#------------------------------------------------------------------------------
#$Date: 2017-11-11 02:30:53 +0200 (Sat, 11 Nov 2017) $
#$Revision: 203088 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/67/4126731.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_4126731
loop_
_publ_author_name
'Pang, Jiandong'
'Yuan, Shuai'
'Qin, Junsheng'
'Liu, Caiping'
'Lollar, Christina'
'Wu, Mingyan'
'Yuan, Daqiang'
'Zhou, Hong-Cai'
'Hong, Maochun'
_publ_section_title
;
 Control the Structure of Zr-Tetracarboxylate Frameworks through Steric
 Tuning.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b09973
_journal_year                    2017
_chemical_formula_sum            'C44.67 H44 O16.67 Zr3'
_chemical_formula_weight         1121.22
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_symmetry_space_group_name_Hall  '-P 6 2'
_symmetry_space_group_name_H-M   'P 6/m m m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   40.4113(11)
_cell_length_b                   40.4113(11)
_cell_length_c                   15.6898(6)
_cell_measurement_reflns_used    7751
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      48.8531
_cell_measurement_theta_min      2.8164
_cell_volume                     22189.8(12)
_computing_cell_refinement       'SAINT+ ver. (Bruker, 2001)'
_computing_data_collection       'APEX2  (Bruker, 2008)'
_computing_data_reduction        'SAINT+ ver. (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2198
_diffrn_reflns_av_unetI/netI     0.1255
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5992
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        59.135
_diffrn_reflns_theta_max         59.135
_diffrn_reflns_theta_min         2.187
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.893
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5117
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.503
_exptl_crystal_description       Block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.782
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         5992
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.784
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0369P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2735
_reflns_number_total             5992
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b09973_si_002.cif
_cod_data_source_block           MLPCN-608-2
_cod_original_cell_volume        22189.8(15)
_cod_database_code               4126731
_shelx_shelxl_version_number     2016/6
_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, x, z'
'-y, x-y, z'
'-x, -y, z'
'-x+y, -x, z'
'y, -x+y, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'-x+y, -x, -z'
'y, -x+y, -z'
'x, y, -z'
'x-y, x, -z'
'-y, x-y, -z'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Zr1 Zr 0.53533(2) 0.07067(2) 0.500000 0.0498(2) Uani 1 4 d S T P
Zr2 Zr 0.45637(2) 0.000000 0.38824(3) 0.05807(17) Uani 1 2 d S T P
O1 O 0.51780(7) 0.10203(6) 0.41371(16) 0.0643(7) Uani 1 1 d . . .
O2 O 0.46599(7) 0.05685(7) 0.34374(16) 0.0828(9) Uani 1 1 d . . .
O3 O 0.47419(8) 0.03482(8) 0.500000 0.0779(11) Uani 1 2 d S T P
O4 O 0.51742(4) 0.03483(9) 0.3872(2) 0.0971(13) Uani 1 2 d S T P
O5 O 0.40231(7) 0.000000 0.4298(2) 0.1354(18) Uani 1 2 d S T P
H5A H 0.381146 -0.019260 0.415318 0.203 Uiso 1 1 d R U .
O6 O 0.45963(10) 0.000000 0.2473(2) 0.1206(14) Uani 1 2 d S T P
H6A H 0.453917 -0.019620 0.217182 0.181 Uiso 1 1 d R U .
O7 O 0.4811(4) 0.2405(2) 0.3165(7) 0.159(6) Uani 0.3355 2 d DS T P
C1 C 0.49004(13) 0.09065(12) 0.3634(3) 0.0712(13) Uani 1 1 d . . .
C2 C 0.48704(13) 0.12155(12) 0.3166(3) 0.0732(12) Uani 1 1 d . . .
C3 C 0.45963(13) 0.11263(12) 0.2566(3) 0.1116(17) Uani 1 1 d . . .
H3 H 0.442268 0.087137 0.244807 0.134 Uiso 1 1 calc R U .
C4 C 0.45727(13) 0.14162(12) 0.2121(3) 0.1144(18) Uani 1 1 d . . .
H4 H 0.438873 0.135260 0.170013 0.137 Uiso 1 1 calc R U .
C5 C 0.48218(15) 0.17938(12) 0.2310(3) 0.0872(15) Uani 1 1 d . . .
