#------------------------------------------------------------------------------
#$Date: 2019-11-26 03:05:32 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242466 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/24/4132493.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_4132493
loop_
_publ_author_name
'Zhang, Xin'
'Frey, Brandon L.'
'Chen, Yu-Sheng'
'Zhang, Jian'
_publ_section_title
;
 Topology-Guided Stepwise Insertion of Three Secondary Linkers in
 Zirconium Metal-Organic Frameworks.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7710
_journal_page_last               7715
_journal_paper_doi               10.1021/jacs.8b04277
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C44 H22 O16 Zr3'
_chemical_formula_weight         1080.28
_space_group_IT_number           65
_space_group_name_Hall           '-C 2 2'
_space_group_name_H-M_alt        'C m m m'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C m m 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                   20.2175(9)
_cell_length_b                   34.4927(15)
_cell_length_c                   21.0753(9)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      32.961
_cell_measurement_theta_min      4.447
_cell_volume                     14697.0(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.51500
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57492
_diffrn_reflns_theta_full        17.01
_diffrn_reflns_theta_max         17.01
_diffrn_reflns_theta_min         0.85
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    0.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.00059(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         5699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0900P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1568
_reflns_number_gt                3277
_reflns_number_total             5699
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b04277_si_003.cif
_cod_data_source_block           NPF-300-LT
_cod_original_sg_symbol_H-M      cmmm
_cod_database_code               4132493
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
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 0.0000 0.429315(15) 0.5000 0.0744(3) Uani 1 4 d S
Zr2 Zr 0.08716(3) 0.5000 0.41604(2) 0.0780(3) Uani 1 2 d S
O1 O 0.0000 0.46452(11) 0.4156(2) 0.1126(17) Uani 1 2 d S
O2 O 0.0877(3) 0.46576(13) 0.5000 0.1183(18) Uani 1 2 d S
O3 O 0.12194(19) 0.44115(7) 0.38169(15) 0.1071(11) Uani 1 1 d .
O4 O 0.06644(16) 0.39666(6) 0.43757(14) 0.0830(9) Uani 1 1 d .
O5 O 0.1961(3) 0.5000 0.4210(2) 0.1153(16) Uani 1 2 d S
O6 O 0.0784(2) 0.5000 0.31291(19) 0.1049(15) Uani 1 2 d S
C1 C 0.1056(3) 0.40639(11) 0.3947(2) 0.0879(15) Uani 1 1 d .
C2 C 0.1376(3) 0.37515(10) 0.3585(2) 0.0889(14) Uani 1 1 d .
C3 C 0.1286(3) 0.33722(11) 0.3775(2) 0.1109(18) Uani 1 1 d .
H3A H 0.1021 0.3316 0.4124 0.133 Uiso 1 1 calc R
C4 C 0.1591(3) 0.30760(12) 0.3444(2) 0.125(2) Uani 1 1 d .
H4A H 0.1559 0.2823 0.3594 0.150 Uiso 1 1 calc R
C5 C 0.1942(3) 0.31479(11) 0.2897(2) 0.1062(17) Uani 1 1 d .
C6 C 0.2034(3) 0.35262(11) 0.2716(2) 0.115(2) Uani 1 1 d .
H6B H 0.2293 0.3582 0.2363 0.137 Uiso 1 1 calc R
C7 C 0.1748(3) 0.38211(11) 0.3050(2) 0.1092(17) Uani 1 1 d .
H7A H 0.1806 0.4075 0.2913 0.131 Uiso 1 1 calc R
C8 C 0.2247(3) 0.28149(13) 0.2540(2) 0.1222(19) Uani 1 1 d .
C9 C 0.2500 0.2500 0.2861(3) 0.112(3) Uani 1 2 d S
H9A H 0.2500 0.2500 0.3302 0.134 Uiso 1 2 calc SR
C10 C 0.2227(3) 0.28160(13) 0.1880(2) 0.138(2) Uani 1 1 d .
