#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/11/2201132.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_2201132
loop_
_publ_author_name
'Gordon, Laura E.'
'Harrison, William T. A.'
_publ_section_title
;
 Ammonium zinc hydrogenphosphite hydrate,
 (NH₄)₂Zn₅(HPO₃)₆·4H₂O
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i41
_journal_page_last               i43
_journal_paper_doi               10.1107/S1600536802008243
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(N H4)2 Zn5  (H P O3)6,  4H2 O'
_chemical_formula_moiety         '(N H4)2 Zn5  (H P O3)6,  4H2 O'
_chemical_formula_sum            'H11 N O11 P3 Zn2.5'
_chemical_formula_weight         457.43
_chemical_melting_point          'decomposes before melting'
_chemical_name_common            'Ammonium zinc hydrogen phosphite hydrate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                63.4090(10)
_cell_angle_beta                 87.1620(10)
_cell_angle_gamma                72.9690(10)
_cell_formula_units_Z            2
_cell_length_a                   7.2263(3)
_cell_length_b                   9.7728(4)
_cell_length_c                   10.2349(5)
_cell_measurement_reflns_used    3972
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.43
_cell_measurement_theta_min      2.46
_cell_volume                     615.18(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SMART
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_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  0.0128
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6425
_diffrn_reflns_theta_full        32.52
_diffrn_reflns_theta_max         32.52
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.288
_exptl_absorpt_correction_T_max  0.547
_exptl_absorpt_correction_T_min  0.232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'chunky plate'
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.643
_refine_ls_extinction_coef       0.0101(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         4274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0265
_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)+(0.0457P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0741
_reflns_number_gt                3646
_reflns_number_total             4274
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            mg6009.cif
_cod_data_source_block           I
_cod_original_formula_sum        'H11 N O11 P3 Zn2.50'
_cod_database_code               2201132
_cod_database_fobs_code          2201132
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
N1 0.2216(3) 0.0432(3) -0.1527(2) 0.0323(4) Uani d . 1 . . N
H4 0.0901 0.0626 -0.1832 0.039 Uiso d R 1 . . H
H5 0.3153 0.0389 -0.1983 0.039 Uiso d R 1 . . H
H6 0.2653 -0.0598 -0.0947 0.039 Uiso d R 1 . . H
H7 0.2341 0.0888 -0.0898 0.039 Uiso d R 1 . . H
Zn1 0.33591(3) 0.70373(3) 0.33542(2) 0.02207(7) Uani d . 1 . . Zn
Zn2 0.36418(3) 0.35646(3) -0.01856(2) 0.02207(7) Uani d . 1 . . Zn
Zn3 0.5000 0.0000 0.5000 0.02457(8) Uani d S 1 . . Zn
P1 0.76267(7) 0.49691(6) 0.34845(5) 0.02117(10) Uani d . 1 . . P
H1 0.9357 0.4953 0.3861 0.025 Uiso calc R 1 . . H
P2 0.23711(8) 0.59235(7) 0.11813(6) 0.02365(11) Uani d . 1 . . P
H2 0.0574 0.6545 0.0550 0.028 Uiso calc R 1 . . H
P3 0.24927(7) 0.06249(6) 0.20335(5) 0.01984(10) Uani d . 1 . . P
H3 0.1040 0.1587 0.2343 0.024 Uiso calc R 1 . . H
O1 0.6177(2) 0.65059(19) 0.3397(2) 0.0319(3) Uani d . 1 . . O
O2 0.7265(3) 0.34607(19) 0.46569(17) 0.0351(4) Uani d . 1 . . O
O3 0.7754(3) 0.4894(2) 0.20445(17) 0.0364(4) Uani d . 1 . . O
O4 0.3106(3) 0.42325(19) 0.13484(17) 0.0324(3) Uani d . 1 . . O
O5 0.3533(2) 0.7013(2) 0.01944(19) 0.0323(3) Uani d . 1 . . O
O6 0.2266(3) 0.5857(2) 0.2685(2) 0.0414(4) Uani d . 1 . . O
O7 0.2957(2) 0.15858(18) 0.04834(15) 0.0265(3) Uani d . 1 . . O
O8 0.1819(2) -0.07397(18) 0.21001(17) 0.0274(3) Uani d . 1 . . O
O9 0.4199(3) 0.0023(2) 0.31444(18) 0.0340(4) Uani d . 1 . . O
O10 0.2921(3) 0.2245(2) 0.4567(2) 0.0510(5) Uani d . 1 . . O
H8 0.3268 0.2750 0.4848 0.061 Uiso d R 1 . . H
H9 0.2797 0.3058 0.3576 0.061 Uiso d R 1 . . H
O11 0.6953(4) 0.1300(3) 0.3727(3) 0.0661(7) Uani d . 1 . . O
H10 0.7417 0.1837 0.3945 0.079 Uiso d R 1 . . H
H11 0.6129 0.2208 0.2671 0.079 Uiso d R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 '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'
O O 0.0106 0.0060 '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'
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
H4 N1 H5 . . 128.6 ?
H4 N1 H6 . . 105.4 ?
H5 N1 H6 . . 91.0 ?
H4 N1 H7 . . 113.4 ?
H5 N1 H7 . . 109.5 ?
H6 N1 H7 . . 102.7 ?
O6 Zn1 O2 . 2_666 108.41(7) ?
O6 Zn1 O1 . . 114.27(8) ?
O2 Zn1 O1 2_666 . 106.63(8) ?
O6 Zn1 O8 . 1_565 102.07(8) ?
