#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:08:35 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179013 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/11/4121119.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_4121119
loop_
_publ_author_name
'Dawei Feng'
'Wan-Chun Chung'
'Zhangwen Wei'
'Zhi-Yuan Gu'
'Hai-Long Jiang'
'Ying-Pin Chen'
'Donald J. Darensbourg'
'Hong-Cai Zhou'
_publ_section_title
;
 Construction of Ultrastable Porphyrin Zr Metal-Organic Frameworks through
 Linker Elimination
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17105
_journal_page_last               17110
_journal_paper_doi               10.1021/ja408084j
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C144 H72 N12 O64 Zr15'
_chemical_formula_sum            'C144 H72 N12 O64 Zr15'
_chemical_formula_weight         4362.44
_chemical_name_common            PCN224No
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           229
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 4 2 3'
_symmetry_space_group_name_H-M   'I m -3 m'
_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            4
_cell_length_a                   38.465(18)
_cell_length_b                   38.465(18)
_cell_length_c                   38.465(18)
_cell_measurement_reflns_used    7996
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      15.15
_cell_measurement_theta_min      2.25
_cell_volume                     56911(5)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1968
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            226679
_diffrn_reflns_theta_full        24.70
_diffrn_reflns_theta_max         24.70
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    0.509
_exptl_crystal_description       Cuibc
_exptl_crystal_F_000             8528
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.373
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.542
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         4510
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.662
_refine_ls_R_factor_all          0.2231
_refine_ls_R_factor_gt           0.1729
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4091
_refine_ls_wR_factor_ref         0.4400
_reflns_number_gt                3257
_reflns_number_total             4510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408084j_si_004.cif
_cod_data_source_block           e:\xray\pcn224~1\dwpcn2~1\workse~1\3
_cod_original_cell_volume        56911(46)
_cod_database_code               4121119
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, y+1/2, z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'x+1/2, -y+1/2, z+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-z+1/2, x+1/2, y+1/2'
'y+1/2, -z+1/2, x+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, z+1/2, x+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, y+1/2, x+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_group
Zr1 Zr 0.27174(5) 0.20715(5) 0.20715(5) 0.1136(12) Uani 1 2 d SD .
Zr2 Zr 0.5000 0.0000 0.2500 0.1291(17) Uani 1 8 d S .
O1 O 0.3152(2) 0.1715(2) 0.2206(3) 0.123(4) Uani 1 1 d U .
O3 O 0.21653(15) 0.21653(15) 0.21653(15) 0.022(2) Uani 1 6 d SU .
O4 O 0.2473(3) 0.2019(4) 0.1514(2) 0.169(5) Uani 1 1 d . .
C1 C 0.3329(4) 0.1671(4) 0.2500 0.135(6) Uani 1 2 d SU .
C2 C 0.35964(16) 0.14036(16) 0.2500 0.126(6) Uani 1 2 d SDU .
C3 C 0.3667(3) 0.1216(3) 0.21978(14) 0.132(5) Uani 1 1 d DU .
H3 H 0.3541 0.1265 0.1991 0.158 Uiso 1 1 calc R .
C4 C 0.3920(3) 0.0959(3) 0.21992(15) 0.143(6) Uani 1 1 d DU .
H4 H 0.3964 0.0829 0.1994 0.171 Uiso 1 1 calc R .
C5 C 0.41090(15) 0.08910(15) 0.2500 0.142(8) Uani 1 2 d SDU .
C6 C 0.43610(17) 0.06390(17) 0.2500 0.068(4) Uani 1 2 d SDU .
N1 N 0.5000 0.0499(6) 0.2426(7) 0.1291(17) Uani 0.575(18) 2 d SPDU 1
C7 C 0.4721(4) 0.0726(3) 0.2384(4) 0.061(4) Uani 0.575(18) 1 d PDU 1
C8 C 0.48132(13) 0.1062(3) 0.2323(5) 0.061(5) Uani 0.575(18) 1 d PDU 1
H8 H 0.4663 0.1255 0.2287 0.073 Uiso 0.575(18) 1 calc PR 1
N2 N 0.5000 0.0498(7) 0.2569(9) 0.1291(17) Uani 0.425(18) 2 d SPDU 2
C9 C 0.4739(6) 0.0746(4) 0.2596(6) 0.063(5) Uani 0.425(18) 1 d PDU 2
C10 C 0.48130(14) 0.1090(4) 0.2634(7) 0.068(6) Uani 0.425(18) 1 d PDU 2
H10 H 0.4658 0.1281 0.2654 0.082 Uiso 0.425(18) 1 calc PR 2
O2 O 0.2621(3) 0.2011(8) 0.2621(3) 0.288(19) Uani 1 2 d SD .
