#------------------------------------------------------------------------------
#$Date: 2016-03-22 14:06:56 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178985 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/08/4120804.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_4120804
loop_
_publ_author_name
'Hai-Long Jiang'
'Dawei Feng'
'Kecheng Wang'
'Zhi-Yuan Gu'
'Zhangwen Wei'
'Ying-Pin Chen'
'Hong-Cai Zhou'
_publ_section_title
;
 An Exceptionally Stable, Porphyrinic Zr Metal-Organic Framework
 Exhibiting pH-Dependent Fluorescence
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13934
_journal_page_last               13938
_journal_paper_doi               10.1021/ja406844r
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C48 H26 N4 O16 Zr3'
_chemical_formula_sum            'C48 H26 N4 O16 Zr3'
_chemical_formula_weight         1188.39
_chemical_name_common            PCN225
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           141
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.581(5)
_cell_length_b                   16.581(5)
_cell_length_c                   78.30(2)
_cell_measurement_reflns_used    6225
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      20.34
_cell_measurement_theta_min      2.20
_cell_volume                     21527(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.1036
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       97
_diffrn_reflns_limit_l_min       -97
_diffrn_reflns_number            102518
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.319
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_density_diffrn    0.733
_exptl_crystal_F_000             4720
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         5921
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.0557
_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)+(0.0936P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1709
_reflns_number_gt                3333
_reflns_number_total             5921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406844r_si_002.cif
_cod_data_source_block           e:\xray\pcn225~1\work\1
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               4120804
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z'
'-x, y+1/2, -z'
'y+1/4, x+3/4, -z+1/4'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z'
'x, -y-1/2, z'
'-y-1/4, -x-3/4, z-1/4'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'y+1/4, x+1/4, z-1/4'
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 0.5000 0.2500 0.093879(7) 0.0615(2) Uani 1 4 d S . .
Zr2 Zr 0.39348(2) 0.35652(2) 0.1250 0.0765(2) Uani 1 2 d S . .
O1 O 0.34398(17) 0.3915(2) 0.09881(3) 0.1048(10) Uani 1 1 d . . .
O2 O 0.41913(17) 0.32824(19) 0.07943(3) 0.0868(8) Uani 1 1 d . . .
O3 O 0.40978(18) 0.2500 0.11150(3) 0.0628(9) Uani 1 2 d S . .
O4 O 0.5000 0.37229(19) 0.10779(3) 0.0697(10) Uani 1 2 d S . .
O5 O 0.4016(2) 0.48777(19) 0.12406(3) 0.1265(13) Uani 1 1 d . . .
N1 N 0.0000 0.4799(4) 0.02595(7) 0.145(3) Uani 1 2 d S . .
H1 H 0.0000 0.4979 0.0154 0.174 Uiso 0.24(4) 1 calc PR A 1
N2 N 0.1244(3) 0.5000 0.0000 0.132(3) Uani 1 2 d S . .
H2 H 0.0714 0.5000 0.0000 0.159 Uiso 0.26(4) 1 calc PR A 2
C1 C 0.3623(3) 0.3730(3) 0.08374(5) 0.0924(14) Uani 1 1 d . . .
C2 C 0.3122(2) 0.4033(3) 0.06955(4) 0.0926(14) Uani 1 1 d D . .
C3 C 0.3108(2) 0.3613(2) 0.05426(4) 0.1035(16) Uani 1 1 d D . .
H3 H 0.3451 0.3160 0.0526 0.124 Uiso 1 1 calc R . .
C4 C 0.2587(3) 0.3858(3) 0.04139(4) 0.1129(16) Uani 1 1 d D . .
H4 H 0.2579 0.3574 0.0309 0.136 Uiso 1 1 calc R . .
C5 C 0.2079(2) 0.4514(3) 0.04372(5) 0.1141(18) Uani 1 1 d D . .
C6 C 0.2110(2) 0.4940(3) 0.05899(5) 0.124(2) Uani 1 1 d D . .
H6 H 0.1780 0.5403 0.0606 0.149 Uiso 1 1 calc R . .
C7 C 0.2626(3) 0.4687(3) 0.07203(5) 0.1153(18) Uani 1 1 d D . .
H7 H 0.2633 0.4967 0.0826 0.138 Uiso 1 1 calc R . .
