#------------------------------------------------------------------------------
#$Date: 2013-12-28 14:58:47 +0100 (Sat, 28 Dec 2013) $
#$Revision: 91933 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/26/2012691.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_2012691
loop_
_publ_author_name
'Ben Smail, Ridha'
'Jouini, Tahar'
_publ_section_title
;
 AgNi~3~(PO~4~)(HPO~4~)~2~: an alluaudite-like structure
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i61
_journal_page_last               i62
_journal_volume                  58
_journal_year                    2002
_chemical_formula_structural     'Ag Ni3 (P O4) (H P O4)2'
_chemical_formula_sum            'Ag H2 Ni3 O12 P3'
_chemical_formula_weight         570.93
_chemical_name_systematic
;
Silver trinickel phosphate bis(hydrogenphosphate)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 113.82(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.865(4)
_cell_length_b                   12.117(3)
_cell_length_c                   6.467(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.88
_cell_measurement_theta_min      6.55
_cell_volume                     850.6(5)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection
'CAD-4 EXPRESS (Duisenberg, 1992; Mac\'i\<cek & Yordanov, 1992)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1998)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_av_sigmaI/netI    0.010
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1012
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        0.98
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    9.449
_exptl_absorpt_correction_T_max  0.221
_exptl_absorpt_correction_T_min  0.119
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            brown-yellow
_exptl_crystal_density_diffrn    4.458
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.87
_refine_diff_density_min         -1.07
_refine_ls_extinction_coef       0.0112(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.020
_refine_ls_R_factor_gt           0.020
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0174P)^2^+8.9075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.051
_refine_ls_wR_factor_ref         0.051
_reflns_number_gt                916
_reflns_number_total             928
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    br1359.cif
_[local]_cod_data_source_block   I
_[local]_cod_cif_authors_sg_H-M  'C 2/c'
_cod_original_cell_volume        850.6(4)
_cod_database_code               2012691
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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
Ag 0.0000 0.46944(4) 0.2500 0.01576(15) Uani d S 1 . . Ag
Ni1 0.5000 0.27617(5) 0.2500 0.00488(16) Uani d S 1 . . Ni
Ni2 0.28914(4) 0.16290(3) 0.37743(7) 0.00391(15) Uani d . 1 . . Ni
P1 0.0000 0.18445(10) 0.2500 0.0031(2) Uani d S 1 . . P
P2 0.22359(8) 0.38701(7) 0.11454(14) 0.00311(18) Uani d . 1 . . P
O1 0.1079(2) 0.10763(19) 0.2648(4) 0.0063(5) Uani d . 1 . . O
O2 0.0354(2) 0.25737(19) 0.4643(4) 0.0050(5) Uani d . 1 . . O
O3 0.3430(2) 0.17260(19) 0.1127(4) 0.0052(5) Uani d . 1 . . O
O4 0.2178(2) 0.31833(19) 0.3092(4) 0.0052(5) Uani d . 1 . . O
O5 0.3362(2) 0.00011(19) 0.3945(4) 0.0069(5) Uani d . 1 . . O
O6 0.3631(2) 0.4049(2) 0.1578(4) 0.0057(5) Uani d . 1 . . O
