#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/47/7204746.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_7204746
loop_
_publ_author_name
'Neeraj, S.'
'Rao, C. N. R.'
'Cheetham, Anthony K.'
_publ_section_title
;
 Open-framework zinc and cobalt phosphates synthesized by the
 tributylphosphate routeElectronic supplementary information (ESI)
 available: Tables S1?16: Atomic coordinates, equivalent isotropic
 displacement parameters and bond lengths and angles for compounds
 I?VII. See http://www.rsc.org/suppdata/jm/b3/b311529a/
;
_journal_issue                   5
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              814
_journal_paper_doi               10.1039/b311529a
_journal_volume                  14
_journal_year                    2004
_chemical_formula_moiety         '[NH4][H3O][Zn4(PO4)3]2.H2O'
_chemical_formula_sum            'H2 N0.5 O13 P3 Zn4'
_chemical_formula_weight         571.41
_chemical_name_common            'Zinc Phosphate'
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_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                101.094(19)
_cell_angle_beta                 100.931(19)
_cell_angle_gamma                103.598(18)
_cell_formula_units_Z            2
_cell_length_a                   5.0400(9)
_cell_length_b                   9.584(3)
_cell_length_c                   13.117(2)
_cell_measurement_temperature    293(2)
_cell_volume                     585.7(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.867
_diffrn_measured_fraction_theta_max 0.867
_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  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3484
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    8.572
_exptl_crystal_density_diffrn    3.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             549
_refine_diff_density_max         1.514
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0456
_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)+(0.0658P)²+3.9700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1228
_reflns_number_gt                2327
_reflns_number_total             2529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b311529a.txt
_cod_data_source_block           COMPOUND_III
_cod_original_formula_sum        'H2 N0.50 O13 P3 Zn4'
_cod_database_code               7204746
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.44980(14) 0.02160(7) 0.79790(6) 0.01408(19) Uani 1 1 d . . .
Zn2 Zn 0.87434(14) -0.19176(8) 0.84527(6) 0.01430(19) Uani 1 1 d . . .
Zn3 Zn 0.05894(15) 0.34251(8) 0.72382(6) 0.01465(19) Uani 1 1 d . . .
Zn4 Zn 0.14456(14) -0.15780(8) 0.54017(5) 0.01392(19) Uani 1 1 d . . .
P1 P 0.2403(3) -0.32500(16) 0.71453(12) 0.0111(3) Uani 1 1 d . . .
P2 P 0.0448(3) 0.16685(16) 0.90468(12) 0.0122(3) Uani 1 1 d . . .
P3 P 0.4293(3) 0.17393(16) 0.60406(12) 0.0114(3) Uani 1 1 d . . .
O1 O 0.3329(9) 0.1518(5) 0.8962(4) 0.0212(10) Uani 1 1 d . . .
O2 O 0.8249(9) 0.0111(5) 0.8623(4) 0.0210(10) Uani 1 1 d . . .
O3 O 0.3717(9) 0.0306(5) 0.6458(3) 0.0161(9) Uani 1 1 d . . .
O4 O 0.2010(9) -0.1800(4) 0.7819(3) 0.0136(8) Uani 1 1 d . . .
O5 O -0.0620(10) 0.2623(5) 0.8349(4) 0.0212(10) Uani 1 1 d . . .
O6 O 0.0604(10) 0.5452(5) 0.7430(4) 0.0213(10) Uani 1 1 d . . .
O7 O 0.3885(9) 0.3002(5) 0.6830(4) 0.0201(9) Uani 1 1 d . . .
O8 O -0.2607(8) 0.2158(5) 0.5949(3) 0.0142(8) Uani 1 1 d . . .
O9 O 0.1361(11) -0.3303(5) 0.5964(4) 0.0251(10) Uani 1 1 d . . .
O10 O -0.2374(9) -0.1395(6) 0.5062(4) 0.0225(10) Uani 1 1 d . . .
O11 O 0.5494(10) -0.3180(6) 0.7385(5) 0.0306(12) Uani 1 1 d . . .
O12 O 0.0450(10) 0.2353(5) 1.0185(4) 0.0210(10) Uani 1 1 d . . .
N1 N 0.5000 -0.5000 0.5000 0.040(3) Uani 1 2 d S . .
O20 O -0.269(6) 0.4517(19) 0.964(3) 0.072(13) Uani 0.51(6) 1 d P . .
O20A O 0.582(9) 0.463(2) 0.898(3) 0.074(11) Uani 0.49(6) 1 d P . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O2 110.0(2) . . ?
O1 Zn1 O3 118.2(2) . . ?
O2 Zn1 O3 117.1(2) . . ?
O1 Zn1 O4 105.87(19) . . ?
O2 Zn1 O4 103.99(19) . . ?
O3 Zn1 O4 99.28(18) . . ?
O12 Zn2 O11 118.6(2) 2_657 . ?
O12 Zn2 O4 110.46(19) 2_657 1_655 ?