C6 C 0.50985(14) 0.18824(12) 0.2911(3) 0.1148(18) Uani 1 1 d . . .
H6 H 0.527195 0.213690 0.303390 0.138 Uiso 1 1 calc R U .
C7 C 0.51219(12) 0.15900(12) 0.3347(3) 0.1038(16) Uani 1 1 d . . .
H7 H 0.530938 0.165210 0.375892 0.125 Uiso 1 1 calc R U .
C8 C 0.48127(19) 0.24063(9) 0.2237(4) 0.096(2) Uani 1 2 d DS T P
C9 C 0.48066(12) 0.21058(11) 0.1809(3) 0.0953(15) Uani 1 1 d . . .
C10 C 0.47894(13) 0.20940(11) 0.0922(3) 0.0944(15) Uani 1 1 d . . .
C11 C 0.47793(16) 0.23897(8) 0.0469(3) 0.092(2) Uani 1 2 d S T P
C12 C 0.4883(3) 0.1847(3) 0.0432(6) 0.083(4) Uani 0.3333 1 d . U P
H12 H 0.494434 0.168358 0.071951 0.099 Uiso 0.3333 1 calc R U P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 '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 108.63(17) . 19_655
O3 Zr1 O4 70.29(7) . .
O3 Zr1 O4 70.29(7) 19_655 .
O3 Zr1 O4 70.29(7) . 16_556
O3 Zr1 O4 70.28(7) 19_655 16_556
O4 Zr1 O4 109.4(2) . 16_556
O3 Zr1 O1 78.20(9) . .
O3 Zr1 O1 141.87(6) 19_655 .
O4 Zr1 O1 77.66(10) . .
O4 Zr1 O1 142.25(6) 16_556 .
O3 Zr1 O1 78.20(9) . 16_556
O3 Zr1 O1 141.87(6) 19_655 16_556
O4 Zr1 O1 142.24(6) . 16_556
O4 Zr1 O1 77.66(10) 16_556 16_556
O1 Zr1 O1 75.97(12) . 16_556
O3 Zr1 O1 141.87(6) . 11_656
O3 Zr1 O1 78.20(9) 19_655 11_656
O4 Zr1 O1 142.24(6) . 11_656
O4 Zr1 O1 77.66(10) 16_556 11_656
O1 Zr1 O1 120.14(13) . 11_656
O1 Zr1 O1 75.20(12) 16_556 11_656
O3 Zr1 O1 141.87(6) . 19_655
O3 Zr1 O1 78.20(9) 19_655 19_655
O4 Zr1 O1 77.66(10) . 19_655
O4 Zr1 O1 142.24(6) 16_556 19_655
O1 Zr1 O1 75.20(12) . 19_655
O1 Zr1 O1 120.14(13) 16_556 19_655
O1 Zr1 O1 75.97(12) 11_656 19_655
O3 Zr1 Zr2 34.95(4) . .
O3 Zr1 Zr2 89.83(8) 19_655 .
O4 Zr1 Zr2 35.35(5) . .
O4 Zr1 Zr2 90.02(9) 16_556 .
O1 Zr1 Zr2 74.77(6) . .
O1 Zr1 Zr2 110.66(6) 16_556 .
O1 Zr1 Zr2 165.08(6) 11_656 .
O1 Zr1 Zr2 110.54(6) 19_655 .