H 0.371(9) 0.480(8) 0.176(17) 0.10(3) Uiso d . 1 . . H
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
Ag 0.0063(2) 0.0284(3) 0.0109(2) 0.000 0.00180(16) 0.000
Ni1 0.0046(3) 0.0053(3) 0.0056(3) 0.000 0.0029(2) 0.000
Ni2 0.0041(2) 0.0036(2) 0.0048(2) 0.00018(15) 0.00269(17) 0.00007(15)
P1 0.0019(5) 0.0036(5) 0.0038(5) 0.000 0.0009(4) 0.000
P2 0.0036(4) 0.0020(4) 0.0042(4) -0.0003(3) 0.0021(3) -0.0003(3)
O1 0.0031(11) 0.0039(11) 0.0126(12) 0.0006(8) 0.0037(9) -0.0011(9)
O2 0.0058(11) 0.0062(11) 0.0035(10) -0.0002(9) 0.0023(9) -0.0006(8)
O3 0.0061(11) 0.0069(11) 0.0042(11) -0.0015(8) 0.0037(9) -0.0011(8)
O4 0.0067(11) 0.0055(11) 0.0048(11) -0.0007(9) 0.0037(9) 0.0009(8)
O5 0.0063(11) 0.0040(11) 0.0108(12) 0.0004(9) 0.0039(10) 0.0003(9)
O6 0.0037(11) 0.0034(11) 0.0112(12) 0.0004(9) 0.0041(9) -0.0010(9)
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
Ag O5 7_556 2.364(3) y
Ag O5 8_455 2.364(3) n
Ag O5 3_455 2.501(3) n
Ag O5 4 2.501(3) y
Ni1 O2 7_556 2.093(2) n
Ni1 O2 8 2.093(2) y
Ni1 O3 . 2.121(2) y
Ni1 O3 2_655 2.121(2) n
Ni1 O6 2_655 2.155(2) n
Ni1 O6 . 2.155(2) y
Ni2 O4 . 2.039(2) y
Ni2 O5 . 2.041(2) y
Ni2 O3 . 2.058(2) y
Ni2 O4 7_556 2.074(2) y
Ni2 O1 . 2.083(2) y
Ni2 O2 7_556 2.144(3) y
P1 O2 . 1.551(2) y
P1 O2 2 1.551(2) n
P1 O1 2 1.554(2) n
P1 O1 . 1.554(2) y
P2 O5 4 1.533(2) y
P2 O4 . 1.534(2) y
P2 O3 7 1.539(2) y
P2 O6 . 1.578(3) y
O6 H . 0.90(10) n
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'
Ni Ni 0.3393 1.1124 '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'
Ag Ag -0.8971 1.1015 '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'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-1 1 4
-1 7 1
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
O5 Ag O5 7_556 8_455 162.04(12) n
O5 Ag O5 7_556 3_455 94.07(9) n
O5 Ag O5 8_455 3_455 83.26(8) n
O5 Ag O5 7_556 4 83.26(8) n
O5 Ag O5 8_455 4 94.07(9) n
O5 Ag O5 3_455 4 162.91(11) n
O2 Ni1 O2 7_556 8 157.61(13) n
O2 Ni1 O3 7_556 . 78.43(9) n
O2 Ni1 O3 8 . 88.33(9) n
O2 Ni1 O3 7_556 2_655 88.33(9) n
O2 Ni1 O3 8 2_655 78.43(9) n
O3 Ni1 O3 . 2_655 107.44(13) n
O2 Ni1 O6 7_556 2_655 107.08(9) n
O2 Ni1 O6 8 2_655 89.27(9) n
O3 Ni1 O6 . 2_655 168.70(9) n
O3 Ni1 O6 2_655 2_655 82.86(9) n
O2 Ni1 O6 7_556 . 89.27(9) n
O2 Ni1 O6 8 . 107.08(9) n
O3 Ni1 O6 . . 82.86(9) n
O3 Ni1 O6 2_655 . 168.70(9) n
O6 Ni1 O6 2_655 . 87.30(13) n
O4 Ni2 O5 . . 170.12(10) n
O4 Ni2 O3 . . 90.49(9) n
O5 Ni2 O3 . . 85.99(10) n
O4 Ni2 O4 . 7_556 86.18(10) n
O5 Ni2 O4 . 7_556 99.85(10) n
O3 Ni2 O4 . 7_556 162.69(10) n
O4 Ni2 O1 . . 86.63(10) n
O5 Ni2 O1 . . 85.96(10) n
O3 Ni2 O1 . . 110.55(10) n
O4 Ni2 O1 7_556 . 86.23(10) n
O4 Ni2 O2 . 7_556 85.73(10) n
O5 Ni2 O2 . 7_556 102.59(10) n
O3 Ni2 O2 . 7_556 78.67(10) n
O4 Ni2 O2 7_556 7_556 84.14(9) n
O1 Ni2 O2 . 7_556 168.08(9) n
O2 P1 O2 . 2 110.57(19) n
O2 P1 O1 . 2 108.37(13) n
O2 P1 O1 2 2 111.54(13) n
O2 P1 O1 . . 111.54(13) n
O2 P1 O1 2 . 108.37(13) n
O1 P1 O1 2 . 106.40(19) n
O5 P2 O4 4 . 110.04(14) n
O5 P2 O3 4 7 109.38(14) n
O4 P2 O3 . 7 110.67(14) n
O5 P2 O6 4 . 108.69(14) n
O4 P2 O6 . . 108.70(14) n
O3 P2 O6 7 . 109.32(14) n
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
O6 H O1 4_555 0.90(10) 1.50(10) 2.503(3) 174(10) yes
_cod_database_fobs_code 2012691
_journal_paper_doi 10.1107/S0108270102003153