O2 Zn1 O8 2_666 1_565 107.23(7) ?
O1 Zn1 O8 . 1_565 117.79(7) ?
O3 Zn2 O4 2_665 . 114.23(7) ?
O3 Zn2 O7 2_665 . 109.52(7) ?
O4 Zn2 O7 . . 106.65(6) ?
O3 Zn2 O5 2_665 2_665 114.45(8) ?
O4 Zn2 O5 . 2_665 104.69(7) ?
O7 Zn2 O5 . 2_665 106.73(7) ?
O9 Zn3 O9 2_656 . 180.0 ?
O9 Zn3 O10 2_656 . 85.46(7) ?
O9 Zn3 O10 . . 94.54(7) ?
O9 Zn3 O10 2_656 2_656 94.54(7) ?
O9 Zn3 O10 . 2_656 85.46(7) ?
O10 Zn3 O10 . 2_656 180.0 ?
O9 Zn3 O11 2_656 2_656 86.14(8) ?
O9 Zn3 O11 . 2_656 93.86(8) ?
O10 Zn3 O11 . 2_656 91.57(10) ?
O10 Zn3 O11 2_656 2_656 88.43(10) ?
O9 Zn3 O11 2_656 . 93.86(8) ?
O9 Zn3 O11 . . 86.14(8) ?
O10 Zn3 O11 . . 88.43(10) ?
O10 Zn3 O11 2_656 . 91.57(10) ?
O11 Zn3 O11 2_656 . 180.0(2) ?
O3 P1 O2 . . 109.52(10) ?
O3 P1 O1 . . 113.71(10) ?
O2 P1 O1 . . 113.08(10) ?
O3 P1 H1 . . 106.7 ?
O2 P1 H1 . . 106.7 ?
O1 P1 H1 . . 106.7 ?
O6 P2 O4 . . 109.10(10) ?
O6 P2 O5 . . 112.87(10) ?
O4 P2 O5 . . 113.41(10) ?
O6 P2 H2 . . 107.0 ?
O4 P2 H2 . . 107.0 ?
O5 P2 H2 . . 107.0 ?
O9 P3 O7 . . 111.59(10) ?
O9 P3 O8 . . 111.91(9) ?
O7 P3 O8 . . 109.55(8) ?
O9 P3 H3 . . 107.9 ?
O7 P3 H3 . . 107.9 ?
O8 P3 H3 . . 107.9 ?
P1 O1 Zn1 . . 127.86(10) yes
P1 O2 Zn1 . 2_666 129.28(10) yes
P1 O3 Zn2 . 2_665 128.74(11) yes
P2 O4 Zn2 . . 127.96(10) yes
P2 O5 Zn2 . 2_665 126.35(10) yes
P2 O6 Zn1 . . 125.97(10) yes
P3 O7 Zn2 . . 124.65(8) yes
P3 O8 Zn1 . 1_545 119.29(9) yes
P3 O9 Zn3 . . 143.17(12) yes
Zn3 O10 H8 . . 114.5 ?
Zn3 O10 H9 . . 114.5 ?
H8 O10 H9 . . 90.9 ?
Zn3 O11 H10 . . 125.1 ?
Zn3 O11 H11 . . 106.4 ?
H10 O11 H11 . . 101.0 ?
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
N1 H4 . 0.9525 ?
N1 H5 . 0.8048 ?
N1 H6 . 0.8733 ?
N1 H7 . 0.9526 ?
Zn1 O6 . 1.9283(16) yes
Zn1 O2 2_666 1.9325(15) yes
Zn1 O1 . 1.9462(17) yes
Zn1 O8 1_565 1.9583(15) yes
Zn2 O3 2_665 1.9079(16) yes
Zn2 O4 . 1.9365(15) yes
Zn2 O7 . 1.9480(14) yes
Zn2 O5 2_665 1.9529(17) yes
Zn3 O9 2_656 2.0014(14) yes
Zn3 O9 . 2.0014(14) yes
Zn3 O10 . 2.1290(19) yes
Zn3 O10 2_656 2.1290(19) yes
Zn3 O11 2_656 2.166(2) yes
Zn3 O11 . 2.166(2) yes
P1 O3 . 1.5050(17) yes
P1 O2 . 1.5140(16) yes
P1 O1 . 1.5260(17) yes
P1 H1 . 1.3200 ?
P2 O6 . 1.5104(18) yes
P2 O4 . 1.5114(16) yes
P2 O5 . 1.5281(16) yes
P2 H2 . 1.3200 ?
P3 O9 . 1.5079(16) yes
P3 O7 . 1.5197(15) yes
P3 O8 . 1.5219(15) yes
P3 H3 . 1.3200 ?
O10 H8 . 0.7717 ?
O10 H9 . 0.9566 ?
O11 H10 . 0.8084 ?
O11 H11 . 1.0981 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H4 O8 2 0.95 1.96 2.904(2) 169.7 yes
N1 H5 O9 2_655 0.80 2.23 3.035(3) 173.6 yes
N1 H6 O5 1_545 0.87 2.00 2.865(3) 173.4 yes
N1 H7 O7 . 0.95 1.94 2.887(2) 171.8 yes
O10 H8 O1 2_666 0.77 2.31 3.022(3) 154.3 yes
O10 H9 O4 . 0.96 2.08 3.004(3) 162.3 yes
O10 H9 O6 . 0.96 2.38 3.069(3) 128.9 yes
O11 H10 O2 . 0.81 2.00 2.742(2) 153.1 yes
O11 H11 O4 . 1.10 2.43 3.410(3) 148.4 yes