C8 C 0.1475(3) 0.4716(4) 0.03072(5) 0.130(2) Uani 1 1 d . . .
C9 C 0.1740(2) 0.4861(4) 0.01378(6) 0.127(2) Uani 1 1 d . . .
C10 C 0.2542(3) 0.4918(4) 0.00840(6) 0.140(2) Uani 1 1 d . . .
H10 H 0.3005 0.4853 0.0154 0.168 Uiso 1 1 calc R . .
C11 C 0.0670(3) 0.4635(4) 0.03561(5) 0.144(2) Uani 1 1 d . . .
C12 C 0.0397(3) 0.4306(5) 0.05148(6) 0.192(4) Uani 1 1 d . . .
H12 H 0.0732 0.4119 0.0605 0.230 Uiso 1 1 calc R . .
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'
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
O3 Zr1 O3 94.63(16) 3_655 .
O3 Zr1 O2 143.44(8) 3_655 .
O3 Zr1 O2 84.24(10) . .
O3 Zr1 O2 143.44(8) 3_655 22_565
O3 Zr1 O2 84.24(10) . 22_565
O2 Zr1 O2 72.96(15) . 22_565
O3 Zr1 O2 84.24(10) 3_655 21_655
O3 Zr1 O2 143.44(8) . 21_655
O2 Zr1 O2 75.85(14) . 21_655
O2 Zr1 O2 117.55(14) 22_565 21_655
O3 Zr1 O2 84.24(10) 3_655 3_655
O3 Zr1 O2 143.44(8) . 3_655
O2 Zr1 O2 117.55(14) . 3_655
O2 Zr1 O2 75.85(14) 22_565 3_655
O2 Zr1 O2 72.96(15) 21_655 3_655
O3 Zr1 O4 71.29(5) 3_655 3_655
O3 Zr1 O4 71.29(5) . 3_655
O2 Zr1 O4 140.27(8) . 3_655
O2 Zr1 O4 73.83(9) 22_565 3_655
O2 Zr1 O4 140.27(8) 21_655 3_655
O2 Zr1 O4 73.83(9) 3_655 3_655
O3 Zr1 O4 71.29(5) 3_655 .
O3 Zr1 O4 71.29(5) . .
O2 Zr1 O4 73.83(9) . .
O2 Zr1 O4 140.27(8) 22_565 .
O2 Zr1 O4 73.83(9) 21_655 .
O2 Zr1 O4 140.27(8) 3_655 .
O4 Zr1 O4 123.52(14) 3_655 .
O3 Zr1 Zr2 84.18(7) 3_655 .
O3 Zr1 Zr2 32.27(3) . .
O2 Zr1 Zr2 75.52(7) . .
O2 Zr1 Zr2 110.60(7) 22_565 .
O2 Zr1 Zr2 111.85(8) 21_655 .
O2 Zr1 Zr2 166.91(7) 3_655 .
O4 Zr1 Zr2 96.63(6) 3_655 .
O4 Zr1 Zr2 39.07(4) . .
O3 Zr1 Zr2 32.28(3) 3_655 26_565
O3 Zr1 Zr2 84.18(7) . 26_565
O2 Zr1 Zr2 111.85(8) . 26_565
O2 Zr1 Zr2 166.91(7) 22_565 26_565
O2 Zr1 Zr2 75.52(7) 21_655 26_565
O2 Zr1 Zr2 110.60(7) 3_655 26_565
O4 Zr1 Zr2 96.63(6) 3_655 26_565
O4 Zr1 Zr2 39.07(4) . 26_565
Zr2 Zr1 Zr2 60.813(16) . 26_565
O3 Zr1 Zr2 32.28(3) 3_655 3_655
O3 Zr1 Zr2 84.18(7) . 3_655
O2 Zr1 Zr2 166.91(7) . 3_655
O2 Zr1 Zr2 111.85(8) 22_565 3_655
O2 Zr1 Zr2 110.60(7) 21_655 3_655
O2 Zr1 Zr2 75.52(7) 3_655 3_655
O4 Zr1 Zr2 39.08(4) 3_655 3_655
O4 Zr1 Zr2 96.63(6) . 3_655
Zr2 Zr1 Zr2 91.41(3) . 3_655
Zr2 Zr1 Zr2 60.813(16) 26_565 3_655
O3 Zr1 Zr2 84.19(7) 3_655 20_656
O3 Zr1 Zr2 32.27(3) . 20_656
O2 Zr1 Zr2 110.60(7) . 20_656
O2 Zr1 Zr2 75.52(7) 22_565 20_656
O2 Zr1 Zr2 166.91(7) 21_655 20_656
O2 Zr1 Zr2 111.85(8) 3_655 20_656
O4 Zr1 Zr2 39.08(4) 3_655 20_656
O4 Zr1 Zr2 96.63(6) . 20_656
Zr2 Zr1 Zr2 60.813(16) . 20_656
Zr2 Zr1 Zr2 91.41(3) 26_565 20_656
Zr2 Zr1 Zr2 60.813(16) 3_655 20_656
O3 Zr2 O3 92.17(16) . 26_565
O3 Zr2 O5 95.40(13) . 16_554
O3 Zr2 O5 145.43(9) 26_565 16_554
O3 Zr2 O5 145.43(9) . .
