#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:08:35 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179013 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/11/4121118.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_4121118
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 Ni3 O64 Zr12'
_chemical_formula_sum            'C144 H72 N12 Ni3 O64 Zr12'
_chemical_formula_weight         4264.91
_chemical_name_common            PCN224Ni
_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                   38.512(2)
_cell_length_b                   38.512(2)
_cell_length_c                   38.512(2)
_cell_measurement_reflns_used    6970
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      19.43
_cell_measurement_theta_min      2.24
_cell_volume                     57120(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0786
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            73944
_diffrn_reflns_theta_full        25.66
_diffrn_reflns_theta_max         25.66
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    0.496
_exptl_crystal_density_meas      ?
_exptl_crystal_description       cubic
_exptl_crystal_F_000             8384
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         5052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0631
_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)+(0.1162P)²+1.2617P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2007
_reflns_number_gt                3514
_reflns_number_total             5052
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408084j_si_003.cif
_cod_data_source_block           e:\xray\pcn224~1\pcn224~2\work\1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measued' 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_database_code               4121118
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
Zr1 Zr 0.207106(15) 0.271576(17) 0.207106(15) 0.1069(4) Uani 1 2 d S
Ni1 Ni 0.2500 0.5000 0.0000 0.0855(6) Uani 1 8 d S
O1 O 0.22221(9) 0.31474(8) 0.17248(8) 0.1106(12) Uani 1 1 d .
O2 O 0.15344(11) 0.24905(13) 0.20099(16) 0.196(2) Uani 1 1 d .
O3 O 0.1963(2) 0.25898(10) 0.25898(10) 0.198(4) Uani 1 2 d S
O4 O 0.21794(9) 0.21794(9) 0.21794(9) 0.0558(14) Uani 1 6 d S
N1 N 0.24990(15) 0.5000 0.05058(9) 0.0907(17) Uani 1 2 d S
C1 C 0.2500 0.33167(10) 0.16833(10) 0.109(3) Uani 1 2 d S
C2 C 0.2500 0.35900(8) 0.14100(8) 0.092(2) Uani 1 2 d S
C3 C 0.22018(16) 0.36654(11) 0.12348(12) 0.1224(18) Uani 1 1 d .
H3 H 0.1993 0.3545 0.1288 0.147 Uiso 1 1 calc R
C4 C 0.22048(17) 0.39212(12) 0.09757(12) 0.132(2) Uani 1 1 d .
H4 H 0.1998 0.3970 0.0851 0.158 Uiso 1 1 calc R
C5 C 0.2500 0.41003(9) 0.08997(9) 0.100(2) Uani 1 2 d S
C6 C 0.2500 0.43734(7) 0.06266(7) 0.099(2) Uani 1 2 d S
C7 C 0.24853(15) 0.47163(8) 0.07218(8) 0.1070(18) Uani 1 1 d .
C8 C 0.24654(18) 0.48294(9) 0.10787(8) 0.148(3) Uani 1 1 d .
H8 H 0.2454 0.4684 0.1277 0.178 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'
Ni Ni 0.3393 1.1124 '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 108.8(4) . 12
O3 Zr1 O4 68.34(12) . .
O3 Zr1 O4 68.34(12) 12 .
O3 Zr1 O1 143.24(19) . .
O3 Zr1 O1 78.69(13) 12 .
O4 Zr1 O1 142.15(7) . .
O3 Zr1 O1 78.69(13) . 72
O3 Zr1 O1 143.24(19) 12 72
O4 Zr1 O1 142.15(7) . 72
O1 Zr1 O1 75.62(13) . 72
O3 Zr1 O3 71.6(3) . 83
O3 Zr1 O3 71.6(3) 12 83
O4 Zr1 O3 107.8(2) . 83
O1 Zr1 O3 77.38(16) . 83
O1 Zr1 O3 77.39(17) 72 83
O3 Zr1 O2 80.2(3) . .
O3 Zr1 O2 139.8(2) 12 .
O4 Zr1 O2 80.11(16) . .
O1 Zr1 O2 117.91(16) . .
O1 Zr1 O2 76.33(15) 72 .
O3 Zr1 O2 144.53(15) 83 .