O3 Zr1 Zr2 34.95(4) . 16_556
O3 Zr1 Zr2 89.83(8) 19_655 16_556
O4 Zr1 Zr2 90.02(9) . 16_556
O4 Zr1 Zr2 35.35(5) 16_556 16_556
O1 Zr1 Zr2 110.66(6) . 16_556
O1 Zr1 Zr2 74.77(6) 16_556 16_556
O1 Zr1 Zr2 110.54(6) 11_656 16_556
O1 Zr1 Zr2 165.08(6) 19_655 16_556
Zr2 Zr1 Zr2 59.998(16) . 16_556
O3 Zr1 Zr2 89.83(8) . 4_655
O3 Zr1 Zr2 34.94(4) 19_655 4_655
O4 Zr1 Zr2 35.35(5) . 4_655
O4 Zr1 Zr2 90.01(9) 16_556 4_655
O1 Zr1 Zr2 110.54(6) . 4_655
O1 Zr1 Zr2 165.08(6) 16_556 4_655
O1 Zr1 Zr2 110.66(6) 11_656 4_655
O1 Zr1 Zr2 74.77(6) 19_655 4_655
Zr2 Zr1 Zr2 60.363(15) . 4_655
Zr2 Zr1 Zr2 90.314(16) 16_556 4_655
O3 Zr1 Zr2 89.83(8) . 13_656
O3 Zr1 Zr2 34.94(4) 19_655 13_656
O4 Zr1 Zr2 90.02(9) . 13_656
O4 Zr1 Zr2 35.34(5) 16_556 13_656
O1 Zr1 Zr2 165.08(6) . 13_656
O1 Zr1 Zr2 110.54(6) 16_556 13_656
O1 Zr1 Zr2 74.77(6) 11_656 13_656
O1 Zr1 Zr2 110.66(6) 19_655 13_656
Zr2 Zr1 Zr2 90.314(16) . 13_656
Zr2 Zr1 Zr2 60.364(15) 16_556 13_656
Zr2 Zr1 Zr2 59.998(16) 4_655 13_656
O3 Zr2 O3 69.59(12) 7_556 .
O3 Zr2 O4 71.06(11) 7_556 4_655
O3 Zr2 O4 108.93(13) . 4_655
O3 Zr2 O4 108.93(13) 7_556 .
O3 Zr2 O4 71.06(11) . .
O4 Zr2 O4 69.31(14) 4_655 .
O3 Zr2 O6 145.01(6) 7_556 .
O3 Zr2 O6 145.01(6) . .
O4 Zr2 O6 86.76(13) 4_655 .
O4 Zr2 O6 86.76(13) . .
O3 Zr2 O2 139.90(9) 7_556 .
O3 Zr2 O2 75.63(9) . .
O4 Zr2 O2 141.38(9) 4_655 .
O4 Zr2 O2 76.80(10) . .
O6 Zr2 O2 73.10(8) . .
O3 Zr2 O2 75.63(9) 7_556 23
O3 Zr2 O2 139.90(9) . 23
O4 Zr2 O2 76.80(10) 4_655 23
O4 Zr2 O2 141.38(9) . 23
O6 Zr2 O2 73.10(8) . 23
O2 Zr2 O2 125.17(12) . 23
O3 Zr2 O5 76.87(11) 7_556 .
O3 Zr2 O5 76.87(11) . .
O4 Zr2 O5 142.23(7) 4_655 .
O4 Zr2 O5 142.23(7) . .
O6 Zr2 O5 110.01(13) . .
O2 Zr2 O5 76.35(7) . .
O2 Zr2 O5 76.35(7) 23 .
O3 Zr2 Zr1 35.23(8) 7_556 13_656
O3 Zr2 Zr1 89.31(8) . 13_656
O4 Zr2 Zr1 35.84(8) 4_655 13_656
O4 Zr2 Zr1 89.50(9) . 13_656
O6 Zr2 Zr1 117.98(6) . 13_656
O2 Zr2 Zr1 162.21(6) . 13_656
O2 Zr2 Zr1 72.56(6) 23 13_656
O5 Zr2 Zr1 109.81(6) . 13_656
O3 Zr2 Zr2 34.80(6) 7_556 16_556
O3 Zr2 Zr2 34.80(6) . 16_556
O4 Zr2 Zr2 90.44(10) 4_655 16_556
O4 Zr2 Zr2 90.44(10) . 16_556
O6 Zr2 Zr2 176.59(10) . 16_556
O2 Zr2 Zr2 108.15(7) . 16_556
O2 Zr2 Zr2 108.15(7) 23 16_556
O5 Zr2 Zr2 73.40(9) . 16_556
Zr1 Zr2 Zr2 60.000(8) 13_656 16_556
O3 Zr2 Zr1 89.31(8) 7_556 .
O3 Zr2 Zr1 35.22(8) . .
O4 Zr2 Zr1 89.50(9) 4_655 .
O4 Zr2 Zr1 35.84(8) . .
O6 Zr2 Zr1 117.98(6) . .
O2 Zr2 Zr1 72.56(6) . .
O2 Zr2 Zr1 162.21(6) 23 .
