#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:24:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179244 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/64/4316486.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_4316486
loop_
_publ_author_name
'Lei Liu'
'Zhao-Feng Chen'
'Hai-Bo Wei'
'Yang Li'
'Yu-Chuan Fu'
'Hong Xu'
'Jin-Ping Li'
'Alexandra M. Z. Slawin'
'Jin-Xiang Dong'
_publ_section_title
;
 Ionothermal Synthesis of Layered Zirconium Phosphates and Their
 Tribological Properties in Mineral Oil
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8270
_journal_page_last               8275
_journal_paper_doi               10.1021/ic100657a
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'H O8 P2 Zr, 0.5(C6 H16 N2), H2 O '
_chemical_formula_sum            'C3 H11 N O9 P2 Zr'
_chemical_formula_weight         358.29
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 109.236(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.372(5)
_cell_length_b                   10.613(4)
_cell_length_c                   9.281(5)
_cell_measurement_reflns_used    1588
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      54.91
_cell_measurement_theta_min      6.03
_cell_volume                     1057.6(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2004)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    PLATON(Spek,2003)
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6838
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.378
_exptl_absorpt_correction_T_max  0.9864
_exptl_absorpt_correction_T_min  0.9343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku,2004)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0536P)²+0.3075P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0979
_reflns_number_gt                1972
_reflns_number_total             2206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100657a_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               4316486
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Zr1 Zr 0.97269(3) 0.12474(2) 0.24038(3) 0.00769(14) Uani 1 1 d . . .
P1 P 0.83853(7) 0.38807(7) 0.02336(8) 0.00926(19) Uani 1 1 d . . .
P2 P 0.85141(7) -0.13549(6) 0.01022(8) 0.00867(19) Uani 1 1 d . . .
O1 O 0.85937(18) 0.25937(19) 0.1007(2) 0.0133(4) Uani 1 1 d . . .
O2 O 0.86346(18) -0.01036(19) 0.0967(2) 0.0138(4) Uani 1 1 d . . .
O5 O 0.8466(2) 0.12255(16) 0.3638(2) 0.0132(5) Uani 1 1 d . . .
O4 O 1.07984(19) 0.26021(18) 0.3811(2) 0.0144(4) Uani 1 1 d . . .
O3 O 1.07319(18) -0.01352(18) 0.3820(2) 0.0134(4) Uani 1 1 d . . .
O6 O 1.0910(2) 0.12145(17) 0.1166(2) 0.0175(5) Uani 1 1 d . . .
O9 O 0.3514(2) 0.1446(2) 0.3958(3) 0.0183(5) Uani 1 1 d . . .
O7 O 0.71268(18) -0.1663(2) -0.0613(2) 0.0151(4) Uani 1 1 d . . .
O8 O 0.70118(18) 0.4269(2) 0.0065(2) 0.0155(4) Uani 1 1 d . . .
H8 H 0.7013 0.4983 0.0455 0.023 Uiso 1 1 calc R . .
C2 C 0.5834(3) 0.1039(3) 0.0472(4) 0.0214(7) Uani 1 1 d . . .
H2A H 0.5245 0.1755 0.0310 0.026 Uiso 1 1 calc R . .
H2B H 0.6691 0.1378 0.0882 0.026 Uiso 1 1 calc R . .
N1 N 0.5662(2) 0.0398(2) -0.1007(3) 0.0211(6) Uani 1 1 d . . .
H1 H 0.6227 -0.0265 -0.0829 0.025 Uiso 1 1 calc R . .
C3 C 0.5929(5) 0.1283(3) -0.2129(5) 0.0435(12) Uani 1 1 d . . .
H3A H 0.5733 0.0866 -0.3122 0.065 Uiso 1 1 calc R . .
H3B H 0.6812 0.1518 -0.1760 0.065 Uiso 1 1 calc R . .
H3C H 0.5416 0.2042 -0.2235 0.065 Uiso 1 1 calc R . .
C1 C 0.4389(3) -0.0136(3) -0.1600(3) 0.0211(7) Uani 1 1 d . . .
H1A H 0.4280 -0.0579 -0.2574 0.025 Uiso 1 1 calc R . .
H1B H 0.3771 0.0555 -0.1804 0.025 Uiso 1 1 calc R . .
H9A H 0.321(3) 0.207(4) 0.446(4) 0.036(10) Uiso 1 1 d . . .
H9B H 0.319(4) 0.158(3) 0.303(5) 0.028(10) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Zr1 O3 90.98(8) . . ?
O6 Zr1 O4 90.39(8) . . ?
O3 Zr1 O4 90.28(9) . . ?
O6 Zr1 O1 92.82(8) . . ?
O3 Zr1 O1 175.66(8) . . ?
O4 Zr1 O1 91.81(9) . . ?
O6 Zr1 O2 89.56(8) . . ?
O3 Zr1 O2 90.38(9) . . ?
O4 Zr1 O2 179.34(7) . . ?
O1 Zr1 O2 87.54(9) . . ?
O6 Zr1 O5 177.90(7) . . ?
O3 Zr1 O5 88.80(8) . . ?
O4 Zr1 O5 91.69(8) . . ?
O1 Zr1 O5 87.33(8) . . ?
O2 Zr1 O5 88.35(8) . . ?
O3 P1 O5 112.07(11) 2_755 4_565 ?
O3 P1 O1 112.00(12) 2_755 . ?
O5 P1 O1 110.05(11) 4_565 . ?
O3 P1 O8 108.92(12) 2_755 . ?
O5 P1 O8 107.47(12) 4_565 . ?
O1 P1 O8 106.05(12) . . ?