O3 Zr2 O5 95.41(13) 26_565 .
O5 Zr2 O5 97.2(2) 16_554 .
O3 Zr2 O4 71.94(11) . .
O3 Zr2 O4 69.54(8) 26_565 .
O5 Zr2 O4 144.59(9) 16_554 .
O5 Zr2 O4 79.29(12) . .
O3 Zr2 O4 69.53(8) . 20_656
O3 Zr2 O4 71.93(11) 26_565 20_656
O5 Zr2 O4 79.29(12) 16_554 20_656
O5 Zr2 O4 144.59(9) . 20_656
O4 Zr2 O4 123.20(15) . 20_656
O3 Zr2 O1 78.78(11) . .
O3 Zr2 O1 142.77(9) 26_565 .
O5 Zr2 O1 71.78(10) 16_554 .
O5 Zr2 O1 74.87(11) . .
O4 Zr2 O1 73.33(9) . .
O4 Zr2 O1 134.38(11) 20_656 .
O3 Zr2 O1 142.76(9) . 16_554
O3 Zr2 O1 78.77(11) 26_565 16_554
O5 Zr2 O1 74.87(11) 16_554 16_554
O5 Zr2 O1 71.79(10) . 16_554
O4 Zr2 O1 134.37(11) . 16_554
O4 Zr2 O1 73.33(9) 20_656 16_554
O1 Zr2 O1 128.61(14) . 16_554
O3 Zr2 Zr1 31.57(7) . .
O3 Zr2 Zr1 81.91(7) 26_565 .
O5 Zr2 Zr1 119.80(8) 16_554 .
O5 Zr2 Zr1 116.74(8) . .
O4 Zr2 Zr1 40.43(8) . .
O4 Zr2 Zr1 94.61(6) 20_656 .
O1 Zr2 Zr1 71.53(7) . .
O1 Zr2 Zr1 159.63(7) 16_554 .
O3 Zr2 Zr1 81.90(7) . 26_565
O3 Zr2 Zr1 31.56(7) 26_565 26_565
O5 Zr2 Zr1 116.74(8) 16_554 26_565
O5 Zr2 Zr1 119.80(8) . 26_565
O4 Zr2 Zr1 94.61(6) . 26_565
O4 Zr2 Zr1 40.43(8) 20_656 26_565
O1 Zr2 Zr1 159.63(7) . 26_565
O1 Zr2 Zr1 71.53(7) 16_554 26_565
Zr1 Zr2 Zr1 88.59(3) . 26_565
O3 Zr2 Zr2 31.71(6) . 20_656
O3 Zr2 Zr2 82.52(8) 26_565 20_656
O5 Zr2 Zr2 86.45(10) 16_554 20_656
O5 Zr2 Zr2 175.95(10) . 20_656
O4 Zr2 Zr2 96.71(8) . 20_656
O4 Zr2 Zr2 37.86(6) 20_656 20_656
O1 Zr2 Zr2 104.70(8) . 20_656
O1 Zr2 Zr2 111.07(7) 16_554 20_656
Zr1 Zr2 Zr2 59.594(8) . 20_656
Zr1 Zr2 Zr2 59.594(8) 26_565 20_656
O3 Zr2 Zr2 82.52(8) . 26_565
O3 Zr2 Zr2 31.71(6) 26_565 26_565
O5 Zr2 Zr2 175.96(10) 16_554 26_565
O5 Zr2 Zr2 86.45(10) . 26_565
O4 Zr2 Zr2 37.86(6) . 26_565
O4 Zr2 Zr2 96.71(8) 20_656 26_565
O1 Zr2 Zr2 111.07(7) . 26_565
O1 Zr2 Zr2 104.70(8) 16_554 26_565
Zr1 Zr2 Zr2 59.594(8) . 26_565
Zr1 Zr2 Zr2 59.594(8) 26_565 26_565
Zr2 Zr2 Zr2 90.0 20_656 26_565
C1 O1 Zr2 134.0(3) . .