H10A H 0.2037 0.3021 0.1660 0.165 Uiso 1 1 calc R
C11 C 0.2500 0.2500 0.1558(3) 0.147(4) Uani 1 2 d S
C13 C 0.2500 0.2500 0.0890(4) 0.177(6) Uani 1 2 d S
C14 C 0.2500 0.2500 0.0322(4) 0.167(5) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.5364 2.6141 '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
O1 Zr1 O1 111.3(3) 10_556 .
O1 Zr1 O2 70.97(9) 10_556 3_556
O1 Zr1 O2 70.97(9) . 3_556
O1 Zr1 O2 70.97(9) 10_556 .
O1 Zr1 O2 70.97(9) . .
O2 Zr1 O2 109.4(3) 3_556 .
O1 Zr1 O4 78.11(12) 10_556 10_556
O1 Zr1 O4 141.77(8) . 10_556
O2 Zr1 O4 142.86(8) 3_556 10_556
O2 Zr1 O4 78.29(13) . 10_556
O1 Zr1 O4 141.77(8) 10_556 12
O1 Zr1 O4 78.11(12) . 12
O2 Zr1 O4 78.29(13) 3_556 12
O2 Zr1 O4 142.86(8) . 12
O4 Zr1 O4 118.16(14) 10_556 12
O1 Zr1 O4 141.77(8) 10_556 .
O1 Zr1 O4 78.11(12) . .
O2 Zr1 O4 142.86(8) 3_556 .
O2 Zr1 O4 78.29(13) . .
O4 Zr1 O4 73.78(15) 10_556 .
O4 Zr1 O4 75.59(16) 12 .
O1 Zr1 O4 78.11(12) 10_556 3_556
O1 Zr1 O4 141.77(8) . 3_556
O2 Zr1 O4 78.29(13) 3_556 3_556
O2 Zr1 O4 142.86(8) . 3_556
O4 Zr1 O4 75.59(16) 10_556 3_556
O4 Zr1 O4 73.78(15) 12 3_556
O4 Zr1 O4 118.16(14) . 3_556
O1 Zr1 Zr2 35.65(7) 10_556 10_556
O1 Zr1 Zr2 91.42(11) . 10_556
O2 Zr1 Zr2 90.46(12) 3_556 10_556
O2 Zr1 Zr2 35.33(7) . 10_556
O4 Zr1 Zr2 75.24(7) 10_556 10_556
O4 Zr1 Zr2 166.60(7) 12 10_556
O4 Zr1 Zr2 110.73(8) . 10_556
O4 Zr1 Zr2 111.35(7) 3_556 10_556
O1 Zr1 Zr2 35.65(7) 10_556 9_566
O1 Zr1 Zr2 91.42(11) . 9_566
O2 Zr1 Zr2 35.33(7) 3_556 9_566
O2 Zr1 Zr2 90.46(12) . 9_566
O4 Zr1 Zr2 111.35(7) 10_556 9_566
O4 Zr1 Zr2 110.73(8) 12 9_566
O4 Zr1 Zr2 166.60(7) . 9_566
O4 Zr1 Zr2 75.24(7) 3_556 9_566
Zr2 Zr1 Zr2 60.65(2) 10_556 9_566
O1 Zr1 Zr2 91.42(11) 10_556 .
O1 Zr1 Zr2 35.65(6) . .
O2 Zr1 Zr2 90.46(12) 3_556 .
O2 Zr1 Zr2 35.33(7) . .
O4 Zr1 Zr2 110.73(8) 10_556 .
O4 Zr1 Zr2 111.35(7) 12 .
O4 Zr1 Zr2 75.24(7) . .
O4 Zr1 Zr2 166.60(7) 3_556 .
Zr2 Zr1 Zr2 60.929(16) 10_556 .
Zr2 Zr1 Zr2 91.375(17) 9_566 .