O4 P2 O6 108.82(12) 2_745 3_755 ?
O4 P2 O7 111.20(12) 2_745 . ?
O6 P2 O7 109.15(12) 3_755 . ?
O4 P2 O2 110.09(12) 2_745 . ?
O6 P2 O2 109.31(11) 3_755 . ?
O7 P2 O2 108.24(12) . . ?
P1 O1 Zr1 151.83(13) . . ?
P2 O2 Zr1 150.19(13) . . ?
P1 O5 Zr1 143.24(14) 4_566 . ?
P2 O4 Zr1 174.50(13) 2_755 . ?
P1 O3 Zr1 171.94(13) 2_745 . ?
P2 O6 Zr1 163.98(14) 3_755 . ?
N1 C2 C1 110.5(2) . 3_655 ?
C1 N1 C2 109.5(2) . . ?
C1 N1 C3 112.1(3) . . ?
C2 N1 C3 110.9(3) . . ?
N1 C1 C2 110.7(2) . 3_655 ?
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
Zr1 O6 2.037(2) . ?
Zr1 O3 2.049(2) . ?
Zr1 O4 2.051(2) . ?
Zr1 O1 2.069(2) . ?
Zr1 O2 2.070(2) . ?
Zr1 O5 2.109(2) . ?
P1 O3 1.513(2) 2_755 ?
P1 O5 1.518(2) 4_565 ?
P1 O1 1.525(2) . ?
P1 O8 1.573(2) . ?
P2 O4 1.528(2) 2_745 ?
P2 O6 1.532(2) 3_755 ?
P2 O7 1.532(2) . ?
P2 O2 1.534(2) . ?
O5 P1 1.518(2) 4_566 ?
O4 P2 1.528(2) 2_755 ?
O3 P1 1.513(2) 2_745 ?
O6 P2 1.532(2) 3_755 ?
C2 N1 1.486(4) . ?
C2 C1 1.502(4) 3_655 ?
N1 C1 1.481(4) . ?
N1 C3 1.506(4) . ?
C1 C2 1.502(4) 3_655 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O7 0.93 1.78 2.700(3) 172.2 .
O8 H8 O9 0.84 1.81 2.622(3) 161.7 2_655
O9 H9A O7 0.94(4) 1.84(4) 2.768(3) 171(3) 2_655
O9 H9A O4 0.94(4) 2.66(4) 3.284(3) 124(3) 1_455
O9 H9B O7 0.83(4) 2.16(4) 2.954(3) 162(4) 3_655
O9 H9B O6 0.83(4) 2.63(4) 3.239(3) 132(3) 1_455
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 P1 O1 Zr1 -31.2(3) 2_755 . . . ?
O5 P1 O1 Zr1 94.2(3) 4_565 . . . ?
O8 P1 O1 Zr1 -149.9(2) . . . . ?
O6 Zr1 O1 P1 -55.9(3) . . . . ?
O3 Zr1 O1 P1 153.2(8) . . . . ?
O4 Zr1 O1 P1 34.6(3) . . . . ?
O2 Zr1 O1 P1 -145.3(2) . . . . ?
O5 Zr1 O1 P1 126.2(3) . . . . ?
O4 P2 O2 Zr1 51.7(3) 2_745 . . . ?
O6 P2 O2 Zr1 -67.8(3) 3_755 . . . ?
O7 P2 O2 Zr1 173.4(2) . . . . ?
O6 Zr1 O2 P2 46.6(2) . . . . ?
O3 Zr1 O2 P2 -44.4(2) . . . . ?
O4 Zr1 O2 P2 133(6) . . . . ?
O1 Zr1 O2 P2 139.5(2) . . . . ?
O5 Zr1 O2 P2 -133.2(2) . . . . ?
O6 Zr1 O5 P1 123.4(19) . . . 4_566 ?
O3 Zr1 O5 P1 39.47(18) . . . 4_566 ?
O4 Zr1 O5 P1 -50.77(18) . . . 4_566 ?
O1 Zr1 O5 P1 -142.50(19) . . . 4_566 ?
O2 Zr1 O5 P1 129.89(18) . . . 4_566 ?
O6 Zr1 O4 P2 157.9(13) . . . 2_755 ?
O3 Zr1 O4 P2 -111.1(13) . . . 2_755 ?
O1 Zr1 O4 P2 65.1(13) . . . 2_755 ?
O2 Zr1 O4 P2 72(7) . . . 2_755 ?
O5 Zr1 O4 P2 -22.3(13) . . . 2_755 ?
O6 Zr1 O3 P1 13.5(9) . . . 2_745 ?
O4 Zr1 O3 P1 -76.8(9) . . . 2_745 ?
O1 Zr1 O3 P1 164.5(8) . . . 2_745 ?
O2 Zr1 O3 P1 103.1(9) . . . 2_745 ?
O5 Zr1 O3 P1 -168.5(9) . . . 2_745 ?
O3 Zr1 O6 P2 158.6(4) . . . 3_755 ?
O4 Zr1 O6 P2 -111.1(4) . . . 3_755 ?
O1 Zr1 O6 P2 -19.3(4) . . . 3_755 ?
O2 Zr1 O6 P2 68.2(4) . . . 3_755 ?
O5 Zr1 O6 P2 75(2) . . . 3_755 ?
C1 C2 N1 C1 57.8(3) 3_655 . . . ?
C1 C2 N1 C3 -177.9(3) 3_655 . . . ?
C2 N1 C1 C2 -58.0(3) . . . 3_655 ?
C3 N1 C1 C2 178.5(2) . . . 3_655 ?
