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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/91/4339109.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_4339109
loop_
_publ_author_name
'Du, Yu'
'Pan, Qinhe'
'Li, Jiyang'
'Yu, Jihong'
'Xu, Ruren'
_publ_section_title
;
 Synthesis, structure, and photoluminescence property of a new layered
 zirconium phosphate |Co(dien)(2)|[Zr(4)H(8)P(5)O(26)] x 3H(2)O.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5847
_journal_page_last               5851
_journal_paper_doi               10.1021/ic061873i
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C4 H23 Co0.5 N3 O15 P0.5 Si2 Zr2'
_chemical_formula_weight         636.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 107.997(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1149(11)
_cell_length_b                   8.8183(8)
_cell_length_c                   17.3298(16)
_cell_measurement_temperature    273(2)
_cell_volume                     1760.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.898
_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  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10204
_diffrn_reflns_theta_full        27.81
_diffrn_reflns_theta_max         27.81
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    1.903
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.402
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-shaped
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.874
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         3747
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          2.457
_refine_ls_shift/su_mean         0.089
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0425P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                2683
_reflns_number_total             3747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061873isi20060929_023227.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C4 H23 Co0.50 N3 O15 P0.50 Si2 Zr2'
_cod_database_code               4339109
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
Zr1 Zr 0.09212(6) 0.45771(8) 0.14918(4) 0.0150(2) Uani 1 1 d .
Zr2 Zr -0.16127(6) 0.96819(8) 0.07541(4) 0.0160(2) Uani 1 1 d .
Co1 Co -0.5000 1.10379(17) 0.2500 0.0204(4) Uani 1 2 d S
P1 P 0.0000 0.1735(3) 0.2500 0.0304(8) Uani 1 2 d S
Si1 Si -0.17235(18) 0.6079(2) 0.15778(12) 0.0131(4) Uani 1 1 d .
Si2 Si 0.04780(18) 0.7608(2) 0.02028(12) 0.0111(4) Uani 1 1 d .
O1 O -0.1809(5) 0.7734(6) 0.1366(3) 0.0261(13) Uani 1 1 d .
O2 O 0.1590(5) 0.5874(6) 0.2532(3) 0.0320(15) Uani 1 1 d .
O3 O -0.1385(4) 1.1585(5) 0.0094(3) 0.0245(13) Uani 1 1 d .
O4 O -0.0699(6) 1.0737(6) 0.1805(3) 0.0421(17) Uani 1 1 d .
O5 O 0.0377(5) 0.3218(6) 0.0498(3) 0.0301(14) Uani 1 1 d .
O6 O -0.0162(4) 0.8720(5) 0.0574(3) 0.0191(12) Uani 1 1 d .
O7 O 0.0844(6) 0.2746(6) 0.2222(3) 0.0399(17) Uani 1 1 d .
O8 O 0.1134(4) 0.6454(5) 0.0833(3) 0.0224(13) Uani 1 1 d .
O9 O -0.0770(5) 0.5309(6) 0.1338(3) 0.0272(13) Uani 1 1 d .
O10 O -0.2895(5) 0.5334(7) 0.1094(4) 0.0419(17) Uani 1 1 d .
O11 O -0.3044(5) 1.0552(7) 0.0912(4) 0.0381(15) Uani 1 1 d U
O12 O 0.2537(4) 0.4083(5) 0.1541(3) 0.0183(12) Uani 1 1 d U
O13 O -0.2652(4) 0.8879(6) -0.0295(3) 0.0277(14) Uani 1 1 d .
O1W O -0.5218(14) 0.7794(15) 0.4005(9) 0.206(7) Uani 1 1 d .
O2W O -0.3133(5) 0.3912(7) -0.0260(4) 0.0409(16) Uani 1 1 d .
C1 C -0.6087(16) 0.821(2) 0.2587(12) 0.038(5) Uani 0.50 1 d P
C1' C -0.6172(18) 0.832(2) 0.1899(12) 0.043(5) Uani 0.50 1 d P
C2 C -0.7069(8) 0.9204(11) 0.2065(6) 0.039(2) Uani 1 1 d .
C3 C -0.4844(12) 1.3835(12) 0.1809(7) 0.052(3) Uani 1 1 d .
H3A H -0.413(9) 1.442(11) 0.197(7) 0.080 Uiso 1 1 calc .
H3B H -0.547(10) 1.454(12) 0.158(7) 0.080 Uiso 1 1 calc .
C4 C -0.4792(16) 1.2845(13) 0.1194(8) 0.085(6) Uani 1 1 d .
H4A H -0.403(9) 1.292(12) 0.112(7) 0.080 Uiso 1 1 calc .
H4B H -0.536(10) 1.315(12) 0.069(7) 0.080 Uiso 1 1 calc .