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
O2 Zr1 O2 64.4(11) 84 .
O2 Zr1 O2 64.4(11) 84 11
O2 Zr1 O2 100.4(15) . 11
O2 Zr1 O3 108.4(7) 84 .
O2 Zr1 O3 71.8(4) . .
O2 Zr1 O3 71.8(4) 11 .
O2 Zr1 O1 80.4(6) 84 .
O2 Zr1 O1 80.6(5) . .
O2 Zr1 O1 139.3(6) 11 .
O3 Zr1 O1 142.6(2) . .
O2 Zr1 O1 80.4(6) 84 70
O2 Zr1 O1 139.3(6) . 70
O2 Zr1 O1 80.6(5) 11 70
O3 Zr1 O1 142.6(2) . 70
O1 Zr1 O1 73.8(5) . 70
O2 Zr1 O4 144.1(3) 84 .
O2 Zr1 O4 144.6(6) . .
O2 Zr1 O4 85.2(9) 11 .
O3 Zr1 O4 77.0(3) . .
O1 Zr1 O4 117.5(4) . .
O1 Zr1 O4 76.0(4) 70 .
O2 Zr1 O4 144.1(3) 84 70
O2 Zr1 O4 85.2(9) . 70
O2 Zr1 O4 144.6(6) 11 70
O3 Zr1 O4 77.0(3) . 70
O1 Zr1 O4 76.0(4) . 70
O1 Zr1 O4 117.5(4) 70 70
O4 Zr1 O4 71.6(7) . 70
O2 Zr1 Zr1 34.0(3) 84 84
O2 Zr1 Zr1 85.0(9) . 84
O2 Zr1 Zr1 30.7(8) 11 84
O3 Zr1 Zr1 91.8(2) . 84
O1 Zr1 Zr1 110.7(3) . 84
O1 Zr1 Zr1 75.4(3) 70 84
O4 Zr1 Zr1 112.7(3) . 84
O4 Zr1 Zr1 167.0(3) 70 84
O2 Zr1 Zr1 34.0(3) 84 83
O2 Zr1 Zr1 30.7(8) . 83
O2 Zr1 Zr1 85.0(9) 11 83
O3 Zr1 Zr1 91.8(2) . 83
O1 Zr1 Zr1 75.4(3) . 83
O1 Zr1 Zr1 110.7(3) 70 83
O4 Zr1 Zr1 167.0(3) . 83
O4 Zr1 Zr1 112.7(3) 70 83
Zr1 Zr1 Zr1 60.44(10) 84 83
O2 Zr1 Zr1 87.1(5) 84 11
O2 Zr1 Zr1 87.3(5) . 11
O2 Zr1 Zr1 35.5(4) 11 11
O3 Zr1 Zr1 36.45(14) . 11
O1 Zr1 Zr1 165.4(3) . 11
O1 Zr1 Zr1 111.6(2) 70 11
O4 Zr1 Zr1 77.1(3) . 11
O4 Zr1 Zr1 111.2(2) 70 11
Zr1 Zr1 Zr1 59.78(5) 84 11
Zr1 Zr1 Zr1 90.0 83 11
O2 Zr1 Zr1 87.1(5) 84 12
O2 Zr1 Zr1 35.5(4) . 12
O2 Zr1 Zr1 87.3(5) 11 12
O3 Zr1 Zr1 36.45(14) . 12
O1 Zr1 Zr1 111.6(2) . 12
O1 Zr1 Zr1 165.4(3) 70 12
O4 Zr1 Zr1 111.2(2) . 12
O4 Zr1 Zr1 77.1(3) 70 12
Zr1 Zr1 Zr1 90.0 84 12
Zr1 Zr1 Zr1 59.78(5) 83 12
Zr1 Zr1 Zr1 60.0 11 12
N2 Zr2 N2 91.1(3) 76_545 3_655
N2 Zr2 N2 164(2) 76_545 74
N2 Zr2 N2 91.1(3) 3_655 74
N2 Zr2 N2 91.1(3) 76_545 .
N2 Zr2 N2 164(2) 3_655 .
N2 Zr2 N2 91.1(3) 74 .
N2 Zr2 N1 88.85(17) 76_545 3_655
N2 Zr2 N1 16.3(12) 3_655 3_655
N2 Zr2 N1 88.85(17) 74 3_655
N2 Zr2 N1 179.4(14) . 3_655
N2 Zr2 N1 179.4(14) 76_545 74
N2 Zr2 N1 88.85(17) 3_655 74
N2 Zr2 N1 16.3(12) 74 74
N2 Zr2 N1 88.85(17) . 74
N1 Zr2 N1 91.2(2) 3_655 74
N2 Zr2 N1 16.3(12) 76_545 76_545
N2 Zr2 N1 88.85(17) 3_655 76_545
N2 Zr2 N1 179.4(14) 74 76_545
N2 Zr2 N1 88.85(17) . 76_545
N1 Zr2 N1 91.2(2) 3_655 76_545
N1 Zr2 N1 163.1(15) 74 76_545
N2 Zr2 N1 88.85(17) 76_545 .