O3 Zr1 O2 139.8(2) . 72
O3 Zr1 O2 80.2(3) 12 72
O4 Zr1 O2 80.11(16) . 72
O1 Zr1 O2 76.33(15) . 72
O1 Zr1 O2 117.91(16) 72 72
O3 Zr1 O2 144.53(15) 83 72
O2 Zr1 O2 70.1(3) . 72
O3 Zr1 Zr1 91.0(3) . 83
O3 Zr1 Zr1 37.0(2) 12 83
O4 Zr1 Zr1 89.80(13) . 83
O1 Zr1 Zr1 73.54(10) . 83
O1 Zr1 Zr1 109.35(11) 72 83
O3 Zr1 Zr1 34.65(7) 83 83
O2 Zr1 Zr1 168.48(13) . 83
O2 Zr1 Zr1 113.82(15) 72 83
O3 Zr1 Zr1 37.1(2) . 84
O3 Zr1 Zr1 91.0(3) 12 84
O4 Zr1 Zr1 89.80(13) . 84
O1 Zr1 Zr1 109.35(11) . 84
O1 Zr1 Zr1 73.54(10) 72 84
O3 Zr1 Zr1 34.65(7) 83 84
O2 Zr1 Zr1 113.82(15) . 84
O2 Zr1 Zr1 168.48(13) 72 84
Zr1 Zr1 Zr1 60.17(3) 83 84
O3 Zr1 Zr1 88.63(13) . 12
O3 Zr1 Zr1 33.16(9) 12 12
O4 Zr1 Zr1 35.18(8) . 12
O1 Zr1 Zr1 110.24(7) . 12
O1 Zr1 Zr1 163.53(10) 72 12
O3 Zr1 Zr1 88.72(13) 83 12
O2 Zr1 Zr1 112.09(11) . 12
O2 Zr1 Zr1 78.56(13) 72 12
Zr1 Zr1 Zr1 59.916(16) 83 12
Zr1 Zr1 Zr1 90.0 84 12
O3 Zr1 Zr1 33.16(9) . 11
O3 Zr1 Zr1 88.64(13) 12 11
O4 Zr1 Zr1 35.18(8) . 11
O1 Zr1 Zr1 163.53(10) . 11
O1 Zr1 Zr1 110.24(7) 72 11
O3 Zr1 Zr1 88.72(13) 83 11
O2 Zr1 Zr1 78.56(13) . 11
O2 Zr1 Zr1 112.09(11) 72 11
Zr1 Zr1 Zr1 90.0 83 11
Zr1 Zr1 Zr1 59.916(16) 84 11
Zr1 Zr1 Zr1 60.0 12 11
N1 Ni1 N1 179.8(3) 79_554 77
N1 Ni1 N1 90.000(1) 79_554 51
N1 Ni1 N1 90.000(1) 77 51
N1 Ni1 N1 90.000(1) 79_554 .
N1 Ni1 N1 90.000(1) 77 .
N1 Ni1 N1 179.8(3) 51 .
C1 O1 Zr1 133.5(3) . .
Zr1 O3 Zr1 113.68(17) . 11
Zr1 O3 Zr1 108.3(3) . 84
Zr1 O3 Zr1 108.3(3) 11 84
Zr1 O4 Zr1 109.63(15) 12 11
Zr1 O4 Zr1 109.63(15) 12 .
Zr1 O4 Zr1 109.63(15) 11 .
C7 N1 C7 105.3(3) 57_565 .
C7 N1 Ni1 127.27(17) 57_565 .
C7 N1 Ni1 127.26(17) . .
O1 C1 O1 126.0(5) 46 .
O1 C1 C2 117.0(3) 46 .
O1 C1 C2 117.0(3) . .
C3 C2 C3 119.9(5) 46 .
C3 C2 C1 120.0(3) 46 .
C3 C2 C1 120.0(3) . .
C2 C3 C4 119.6(5) . .
C5 C4 C3 121.1(6) . .
C4 C5 C4 118.6(5) 46 .
C4 C5 C6 120.7(3) 46 .
C4 C5 C6 120.7(3) . .
C7 C6 C7 121.1(4) . 46
C7 C6 C5 119.45(19) . .
C7 C6 C5 119.45(19) 46 .
C6 C7 N1 127.0(3) . .
C6 C7 C8 123.2(3) . .
N1 C7 C8 109.8(3) . .
C8 C8 C7 107.55(18) 57_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O3 2.097(2) .
Zr1 O3 2.097(2) 12
Zr1 O4 2.148(2) .
Zr1 O1 2.209(3) .
Zr1 O1 2.209(3) 72
Zr1 O3 2.222(9) 83
Zr1 O2 2.254(5) .
Zr1 O2 2.254(5) 72
Zr1 Zr1 3.5021(16) 83
Zr1 Zr1 3.5021(16) 84
Zr1 Zr1 3.5113(7) 12
Zr1 Zr1 3.5113(7) 11
Ni1 N1 1.948(3) 79_554
Ni1 N1 1.948(3) 77
Ni1 N1 1.948(3) 51
Ni1 N1 1.948(3) .
O1 C1 1.263(4) .
O3 Zr1 2.097(2) 11
O3 Zr1 2.223(9) 84
O4 Zr1 2.148(2) 12
O4 Zr1 2.148(2) 11
N1 C7 1.374(3) 57_565
N1 C7 1.374(3) .
C1 O1 1.263(4) 46
C1 C2 1.489(7) .
C2 C3 1.363(6) 46
C2 C3 1.363(6) .
C3 C4 1.402(5) .
C4 C5 1.362(6) .
C5 C4 1.362(6) 46
C5 C6 1.488(6) .
C6 C7 1.372(4) .
C6 C7 1.372(4) 46
C7 C8 1.444(4) .
C8 C8 1.314(7) 57_565