O11 Zn2 O4 107.6(2) . 1_655 ?
O12 Zn2 O2 110.2(2) 2_657 . ?
O11 Zn2 O2 105.2(2) . . ?
O4 Zn2 O2 103.62(18) 1_655 . ?
O5 Zn3 O6 111.5(2) . . ?
O5 Zn3 O7 117.7(2) . . ?
O6 Zn3 O7 114.3(2) . . ?
O5 Zn3 O8 99.9(2) . . ?
O6 Zn3 O8 109.3(2) . . ?
O7 Zn3 O8 102.26(18) . . ?
O9 Zn4 O10 108.3(2) . . ?
O9 Zn4 O3 113.2(2) . . ?
O10 Zn4 O3 105.3(2) . . ?
O9 Zn4 O8 101.6(2) . 2_556 ?
O10 Zn4 O8 109.53(19) . 2_556 ?
O3 Zn4 O8 118.60(18) . 2_556 ?
O6 P1 O11 113.0(3) 1_545 . ?
O6 P1 O9 110.3(3) 1_545 . ?
O11 P1 O9 109.5(3) . . ?
O6 P1 O4 107.2(2) 1_545 . ?
O11 P1 O4 109.3(3) . . ?
O9 P1 O4 107.3(3) . . ?
O12 P2 O1 111.5(3) . . ?
O12 P2 O5 107.1(3) . . ?
O1 P2 O5 113.1(3) . . ?
O12 P2 O2 110.5(3) . 1_455 ?
O1 P2 O2 109.2(3) . 1_455 ?
O5 P2 O2 105.2(3) . 1_455 ?
O10 P3 O7 113.3(3) 2_556 . ?
O10 P3 O8 108.6(3) 2_556 1_655 ?
O7 P3 O8 108.6(3) . 1_655 ?
O10 P3 O3 107.8(3) 2_556 . ?
O7 P3 O3 109.6(3) . . ?
O8 P3 O3 108.8(3) 1_655 . ?
P2 O1 Zn1 132.3(3) . . ?
P2 O2 Zn1 112.6(3) 1_655 . ?
P2 O2 Zn2 130.9(3) 1_655 . ?
Zn1 O2 Zn2 115.9(2) . . ?
P3 O3 Zn1 126.2(3) . . ?
P3 O3 Zn4 117.4(3) . . ?
Zn1 O3 Zn4 115.7(2) . . ?
P1 O4 Zn2 119.8(2) . 1_455 ?
P1 O4 Zn1 123.3(2) . . ?
Zn2 O4 Zn1 116.8(2) 1_455 . ?
P2 O5 Zn3 134.1(3) . . ?
P1 O6 Zn3 132.6(3) 1_565 . ?
P3 O7 Zn3 133.3(3) . . ?
P3 O8 Zn4 123.7(2) 1_455 2_556 ?
P3 O8 Zn3 121.0(2) 1_455 . ?
Zn4 O8 Zn3 115.25(19) 2_556 . ?
P1 O9 Zn4 124.4(3) . . ?
P3 O10 Zn4 126.5(3) 2_556 . ?
P1 O11 Zn2 133.8(3) . . ?
P2 O12 Zn2 137.2(3) . 2_657 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.893(5) . ?
Zn1 O2 1.953(5) . ?
Zn1 O3 1.981(4) . ?
Zn1 O4 1.988(4) . ?
Zn2 O12 1.903(5) 2_657 ?
Zn2 O11 1.911(5) . ?
Zn2 O4 1.970(4) 1_655 ?
Zn2 O2 1.993(5) . ?
Zn3 O5 1.907(5) . ?
Zn3 O6 1.908(4) . ?
Zn3 O7 1.944(4) . ?
Zn3 O8 2.046(4) . ?
Zn4 O9 1.930(5) . ?
Zn4 O10 1.949(5) . ?
Zn4 O3 1.989(4) . ?
Zn4 O8 1.989(4) 2_556 ?
P1 O6 1.512(4) 1_545 ?
P1 O11 1.512(5) . ?
P1 O9 1.526(5) . ?
P1 O4 1.573(4) . ?
P2 O12 1.511(5) . ?
P2 O1 1.515(5) . ?
P2 O5 1.526(5) . ?
P2 O2 1.560(5) 1_455 ?
P3 O10 1.508(5) 2_556 ?
P3 O7 1.515(5) . ?
P3 O8 1.553(4) 1_655 ?
P3 O3 1.561(4) . ?
O2 P2 1.560(5) 1_655 ?
O4 Zn2 1.970(4) 1_455 ?
O6 P1 1.512(4) 1_565 ?
O8 P3 1.553(4) 1_455 ?
O8 Zn4 1.989(4) 2_556 ?
O10 P3 1.508(5) 2_556 ?
O12 Zn2 1.903(5) 2_657 ?
O20 O20A 1.07(3) 1_455 ?
O20A O20 1.07(3) 1_655 ?