N1 N -0.5000 0.8825(10) 0.2500 0.023(2) Uani 1 2 d S
N2 N -0.6701(6) 1.0838(9) 0.2138(5) 0.034(2) Uani 1 1 d .
H2A H -0.699(9) 1.131(12) 0.249(6) 0.080 Uiso 1 1 calc .
H2B H -0.699(9) 1.130(12) 0.165(7) 0.080 Uiso 1 1 calc .
N3 N -0.5000 1.3202(12) 0.2500 0.067(4) Uani 1 2 d S
N4 N -0.5003(7) 1.1249(8) 0.1362(4) 0.0273(17) Uani 1 1 d .
H4C H -0.445(9) 1.066(12) 0.128(6) 0.080 Uiso 1 1 calc .
H4D H -0.569(9) 1.095(12) 0.102(6) 0.080 Uiso 1 1 calc .
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'
Co Co 0.3494 0.9721 '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'
Si Si 0.0817 0.0704 '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
O12 Zr1 O5 88.0(2) . .
O12 Zr1 O8 84.8(2) . .
O5 Zr1 O8 93.9(2) . .
O12 Zr1 O7 91.9(2) . .
O5 Zr1 O7 89.6(2) . .
O8 Zr1 O7 175.1(2) . .
O12 Zr1 O2 88.2(2) . .
O5 Zr1 O2 175.8(2) . .
O8 Zr1 O2 87.5(2) . .
O7 Zr1 O2 88.8(2) . .
O12 Zr1 O9 172.8(2) . .
O5 Zr1 O9 91.4(2) . .
O8 Zr1 O9 88.1(2) . .
O7 Zr1 O9 95.3(2) . .
O2 Zr1 O9 92.6(2) . .
O11 Zr2 O13 86.0(2) . .
O11 Zr2 O4 87.6(3) . .
O13 Zr2 O4 172.4(2) . .
O11 Zr2 O6 178.1(2) . .
O13 Zr2 O6 92.5(2) . .
O4 Zr2 O6 94.0(2) . .
O11 Zr2 O1 90.4(2) . .
O13 Zr2 O1 91.8(2) . .
O4 Zr2 O1 92.2(2) . .
O6 Zr2 O1 88.53(19) . .
O11 Zr2 O3 91.9(2) . .
O13 Zr2 O3 86.5(2) . .
O4 Zr2 O3 89.7(2) . .
O6 Zr2 O3 89.14(19) . .
O1 Zr2 O3 177.1(2) . .
N3 Co1 N1 180.000(3) . .
N3 Co1 N2 95.1(2) . 2_455
N1 Co1 N2 84.9(2) . 2_455
N3 Co1 N2 95.1(2) . .
N1 Co1 N2 84.9(2) . .
N2 Co1 N2 169.7(5) 2_455 .
N3 Co1 N4 84.6(2) . 2_455
N1 Co1 N4 95.4(2) . 2_455
N2 Co1 N4 90.6(3) 2_455 2_455
N2 Co1 N4 90.3(3) . 2_455
N3 Co1 N4 84.6(2) . .
N1 Co1 N4 95.4(2) . .
N2 Co1 N4 90.3(3) 2_455 .
N2 Co1 N4 90.6(3) . .
N4 Co1 N4 169.2(4) 2_455 .
O4 P1 O4 109.3(5) 2_545 1_545
O4 P1 O7 110.3(3) 2_545 2
O4 P1 O7 108.8(3) 1_545 2
O4 P1 O7 108.8(3) 2_545 .
O4 P1 O7 110.3(3) 1_545 .
O7 P1 O7 109.3(5) 2 .
O1 Si1 O9 111.8(3) . .
O1 Si1 O2 110.1(3) . 2
O9 Si1 O2 112.3(3) . 2
O1 Si1 O10 107.3(3) . .
O9 Si1 O10 108.1(3) . .
O2 Si1 O10 107.0(3) 2 .
O6 Si2 O5 109.8(3) . 3_565
O6 Si2 O8 110.6(3) . .
O5 Si2 O8 109.2(3) 3_565 .
O6 Si2 O3 111.0(3) . 3_575
O5 Si2 O3 109.7(3) 3_565 3_575
O8 Si2 O3 106.4(3) . 3_575
Si1 O1 Zr2 157.2(3) . .
Si1 O2 Zr1 147.3(3) 2 .
Si2 O3 Zr2 141.9(3) 3_575 .
P1 O4 Zr2 170.7(4) 1_565 .
Si2 O5 Zr1 157.5(4) 3_565 .
Si2 O6 Zr2 154.9(3) . .
P1 O7 Zr1 143.2(4) . .
Si2 O8 Zr1 143.3(3) . .
Si1 O9 Zr1 155.8(3) . .