N2 Zr2 N1 179.4(14) 3_655 .
N2 Zr2 N1 88.85(17) 74 .
N2 Zr2 N1 16.3(12) . .
N1 Zr2 N1 163.1(15) 3_655 .
N1 Zr2 N1 91.2(2) 74 .
N1 Zr2 N1 91.2(2) 76_545 .
C1 O1 Zr1 131.5(11) . .
Zr1 O3 Zr1 107.1(3) . 12
Zr1 O3 Zr1 107.1(3) . 11
Zr1 O3 Zr1 107.1(3) 12 11
O1 C1 O1 126.1(18) 44 .
O1 C1 C2 116.9(9) 44 .
O1 C1 C2 116.9(9) . .
C3 C2 C3 119.7(5) 44 .
C3 C2 C1 120.1(3) 44 .
C3 C2 C1 120.1(3) . .
C4 C3 C2 120.1(4) . .
C3 C4 C5 120.2(4) . .
C6 C5 C4 120.1(3) . 44
C6 C5 C4 120.1(3) . .
C4 C5 C4 119.7(5) 44 .
C5 C6 C7 119.9(5) . 44
C5 C6 C7 119.9(5) . .
C7 C6 C7 120.2(11) 44 .
C5 C6 C9 118.3(7) . .
C7 C6 C9 112.6(8) 44 .
C7 C6 C9 31.2(8) . .
C5 C6 C9 118.3(7) . 44
C7 C6 C9 31.2(8) 44 44
C7 C6 C9 112.6(8) . 44
C9 C6 C9 123.5(14) . 44
C7 N1 C7 100.8(19) 54_655 .
C7 N1 Zr2 129.6(10) 54_655 .
C7 N1 Zr2 129.6(10) . .
C8 C7 N1 114.6(15) . .
C8 C7 C6 120.3(9) . .
N1 C7 C6 122.7(10) . .
C7 C8 C8 105.0(7) . 54_655
C9 N2 C9 93(3) 54_655 .
C9 N2 Zr2 133.6(13) 54_655 .
C9 N2 Zr2 133.6(13) . .
C10 C9 N2 122(2) . .
C10 C9 C6 118.6(13) . .
N2 C9 C6 118.5(13) . .
C9 C10 C10 102.1(9) . 54_655
Zr1 O2 Zr1 115.3(10) 83 12
Zr1 O2 Zr1 115.3(10) 83 .
Zr1 O2 Zr1 109.1(7) 12 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O2 1.97(3) 84
Zr1 O2 2.157(10) .
Zr1 O2 2.157(10) 11
Zr1 O3 2.184(4) .
Zr1 O1 2.224(8) .
Zr1 O1 2.224(8) 70
Zr1 O4 2.352(12) .
Zr1 O4 2.352(12) 70
Zr1 Zr1 3.491(5) 84
Zr1 Zr1 3.491(5) 83
Zr1 Zr1 3.514(3) 11
Zr1 Zr1 3.514(3) 12
Zr2 N2 1.93(3) 76_545
Zr2 N2 1.93(3) 3_655
Zr2 N2 1.93(3) 74
Zr2 N2 1.94(3) .
Zr2 N1 1.94(2) 3_655
Zr2 N1 1.94(2) 74
Zr2 N1 1.94(2) 76_545
Zr2 N1 1.94(2) .
O1 C1 1.331(11) .
O3 Zr1 2.184(4) 12
O3 Zr1 2.184(4) 11
C1 O1 1.331(11) 44
C1 C2 1.45(2) .
C2 C3 1.393(5) 44
C2 C3 1.393(5) .
C3 C4 1.390(6) .
C4 C5 1.391(5) .
C5 C6 1.371(9) .
C5 C4 1.391(5) 44
C6 C7 1.494(16) 44
C6 C7 1.494(16) .
C6 C9 1.55(2) .
C6 C9 1.55(2) 44
N1 C7 1.391(10) 54_655
N1 C7 1.391(10) .
C7 C8 1.362(10) .
C8 C8 1.437(10) 54_655
N2 C9 1.389(10) 54_655
N2 C9 1.389(10) .
C9 C10 1.361(10) .
C10 C10 1.439(11) 54_655
O2 Zr1 1.97(3) 83
O2 Zr1 2.157(10) 12
