#------------------------------------------------------------------------------
#$Date: 2019-11-26 05:47:04 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242751 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/28/4132863.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_4132863
loop_
_publ_author_name
'Guillerm, Vincent'
'Grancha, Thais'
'Imaz, Inhar'
'Juanhuix, Judith'
'Maspoch, Daniel'
_publ_section_title
;
 Zigzag Ligands for Transversal Design in Reticular Chemistry: Unveiling
 New Structural Opportunities for Metal-Organic Frameworks.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10153
_journal_page_last               10157
_journal_paper_doi               10.1021/jacs.8b07050
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C24 H8 O16 Zr3'
_chemical_formula_sum            'C24 H8 O16 Zr3'
_chemical_formula_weight         825.96
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   17.540(5)
_cell_length_b                   17.540(5)
_cell_length_c                   22.850(5)
_cell_measurement_reflns_used    1342
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40
_cell_measurement_theta_min      1
_cell_volume                     7030(3)
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measurement_device_type  'PILATUS DECTRIS'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71656
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8977
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.449
_diffrn_reflns_theta_min         1.464
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    0.780
_exptl_crystal_description       prisme
_exptl_crystal_F_000             4140
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.036
_refine_diff_density_min         -2.443
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         2109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1592P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2255
_refine_ls_wR_factor_ref         0.2555
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1479
_reflns_number_total             2109
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b07050_si_003.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        7030(4)
_cod_database_code               4132863
_shelx_shelxl_version_number     2018/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'-y, -x, -z'
'y, x, -z'
'y, -x, z'
'-y, x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'y, x, z'
'-y, -x, z'
'-y, x, -z'
'y, -x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Zr01 Zr 0.500000 0.500000 0.60771(5) 0.0348(4) Uani 1 8 d S T P
Zr02 Zr 0.39909(4) 0.39909(4) 0.500000 0.0421(4) Uani 1 4 d S T P
O003 O 0.5762(2) 0.5762(2) 0.6563(2) 0.0512(12) Uani 1 2 d S T P
O004 O 0.3587(2) 0.3587(2) 0.4119(2) 0.0723(18) Uani 1 2 d S T P
O005 O 0.4054(5) 0.2732(4) 0.500000 0.084(2) Uani 1 2 d S T P
O9 O 0.500000 0.3978(5) 0.5526(3) 0.091(3) Uani 1 2 d S T P
C007 C 0.6663(4) 0.6663(4) 0.6872(4) 0.081(3) Uani 1 2 d S T P
C009 C 0.7425(4) 0.7425(4) 0.7788(4) 0.096(4) Uani 1 2 d S T P
C010 C 0.6250(3) 0.6250(3) 0.6397(4) 0.060(2) Uani 1 2 d S T P
C011 C 0.6493(5) 0.6493(5) 0.7462(6) 0.192(11) Uani 1 2 d S T P
H011 H 0.612745 0.612745 0.755109 0.230 Uiso 1 2 calc R U P
C012 C 0.6855(5) 0.6855(5) 0.7888(5) 0.234(14) Uani 1 2 d S T P
H012 H 0.673201 0.673201 0.827287 0.281 Uiso 1 2 calc R U P
C013 C 0.7193(4) 0.7193(4) 0.6761(4) 0.104(4) Uani 1 2 d S T P
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'
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
O9 Zr01 O9 70.7(2) . 21
O9 Zr01 O9 70.7(2) . 22_665
O9 Zr01 O9 109.8(4) 21 22_665
O9 Zr01 O9 109.8(4) . 2_665
O9 Zr01 O9 70.7(2) 21 2_665
O9 Zr01 O9 70.7(2) 22_665 2_665
O9 Zr01 O003 142.18(5) . .
O9 Zr01 O003 142.18(5) 21 .
O9 Zr01 O003 78.0(2) 22_665 .
O9 Zr01 O003 78.0(2) 2_665 .