C1' C1 N1 70.5(13) . .
C1' C1 C2 62.7(14) . .
N1 C1 C2 106.7(11) . .
C1 C1' C2 71.0(15) . .
C1 C1' N1 64.0(14) . .
C2 C1' N1 107.7(13) . .
C1' C2 N2 108.3(9) . .
C1' C2 C1 46.3(10) . .
N2 C2 C1 110.0(9) . .
N3 C3 C4 117.3(10) . .
N3 C3 H3A 112(8) . .
C4 C3 H3A 104(8) . .
N3 C3 H3B 122(8) . .
C4 C3 H3B 102(8) . .
H3A C3 H3B 96(10) . .
C3 C4 N4 113.3(9) . .
C3 C4 H4A 95(8) . .
N4 C4 H4A 122(8) . .
C3 C4 H4B 110(7) . .
N4 C4 H4B 113(7) . .
H4A C4 H4B 102(10) . .
C1 N1 C1 137.0(16) . 2_455
C1 N1 C1' 45.5(9) . .
C1 N1 C1' 119.4(11) 2_455 .
C1 N1 C1' 119.4(11) . 2_455
C1 N1 C1' 45.5(9) 2_455 2_455
C1' N1 C1' 146.6(16) . 2_455
C1 N1 Co1 111.5(8) . .
C1 N1 Co1 111.5(8) 2_455 .
C1' N1 Co1 106.7(8) . .
C1' N1 Co1 106.7(8) 2_455 .
C2 N2 Co1 111.5(5) . .
C2 N2 H2A 123(7) . .
Co1 N2 H2A 111(7) . .
C2 N2 H2B 95(7) . .
Co1 N2 H2B 111(7) . .
H2A N2 H2B 103(9) . .
C3 N3 C3 132.4(12) 2_455 .
C3 N3 Co1 113.8(6) 2_455 .
C3 N3 Co1 113.8(6) . .
C4 N4 Co1 109.8(6) . .
C4 N4 H4C 119(8) . .
Co1 N4 H4C 99(9) . .
C4 N4 H4D 116(6) . .
Co1 N4 H4D 104(6) . .
H4C N4 H4D 106(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O12 1.982(5) .
Zr1 O5 2.033(5) .
Zr1 O8 2.072(5) .
Zr1 O7 2.071(5) .
Zr1 O2 2.076(5) .
Zr1 O9 2.084(5) .
Zr2 O11 1.990(5) .
Zr2 O13 1.994(5) .
Zr2 O4 2.040(6) .
Zr2 O6 2.060(5) .
Zr2 O1 2.071(5) .
Zr2 O3 2.096(5) .
Co1 N3 1.908(10) .
Co1 N1 1.952(9) .
Co1 N2 1.968(7) 2_455
Co1 N2 1.968(7) .
Co1 N4 1.980(7) 2_455
Co1 N4 1.980(7) .
P1 O4 1.521(6) 2_545
P1 O4 1.521(6) 1_545
P1 O7 1.543(6) 2
P1 O7 1.543(6) .
Si1 O1 1.501(5) .
Si1 O9 1.506(5) .
Si1 O2 1.512(5) 2
Si1 O10 1.554(6) .
Si2 O6 1.512(5) .
Si2 O5 1.517(6) 3_565
Si2 O8 1.525(5) .
Si2 O3 1.526(5) 3_575
O2 Si1 1.512(5) 2
O3 Si2 1.526(5) 3_575
O4 P1 1.521(6) 1_565
O5 Si2 1.517(6) 3_565
C1 C1' 1.17(2) .
C1 N1 1.473(17) .
C1 C2 1.53(2) .
C1' C2 1.44(2) .
C1' N1 1.545(19) .
C2 N2 1.502(12) .
C3 N3 1.386(11) .
C3 C4 1.394(15) .
C3 H3A 0.79(10) .
C3 H3B 0.77(11) .
C4 N4 1.475(12) .
C4 H4A 0.83(10) .
C4 H4B 0.91(10) .
N1 C1 1.473(17) 2_455
N1 C1' 1.54(2) 2_455
N2 H2A 0.92(10) .
N2 H2B 0.86(11) .
N3 C3 1.386(11) 2_455
N4 H4C 0.71(11) .
N4 H4D 1.04(11) .
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
N2 H2B O13 0.86(11) 2.22(11) 3.055(10) 165(10) 3_475
N2 H2A O12 0.92(10) 2.61(10) 3.085(9) 113(8) 1_465
N4 H4C O11 0.71(11) 2.23(10) 2.787(9) 136(10) .
N4 H4C O1W 0.71(11) 2.63(10) 3.141(15) 131(10) 2_455
N4 H4D O13 1.04(11) 1.93(11) 2.873(9) 148(9) 3_475