C1 O2 Zr1 132.7(2) . .
Zr1 O3 Zr2 116.16(8) . .
Zr1 O3 Zr2 116.16(8) . 20_656
Zr2 O3 Zr2 116.59(12) . 20_656
Zr2 O4 Zr2 104.28(11) . 26_565
Zr2 O4 Zr1 100.49(10) . .
Zr2 O4 Zr1 100.49(10) 26_565 .
C11 N1 C11 108.2(5) . 21
C9 N2 C9 106.6(5) . 5_565
O2 C1 O1 125.6(4) . .
O2 C1 C2 115.1(4) . .
O1 C1 C2 119.2(4) . .
C7 C2 C3 120.5(3) . .
C7 C2 C1 120.0(4) . .
C3 C2 C1 119.3(4) . .
C2 C3 C4 119.4(4) . .
C3 C4 C5 120.8(4) . .
C6 C5 C4 119.3(3) . .
C6 C5 C8 120.4(5) . .
C4 C5 C8 120.2(5) . .
C5 C6 C7 119.9(4) . .
C2 C7 C6 120.0(4) . .
C11 C8 C9 124.7(4) . .
C11 C8 C5 116.2(3) . .
C9 C8 C5 118.4(4) . .
N2 C9 C10 108.7(4) . .
N2 C9 C8 125.2(4) . .
C10 C9 C8 126.0(4) . .
C10 C10 C9 108.0(2) 5_565 .
N1 C11 C8 127.2(3) . .
N1 C11 C12 107.4(4) . .
C8 C11 C12 125.3(4) . .
C12 C12 C11 108.4(2) 21 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O3 2.035(3) 3_655
Zr1 O3 2.035(3) .
Zr1 O2 2.182(3) .
Zr1 O2 2.182(3) 22_565
Zr1 O2 2.182(3) 21_655
Zr1 O2 2.182(3) 3_655
Zr1 O4 2.302(3) 3_655
Zr1 O4 2.302(3) .
Zr1 Zr2 3.4895(9) .
Zr1 Zr2 3.4895(9) 26_565
Zr1 Zr2 3.4895(9) 3_655
Zr1 Zr2 3.4895(9) 20_656
Zr2 O3 2.0760(15) .
Zr2 O3 2.0761(15) 26_565
Zr2 O5 2.182(3) 16_554
Zr2 O5 2.182(3) .
Zr2 O4 2.2370(17) .
Zr2 O4 2.2370(17) 20_656
Zr2 O1 2.283(3) .
Zr2 O1 2.284(3) 16_554
Zr2 Zr1 3.4895(9) 26_565
Zr2 Zr2 3.5323(12) 20_656
Zr2 Zr2 3.5323(12) 26_565
O1 C1 1.256(5) .
O2 C1 1.246(5) .
O3 Zr2 2.0760(15) 20_656
O4 Zr2 2.2370(17) 26_565
N1 C11 1.371(5) .
N1 C11 1.371(5) 21
N2 C9 1.376(5) .
N2 C9 1.376(5) 5_565
C1 C2 1.475(5) .
C2 C7 1.375(5) .
C2 C3 1.386(5) .
C3 C4 1.388(4) .
C4 C5 1.388(5) .
C5 C6 1.389(5) .
C5 C8 1.467(5) .
C6 C7 1.397(5) .
C8 C11 1.395(6) .
C8 C9 1.418(5) .
C9 C10 1.398(5) .
C10 C10 1.344(8) 5_565
C11 C12 1.430(5) .
C12 C12 1.316(9) 21
