     782.76(14)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'SHELXTL (Siemens, 1991)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       2θ/ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1080
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.101
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.383
_refine_ls_extinction_coef       0.0275(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0252
_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)+(0.0335P)²+0.9013P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                692
_reflns_number_total             738
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            br1366.cif
_cod_data_source_block           I
_cod_database_code               2012741
_cod_database_fobs_code          2012741
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, 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
Zn1 0.69589(3) 0.2500 0.56130(7) 0.0102(2) Uani d S 1 . . Zn
K1 0.96483(6) 0.2500 -0.11827(15) 0.0195(3) Uani d S 1 . . K
P1 0.86388(5) 0.06111(9) 0.36065(11) 0.0088(2) Uani d . 1 . . P
O1 0.88760(19) 0.2500 0.2742(5) 0.0124(6) Uani d S 1 . . O
O2 0.92463(13) 0.0311(3) 0.5454(3) 0.0148(5) Uani d . 1 . . O
H2 0.9717 -0.0006 0.4944 0.02(2) Uiso d PR 0.50 . . H
O3 0.88466(13) -0.0567(3) 0.1842(3) 0.0141(5) Uani d . 1 . . O
O4 0.77097(13) 0.0615(3) 0.4290(3) 0.0140(5) Uani d . 1 . . O
O5W 0.8937(2) -0.2500 0.8113(5) 0.0173(7) Uani d S 1 . . O
H5W 0.895(3) -0.158(6) 0.733(7) 0.041(12) Uiso d . 1 . . H
O6W 0.7156(2) -0.2500 0.3182(5) 0.0158(7) Uani d S 1 . . O
H6W 0.734(3) -0.168(6) 0.386(7) 0.045(13) Uiso d . 1 . . H
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
O4 Zn1 O4 7_565 . 90.82(11) ?
O4 Zn1 O3 7_565 2_655 177.29(8) ?
O4 Zn1 O3 . 2_655 89.06(8) ?
O4 Zn1 O3 7_565 8_766 89.06(8) ?
O4 Zn1 O3 . 8_766 177.29(8) ?
O3 Zn1 O3 2_655 8_766 90.93(11) ?
O4 Zn1 O5W 7_565 2_654 92.75(9) ?
O4 Zn1 O5W . 2_654 92.75(9) ?
O3 Zn1 O5W 2_655 2_654 84.55(9) ?
O3 Zn1 O5W 8_766 2_654 84.55(9) ?
O4 Zn1 O6W 7_565 2_655 88.02(9) ?
O4 Zn1 O6W . 2_655 88.02(9) ?
O3 Zn1 O6W 2_655 2_655 94.68(9) ?
O3 Zn1 O6W 8_766 2_655 94.68(9) ?
O5W Zn1 O6W 2_654 2_655 178.90(13) ?
O4 Zn1 K1 7_565 6_556 127.17(6) ?
O4 Zn1 K1 . 6_556 127.17(6) ?
O3 Zn1 K1 2_655 6_556 51.22(5) ?
O3 Zn1 K1 8_766 6_556 51.22(5) ?
O5W Zn1 K1 2_654 6_556 55.47(9) ?
O6W Zn1 K1 2_655 6_556 123.43(9) ?
O3 K1 O3 3_755 5_755 64.86(9) ?
O3 K1 O1 3_755 . 119.37(7) ?
O3 K1 O1 5_755 . 119.37(7) ?
O3 K1 O6W 3_755 2_654 143.02(6) ?
O3 K1 O6W 5_755 2_654 143.02(6) ?
O1 K1 O6W . 2_654 73.32(10) ?
O3 K1 O2 3_755 1_554 112.69(7) ?
O3 K1 O2 5_755 1_554 75.08(6) ?
O1 K1 O2 . 1_554 127.17(6) ?
O6W K1 O2 2_654 1_554 70.78(7) ?
O3 K1 O2 3_755 7_564 75.08(6) ?
O3 K1 O2 5_755 7_564 112.69(7) ?
O1 K1 O2 . 7_564 127.17(6) ?
O6W K1 O2 2_654 7_564 70.78(7) ?
O2 K1 O2 1_554 7_564 73.70(9) ?
O3 K1 O5W 3_755 5_756 59.30(7) ?
O3 K1 O5W 5_755 5_756 59.30(7) ?
O1 K1 O5W . 5_756 72.74(9) ?
O6W K1 O5W 2_654 5_756 146.06(10) ?
O2 K1 O5W 1_554 5_756 132.87(6) ?
O2 K1 O5W 7_564 5_756 132.87(6) ?
O3 K1 O3 3_755 7_565 90.86(6) ?
O3 K1 O3 5_755 7_565 141.57(4) ?
O1 K1 O3 . 7_565 46.18(4) ?
O6W K1 O3 2_654 7_565 73.62(6) ?
O2 K1 O3 1_554 7_565 143.35(6) ?
O2 K1 O3 7_564 7_565 86.74(6) ?
O5W K1 O3 5_756 7_565 82.97(6) ?
O3 K1 O3 3_755 . 141.57(4) ?
O3 K1 O3 5_755 . 90.86(6) ?