O1 Zr1 Zr2 91.42(11) 10_556 2_565
O1 Zr1 Zr2 35.65(7) . 2_565
O2 Zr1 Zr2 35.33(7) 3_556 2_565
O2 Zr1 Zr2 90.46(12) . 2_565
O4 Zr1 Zr2 166.60(7) 10_556 2_565
O4 Zr1 Zr2 75.24(7) 12 2_565
O4 Zr1 Zr2 111.35(7) . 2_565
O4 Zr1 Zr2 110.73(8) 3_556 2_565
Zr2 Zr1 Zr2 91.375(17) 10_556 2_565
Zr2 Zr1 Zr2 60.929(16) 9_566 2_565
Zr2 Zr1 Zr2 60.65(2) . 2_565
O2 Zr2 O2 67.4(2) 11_565 .
O2 Zr2 O1 108.9(2) 11_565 .
O2 Zr2 O1 72.01(17) . .
O2 Zr2 O1 72.01(17) 11_565 2_565
O2 Zr2 O1 108.9(2) . 2_565
O1 Zr2 O1 69.56(17) . 2_565
O2 Zr2 O6 146.05(10) 11_565 .
O2 Zr2 O6 146.05(10) . .
O1 Zr2 O6 85.97(17) . .
O1 Zr2 O6 85.97(17) 2_565 .
O2 Zr2 O5 87.42(18) 11_565 .
O2 Zr2 O5 87.42(18) . .
O1 Zr2 O5 145.14(9) . .
O1 Zr2 O5 145.14(9) 2_565 .
O6 Zr2 O5 97.35(18) . .
O2 Zr2 O3 76.51(13) 11_565 11_565
O2 Zr2 O3 139.55(14) . 11_565
O1 Zr2 O3 139.84(14) . 11_565
O1 Zr2 O3 75.08(13) 2_565 11_565
O6 Zr2 O3 72.95(10) . 11_565
O5 Zr2 O3 72.87(11) . 11_565
O2 Zr2 O3 139.55(14) 11_565 .
O2 Zr2 O3 76.51(13) . .
O1 Zr2 O3 75.08(13) . .
O1 Zr2 O3 139.84(14) 2_565 .
O6 Zr2 O3 72.95(10) . .
O5 Zr2 O3 72.87(11) . .
O3 Zr2 O3 127.14(15) 11_565 .
O2 Zr2 Zr1 88.22(13) 11_565 .
O2 Zr2 Zr1 36.23(12) . .
O1 Zr2 Zr1 35.79(11) . .
O1 Zr2 Zr1 89.19(11) 2_565 .
O6 Zr2 Zr1 117.68(8) . .
O5 Zr2 Zr1 118.70(7) . .
O3 Zr2 Zr1 160.74(8) 11_565 .
O3 Zr2 Zr1 72.12(8) . .
O2 Zr2 Zr1 36.23(12) 11_565 9_566
O2 Zr2 Zr1 88.22(13) . 9_566
O1 Zr2 Zr1 89.19(11) . 9_566
O1 Zr2 Zr1 35.79(11) 2_565 9_566
O6 Zr2 Zr1 117.68(8) . 9_566
O5 Zr2 Zr1 118.70(7) . 9_566
O3 Zr2 Zr1 72.12(8) 11_565 9_566
O3 Zr2 Zr1 160.74(8) . 9_566
Zr1 Zr2 Zr1 88.625(17) . 9_566
O2 Zr2 Zr2 90.32(15) 11_565 2_565
O2 Zr2 Zr2 90.32(15) . 2_565
O1 Zr2 Zr2 34.78(9) . 2_565
O1 Zr2 Zr2 34.78(9) 2_565 2_565
O6 Zr2 Zr2 85.37(13) . 2_565
O5 Zr2 Zr2 177.28(11) . 2_565
O3 Zr2 Zr2 108.07(10) 11_565 2_565
O3 Zr2 Zr2 108.07(10) . 2_565
Zr1 Zr2 Zr2 59.674(10) . 2_565
Zr1 Zr2 Zr2 59.674(10) 9_566 2_565
O2 Zr2 Zr2 33.72(10) 11_565 10_556
O2 Zr2 Zr2 33.72(10) . 10_556
O1 Zr2 Zr2 90.23(13) . 10_556
O1 Zr2 Zr2 90.23(13) 2_565 10_556
O6 Zr2 Zr2 175.37(13) . 10_556
O5 Zr2 Zr2 87.28(11) . 10_556
O3 Zr2 Zr2 108.62(8) 11_565 10_556
O3 Zr2 Zr2 108.62(8) . 10_556
Zr1 Zr2 Zr2 59.535(8) . 10_556
Zr1 Zr2 Zr2 59.535(8) 9_566 10_556
Zr2 Zr2 Zr2 90.0 2_565 10_556
Zr2 O1 Zr2 110.44(18) . 2_565
Zr2 O1 Zr1 108.57(15) . .