O5 Zr2 Zr1 109.81(6) . .
Zr1 Zr2 Zr1 89.685(16) 13_656 .
Zr2 Zr2 Zr1 60.001(8) 16_556 .
O3 Zr2 Zr2 89.55(9) 7_556 4_655
O3 Zr2 Zr2 89.55(9) . 4_655
O4 Zr2 Zr2 34.66(7) 4_655 4_655
O4 Zr2 Zr2 34.66(7) . 4_655
O6 Zr2 Zr2 86.59(10) . 4_655
O2 Zr2 Zr2 109.82(6) . 4_655
O2 Zr2 Zr2 109.82(6) 23 4_655
O5 Zr2 Zr2 163.40(9) . 4_655
Zr1 Zr2 Zr2 59.818(8) 13_656 4_655
Zr2 Zr2 Zr2 90.001(1) 16_556 4_655
Zr1 Zr2 Zr2 59.819(8) . 4_655
C1 O1 Zr1 131.5(2) . .
C1 O2 Zr2 133.0(2) . .
Zr2 O3 Zr2 110.40(12) 16_556 .
Zr2 O3 Zr1 109.83(10) 16_556 .
Zr2 O3 Zr1 109.83(10) . .
Zr2 O4 Zr2 110.68(14) . 4_655
Zr2 O4 Zr1 108.81(11) . .
Zr2 O4 Zr1 108.81(11) 4_655 .
O2 C1 O1 128.0(4) . .
O2 C1 C2 116.3(4) . .
O1 C1 C2 115.5(4) . .
C3 C2 C7 119.6(4) . .
C3 C2 C1 120.8(4) . .
C7 C2 C1 119.6(4) . .
C2 C3 C4 120.6(4) . .
C5 C4 C3 120.0(4) . .
C6 C5 C4 119.2(4) . .
C6 C5 C9 120.6(4) . .
C4 C5 C9 120.1(4) . .
C5 C6 C7 120.3(4) . .
C2 C7 C6 120.3(4) . .
C9 C8 C9 121.7(6) . 20
C9 C8 O7 119.1(3) . .
C9 C8 O7 119.1(3) 20 .
C8 C9 C10 119.7(5) . .
C8 C9 C5 119.5(4) . .
C10 C9 C5 120.8(4) . .
C9 C10 C11 119.8(4) . .
C9 C10 C12 121.8(5) . .
C11 C10 C12 116.4(5) . .
C10 C11 C10 119.3(5) 20 .
C10 C11 C11 120.3(3) 20 16
C10 C11 C11 120.3(3) . 16
C12 C12 C10 122.0(4) 16 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O3 2.150(3) .
Zr1 O3 2.150(3) 19_655
Zr1 O4 2.169(3) .
Zr1 O4 2.169(3) 16_556
Zr1 O1 2.200(2) .
Zr1 O1 2.200(2) 16_556
Zr1 O1 2.200(2) 11_656
Zr1 O1 2.200(2) 19_655
Zr1 Zr2 3.5072(5) .
Zr1 Zr2 3.5072(5) 16_556
Zr1 Zr2 3.5072(5) 4_655
Zr1 Zr2 3.5072(5) 13_656
Zr2 O3 2.1355(16) 7_556
Zr2 O3 2.1355(16) .
Zr2 O4 2.1434(18) 4_655
Zr2 O4 2.1436(18) .
Zr2 O6 2.215(3) .
Zr2 O2 2.241(2) .
Zr2 O2 2.241(2) 23
Zr2 O5 2.280(3) .
Zr2 Zr2 3.5071(9) 16_556
Zr2 Zr2 3.5264(9) 4_655
O1 C1 1.256(4) .
O2 C1 1.256(4) .
O7 C8 1.456(8) .
C1 C2 1.504(5) .
C2 C3 1.358(4) .
C2 C7 1.366(4) .
C3 C4 1.407(4) .
C4 C5 1.376(5) .
C5 C6 1.367(5) .
C5 C9 1.512(5) .
C6 C7 1.409(4) .
C8 C9 1.377(4) .
C8 C9 1.377(4) 20
C9 C10 1.394(5) .
C10 C11 1.408(4) .
C10 C12 1.452(9) .
C11 C11 1.471(9) 16
C12 C12 1.356(18) 16