O1 K1 O3 . . 46.18(4) ?
O6W K1 O3 2_654 . 73.62(6) ?
O2 K1 O3 1_554 . 86.74(6) ?
O2 K1 O3 7_564 . 143.35(6) ?
O5W K1 O3 5_756 . 82.97(6) ?
O3 K1 O3 7_565 . 91.50(7) ?
O3 K1 Zn1 3_755 6_656 35.91(4) ?
O3 K1 Zn1 5_755 6_656 35.91(4) ?
O1 K1 Zn1 . 6_656 109.18(7) ?
O6W K1 Zn1 2_654 6_656 177.50(8) ?
O2 K1 Zn1 1_554 6_656 107.28(5) ?
O2 K1 Zn1 7_564 6_656 107.28(5) ?
O5W K1 Zn1 5_756 6_656 36.44(6) ?
O3 K1 Zn1 7_565 6_656 108.03(4) ?
O3 K1 Zn1 . 6_656 108.03(4) ?
O3 K1 P1 3_755 . 132.63(6) ?
O3 K1 P1 5_755 . 105.08(5) ?
O1 K1 P1 . . 22.929(13) ?
O6W K1 P1 2_654 . 73.25(7) ?
O2 K1 P1 1_554 . 108.07(5) ?
O2 K1 P1 7_564 . 140.94(5) ?
O5W K1 P1 5_756 . 75.55(6) ?
O3 K1 P1 7_565 . 68.82(4) ?
O3 K1 P1 . . 23.32(4) ?
Zn1 K1 P1 6_656 . 109.03(3) ?
O3 K1 P1 3_755 7_565 105.08(5) ?
O3 K1 P1 5_755 7_565 132.63(6) ?
O1 K1 P1 . 7_565 22.929(13) ?
O6W K1 P1 2_654 7_565 73.25(7) ?
O2 K1 P1 1_554 7_565 140.94(5) ?
O2 K1 P1 7_564 7_565 108.07(5) ?
O5W K1 P1 5_756 7_565 75.55(6) ?
O3 K1 P1 7_565 7_565 23.32(4) ?
O3 K1 P1 . 7_565 68.82(4) ?
Zn1 K1 P1 6_656 7_565 109.03(3) ?
P1 K1 P1 . 7_565 45.76(2) ?
O3 P1 O4 . . 115.53(12) yes
O3 P1 O2 . . 111.80(12) yes
O4 P1 O2 . . 110.65(12) yes
O3 P1 O1 . . 103.93(13) yes
O4 P1 O1 . . 108.52(13) yes
O2 P1 O1 . . 105.67(14) yes
O3 P1 K1 . . 61.33(8) ?
O4 P1 K1 . . 129.56(9) ?
O2 P1 K1 . . 116.63(9) ?
O1 P1 K1 . . 42.78(10) ?
P1 O1 P1 . 7_565 130.91(19) yes
P1 O1 K1 . . 114.29(10) ?
P1 O1 K1 7_565 . 114.29(10) ?
P1 O2 K1 . 1_556 129.92(12) ?
P1 O3 Zn1 . 2_654 126.67(12) ?
P1 O3 K1 . 5_755 128.40(11) ?
Zn1 O3 K1 2_654 5_755 92.87(7) ?
P1 O3 K1 . . 95.35(9) ?
Zn1 O3 K1 2_654 . 120.46(8) ?
K1 O3 K1 5_755 . 89.14(6) ?
P1 O4 Zn1 . . 131.60(12) ?
Zn1 O5W K1 2_655 5_756 88.09(11) ?
Zn1 O6W K1 2_654 2_655 137.76(15) ?
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
Zn1 O4 7_565 2.059(2) ?
Zn1 O4 . 2.059(2) yes
Zn1 O3 2_655 2.111(2) yes
Zn1 O3 8_766 2.111(2) ?
Zn1 O5W 2_654 2.136(3) yes
Zn1 O6W 2_655 2.160(3) yes
Zn1 K1 6_556 3.5942(11) ?
K1 O3 3_755 2.805(2) ?
K1 O3 5_755 2.805(2) ?
K1 O1 . 2.817(3) ?
K1 O6W 2_654 2.822(3) ?
K1 O2 1_554 2.841(2) ?
K1 O2 7_564 2.841(2) ?
K1 O5W 5_756 2.963(4) ?
K1 O3 7_565 3.332(2) ?
K1 O3 . 3.332(2) ?
K1 Zn1 6_656 3.5942(11) ?
K1 P1 . 3.7807(12) ?
K1 P1 7_565 3.7807(12) ?
P1 O3 . 1.503(2) yes
P1 O4 . 1.505(2) yes
P1 O2 . 1.543(2) yes
P1 O1 . 1.6160(14) yes
O1 P1 7_565 1.6160(14) ?
O2 K1 1_556 2.841(2) ?
O3 Zn1 2_654 2.111(2) ?
O3 K1 5_755 2.805(2) ?
O5W Zn1 2_655 2.136(3) ?
O5W K1 5_756 2.963(4) ?
O6W Zn1 2_654 2.160(3) ?
O6W K1 2_655 2.822(3) ?