O9 Zr01 O003 78.0(2) . 2_665
O9 Zr01 O003 78.0(2) 21 2_665
O9 Zr01 O003 142.18(5) 22_665 2_665
O9 Zr01 O003 142.18(5) 2_665 2_665
O003 Zr01 O003 119.2(3) . 2_665
O9 Zr01 O003 78.0(2) . 20_565
O9 Zr01 O003 142.18(5) 21 20_565
O9 Zr01 O003 78.0(2) 22_665 20_565
O9 Zr01 O003 142.18(5) 2_665 20_565
O003 Zr01 O003 75.16(13) . 20_565
O003 Zr01 O003 75.16(13) 2_665 20_565
O9 Zr01 O003 142.18(5) . 19_655
O9 Zr01 O003 78.0(2) 21 19_655
O9 Zr01 O003 142.18(5) 22_665 19_655
O9 Zr01 O003 78.0(2) 2_665 19_655
O003 Zr01 O003 75.16(13) . 19_655
O003 Zr01 O003 75.16(13) 2_665 19_655
O003 Zr01 O003 119.2(3) 20_565 19_655
O9 Zr01 Zr02 90.55(18) . 3_566
O9 Zr01 Zr02 35.36(10) 21 3_566
O9 Zr01 Zr02 90.55(18) 22_665 3_566
O9 Zr01 Zr02 35.36(10) 2_665 3_566
O003 Zr01 Zr02 110.78(9) . 3_566
O003 Zr01 Zr02 110.79(9) 2_665 3_566
O003 Zr01 Zr02 165.89(14) 20_565 3_566
O003 Zr01 Zr02 74.93(14) 19_655 3_566
O9 Zr01 Zr02 35.36(10) . 19_655
O9 Zr01 Zr02 90.55(18) 21 19_655
O9 Zr01 Zr02 35.36(10) 22_665 19_655
O9 Zr01 Zr02 90.55(18) 2_665 19_655
O003 Zr01 Zr02 110.78(9) . 19_655
O003 Zr01 Zr02 110.79(9) 2_665 19_655
O003 Zr01 Zr02 74.93(14) 20_565 19_655
O003 Zr01 Zr02 165.89(14) 19_655 19_655
Zr02 Zr01 Zr02 90.96(4) 3_566 19_655
O9 Zr01 Zr02 90.55(19) . 17_666
O9 Zr01 Zr02 90.55(19) 21 17_666
O9 Zr01 Zr02 35.36(10) 22_665 17_666
O9 Zr01 Zr02 35.36(10) 2_665 17_666
O003 Zr01 Zr02 74.92(14) . 17_666
O003 Zr01 Zr02 165.89(14) 2_665 17_666
O003 Zr01 Zr02 110.79(9) 20_565 17_666
O003 Zr01 Zr02 110.79(9) 19_655 17_666
Zr02 Zr01 Zr02 60.56(2) 3_566 17_666
Zr02 Zr01 Zr02 60.56(2) 19_655 17_666
O9 Zr01 Zr02 35.36(10) . .
O9 Zr01 Zr02 35.36(10) 21 .
O9 Zr01 Zr02 90.55(19) 22_665 .
O9 Zr01 Zr02 90.55(19) 2_665 .
O003 Zr01 Zr02 165.89(14) . .
O003 Zr01 Zr02 74.92(14) 2_665 .
O003 Zr01 Zr02 110.79(9) 20_565 .
O003 Zr01 Zr02 110.79(9) 19_655 .
Zr02 Zr01 Zr02 60.56(2) 3_566 .
Zr02 Zr01 Zr02 60.56(2) 19_655 .
Zr02 Zr01 Zr02 90.97(4) 17_666 .
O9 Zr02 O9 72.6(4) . 21
O9 Zr02 O9 109.4(5) . 6_556
O9 Zr02 O9 68.4(3) 21 6_556
O9 Zr02 O9 68.4(3) . 18_556
O9 Zr02 O9 109.4(5) 21 18_556
O9 Zr02 O9 72.6(4) 6_556 18_556
O9 Zr02 O005 145.75(13) . 21
O9 Zr02 O005 87.0(3) 21 21
O9 Zr02 O005 87.0(3) 6_556 21
O9 Zr02 O005 145.75(13) 18_556 21
O9 Zr02 O005 87.0(3) . .
O9 Zr02 O005 145.75(13) 21 .
O9 Zr02 O005 145.75(13) 6_556 .
O9 Zr02 O005 87.0(3) 18_556 .
O005 Zr02 O005 95.7(4) 21 .
O9 Zr02 O004 139.49(15) . .
O9 Zr02 O004 139.49(15) 21 .
O9 Zr02 O004 75.8(2) 6_556 .
O9 Zr02 O004 75.8(2) 18_556 .
O005 Zr02 O004 72.62(12) 21 .
O005 Zr02 O004 72.62(12) . .
O9 Zr02 O004 75.8(2) . 18_556
O9 Zr02 O004 75.8(2) 21 18_556
O9 Zr02 O004 139.50(15) 6_556 18_556
O9 Zr02 O004 139.50(15) 18_556 18_556
O005 Zr02 O004 72.62(12) 21 18_556
O005 Zr02 O004 72.62(12) . 18_556
O004 Zr02 O004 127.1(3) . 18_556
O9 Zr02 Zr01 88.98(19) . 17_666
O9 Zr02 Zr01 88.98(19) 21 17_666
O9 Zr02 Zr01 36.3(2) 6_556 17_666
O9 Zr02 Zr01 36.3(2) 18_556 17_666
O005 Zr02 Zr01 118.57(12) 21 17_666
O005 Zr02 Zr01 118.57(12) . 17_666
O004 Zr02 Zr01 71.92(15) . 17_666
O004 Zr02 Zr01 160.96(15) 18_556 17_666
O9 Zr02 Zr01 36.3(2) . .