Zr2 O1 Zr1 108.57(15) 2_565 .
Zr2 O2 Zr2 112.6(2) 10_556 .
Zr2 O2 Zr1 108.45(16) 10_556 .
Zr2 O2 Zr1 108.45(16) . .
C1 O3 Zr2 134.0(3) . .
C1 O4 Zr1 133.3(2) . .
O4 C1 O3 125.0(4) . .
O4 C1 C2 117.3(4) . .
O3 C1 C2 117.7(4) . .
C7 C2 C3 118.4(4) . .
C7 C2 C1 122.5(4) . .
C3 C2 C1 119.1(4) . .
C2 C3 C4 119.7(5) . .
C5 C4 C3 121.3(4) . .
C6 C5 C4 118.3(4) . .
C6 C5 C8 122.0(4) . .
C4 C5 C8 119.5(4) . .
C7 C6 C5 120.5(4) . .
C6 C7 C2 121.6(4) . .
C9 C8 C10 120.2(4) . .
C9 C8 C5 120.5(4) . .
C10 C8 C5 119.1(4) . .
C8 C9 C8 121.2(6) 6 .
C8 C10 C11 118.2(4) . .
C10 C11 C10 121.8(6) . 6
C10 C11 C13 119.1(3) . .
C10 C11 C13 119.1(3) 6 .
C14 C13 C11 180.000(1) . .
C13 C14 C14 180.000(1) . 13
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O1 2.153(4) 10_556
Zr1 O1 2.153(4) .
Zr1 O2 2.174(5) 3_556
Zr1 O2 2.174(5) .
Zr1 O4 2.192(3) 10_556
Zr1 O4 2.192(3) 12
Zr1 O4 2.192(3) .
Zr1 O4 2.192(3) 3_556
Zr1 Zr2 3.4901(5) 10_556
Zr1 Zr2 3.4901(5) 9_566
Zr1 Zr2 3.4901(5) .
Zr1 Zr2 3.4901(5) 2_565
Zr2 O2 2.127(2) 11_565
Zr2 O2 2.127(2) .
Zr2 O1 2.146(2) .
Zr2 O1 2.146(2) 2_565
Zr2 O6 2.181(4) .
Zr2 O5 2.204(6) .
Zr2 O3 2.267(3) 11_565
Zr2 O3 2.267(3) .
Zr2 Zr1 3.4901(5) 9_566
Zr2 Zr2 3.5244(13) 2_565
Zr2 Zr2 3.5390(9) 10_556
O1 Zr2 2.146(2) 2_565
O2 Zr2 2.127(2) 10_556
O3 C1 1.273(5) .
O4 C1 1.248(5) .
C1 C2 1.470(5) .
C2 C7 1.375(6) .
C2 C3 1.380(5) .
C3 C4 1.383(6) .
C4 C5 1.374(6) .
C5 C6 1.373(5) .
C5 C8 1.506(6) .
C6 C7 1.366(5) .
C8 C9 1.378(5) .
C8 C10 1.391(6) .
C9 C8 1.378(5) 6
C10 C11 1.398(5) .
C11 C10 1.398(5) 6
C11 C13 1.407(11) .
C13 C14 1.197(10) .
C14 C14 1.357(18) 13