O9 Zr02 Zr01 36.3(2) 21 .
O9 Zr02 Zr01 88.98(19) 6_556 .
O9 Zr02 Zr01 88.98(19) 18_556 .
O005 Zr02 Zr01 118.57(12) 21 .
O005 Zr02 Zr01 118.57(12) . .
O004 Zr02 Zr01 160.95(15) . .
O004 Zr02 Zr01 71.92(15) 18_556 .
Zr01 Zr02 Zr01 89.03(4) 17_666 .
O9 Zr02 Zr02 90.6(2) . 3_566
O9 Zr02 Zr02 34.20(13) 21 3_566
O9 Zr02 Zr02 34.20(13) 6_556 3_566
O9 Zr02 Zr02 90.6(2) 18_556 3_566
O005 Zr02 Zr02 87.1(2) 21 3_566
O005 Zr02 Zr02 177.1(2) . 3_566
O004 Zr02 Zr02 108.35(10) . 3_566
O004 Zr02 Zr02 108.35(10) 18_556 3_566
Zr01 Zr02 Zr02 59.721(11) 17_666 3_566
Zr01 Zr02 Zr02 59.722(11) . 3_566
O9 Zr02 Zr02 34.20(13) . 19_655
O9 Zr02 Zr02 90.6(2) 21 19_655
O9 Zr02 Zr02 90.6(2) 6_556 19_655
O9 Zr02 Zr02 34.20(13) 18_556 19_655
O005 Zr02 Zr02 177.1(2) 21 19_655
O005 Zr02 Zr02 87.1(2) . 19_655
O004 Zr02 Zr02 108.35(10) . 19_655
O004 Zr02 Zr02 108.35(10) 18_556 19_655
Zr01 Zr02 Zr02 59.721(11) 17_666 19_655
Zr01 Zr02 Zr02 59.722(11) . 19_655
Zr02 Zr02 Zr02 90.0 3_566 19_655
C010 O003 Zr01 132.2(5) . .
C010 O004 Zr02 134.7(6) 17_666 .
Zr02 O9 Zr02 111.6(3) 19_655 .
Zr02 O9 Zr01 108.3(3) 19_655 .
Zr02 O9 Zr01 108.3(3) . .
C013 C007 C011 118.3(9) . .
C013 C007 C010 122.4(8) . .
C011 C007 C010 119.4(9) . .
C009 C009 C013 121.7(12) 25_666 25_666
C009 C009 C012 115.0(11) 25_666 .
C013 C009 C012 123.3(9) 25_666 .
O004 C010 O003 126.2(8) 17_666 .
O004 C010 C007 117.8(8) 17_666 .
O003 C010 C007 115.9(7) . .
C012 C011 C007 120.1(12) . .
C011 C012 C009 123.4(12) . .
C007 C013 C009 121.6(9) . 25_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr01 O9 2.190(7) .
Zr01 O9 2.190(7) 21
Zr01 O9 2.190(7) 22_665
Zr01 O9 2.190(7) 2_665
Zr01 O003 2.193(5) .
Zr01 O003 2.193(5) 2_665
Zr01 O003 2.193(5) 20_565
Zr01 O003 2.193(5) 19_655
Zr01 Zr02 3.5105(12) 3_566
Zr01 Zr02 3.5105(12) 19_655
Zr01 Zr02 3.5105(12) 17_666
Zr01 Zr02 3.5105(12) .
Zr02 O9 2.140(3) .
Zr02 O9 2.140(3) 21
Zr02 O9 2.140(3) 6_556
Zr02 O9 2.140(3) 18_556
Zr02 O005 2.211(7) 21
Zr02 O005 2.211(7) .
Zr02 O004 2.248(6) .
Zr02 O004 2.248(6) 18_556
Zr02 Zr02 3.5399(16) 3_566
Zr02 Zr02 3.5399(16) 19_655
O003 C010 1.268(10) .
O004 C010 1.246(10) 17_666
C007 C013 1.340(14) .
C007 C011 1.412(16) .
C007 C010 1.492(12) .
C009 C009 1.366(19) 25_666
C009 C013 1.401(13) 25_666
C009 C012 1.434(16) .
C011 C012 1.324(16) .
