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#$Date: 2020-06-28 01:23:52 +0300 (Sun, 28 Jun 2020) $
#$Revision: 253527 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/36/4003609.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_4003609
loop_
_publ_author_name
'Gosselin, Eric J.'
'Decker, Gerald E.'
'McNichols, Brett W.'
'Baumann, James E.'
'Yap, Glenn P. A.'
'Sellinger, Alan'
'Bloch, Eric D.'
_publ_section_title
;
 Ligand-Based Phase Control in Porous Zirconium Coordination Cages
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c01965
_journal_year                    2020
_chemical_formula_moiety         'C66 H57 F3 O20 Zr6, 2(Cl)'
_chemical_formula_sum            'C66 H57 Cl2 F3 O20 Zr6'
_chemical_formula_weight         1845.33
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.4279(9)
_cell_length_b                   16.4279(9)
_cell_length_c                   21.9721(19)
_cell_measurement_reflns_used    2193
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.67
_cell_measurement_theta_min      3.70
_cell_volume                     5135.3(6)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36400
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.794
_diffrn_reflns_theta_min         3.106
_exptl_absorpt_coefficient_mu    5.757
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.226
_refine_diff_density_max         3.762
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.231
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.34(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.277
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3616
_refine_ls_number_restraints     289
_refine_ls_restrained_S_all      1.256
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0885
_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)+(0.1669P)²+7.5273P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2477
_refine_ls_wR_factor_ref         0.2514
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                3523
_reflns_number_total             3616
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm0c01965_si_010.cif
_cod_data_source_block           eric316a_sq
_cod_original_cell_volume        5135.3(7)
_cod_database_code               4003609
_shelx_shelxl_version_number     2018/3
_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. 
;
_shelx_estimated_absorpt_t_min   0.203
_shelx_estimated_absorpt_t_max   0.356
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1A Zr 0.38054(7) 0.80060(6) 0.58524(3) 0.0395(4) Uani 1 1 d . . . . .
Cl1 Cl 0.1765(3) 0.7524(4) 0.750000 0.0366(9) Uani 0.6667 2 d S T P . .
O1 O 0.333333 0.666667 0.5500(5) 0.032(2) Uani 1 3 d S T P A .
O2 O 0.2544(5) 0.7092(6) 0.6320(3) 0.0441(17) Uani 1 1 d . . . . .
H2O H 0.228478 0.723262 0.666362 0.053 Uiso 1 1 calc R U . . .
O3 O 0.2929(6) 0.7985(6) 0.5091(3) 0.0486(18) Uani 1 1 d . U . . .
O4 O 0.1681(6) 0.6509(7) 0.5122(4) 0.0517(18) Uani 1 1 d . U . . .
C1 C 0.3727(11) 0.8999(9) 0.66586(6) 0.126(6) Uani 1 1 d DG U . A -1
H1 H 0.325541 0.862423 0.694644 0.151 Uiso 1 1 calc R U . A -1
C2 C 0.4669(12) 0.9184(10) 0.66583(6) 0.124(6) Uani 1 1 d DG U . A -1
H2 H 0.493843 0.895570 0.694592 0.149 Uiso 1 1 calc R U . A -1
C3 C 0.5138(11) 0.9772(12) 0.61525(9) 0.149(7) Uani 1 1 d G U . A -1
H3 H 0.577636 1.000534 0.604244 0.179 Uiso 1 1 calc R U . A -1
C4 C 0.4486(13) 0.9950(8) 0.58403(7) 0.163(8) Uani 1 1 d DG U . A -1
H4 H 0.461121 1.032257 0.548458 0.196 Uiso 1 1 calc R U . A -1
C5 C 0.3614(13) 0.9472(13) 0.61530(9) 0.139(6) Uani 1 1 d DG U . A -1
H5 H 0.305318 0.946900 0.604328 0.167 Uiso 1 1 calc R U . A -1
C6 C 0.2254(8) 0.7252(9) 0.4846(4) 0.045(2) Uani 1 1 d . U . . .
C7 C 0.2074(9) 0.7256(10) 0.4182(5) 0.051(2) Uani 1 1 d . U . . .
H7 H 0.148454 0.680284 0.401688 0.062 Uiso 1 1 calc R U . . .
C8 C 0.2740(9) 0.7898(9) 0.3814(5) 0.050(2) Uani 1 1 d D U . . .
H8 H 0.328171 0.838820 0.400691 0.060 Uiso 1 1 calc R U . B .
C9 C 0.272(2) 0.792(4) 0.3145(9) 0.045(5) Uani 0.5 1 d DG U P B -1
C10 C 0.1864(14) 0.735(2) 0.2860(14) 0.057(6) Uani 0.5 1 d G U P B -1
C11 C 0.1801(12) 0.735(2) 0.2229(14) 0.049(5) Uani 0.5 1 d G U P B -1
H11 H 0.121524 0.696115 0.203449 0.059 Uiso 0.5 1 calc R U P B -1
C12 C 0.260(2) 0.791(4) 0.1883(9) 0.048(7) Uani 0.5 1 d G U P B -1
C13 C 0.3453(14) 0.848(2) 0.2168(16) 0.053(6) Uani 0.5 1 d G U P B -1
H13 H 0.399638 0.886818 0.193147 0.063 Uiso 0.5 1 calc R U P B -1
C14 C 0.3516(12) 0.849(2) 0.2799(17) 0.053(5) Uani 0.5 1 d G U P B -1
H14 H 0.410145 0.887548 0.299374 0.063 Uiso 0.5 1 calc R U P B -1
F1 F 0.1013(13) 0.6833(14) 0.3078(7) 0.076(5) Uani 0.5 1 d . U P B -1
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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
_geom_angle_publ_flag
O1 Zr1A O2 73.7(3) . 3_565 ?
O1 Zr1A O2 73.5(3) . . ?
O2 Zr1A O2 91.7(4) 3_565 . ?
O1 Zr1A O4 79.2(3) . 3_565 ?
O2 Zr1A O4 85.3(3) 3_565 3_565 ?
O2 Zr1A O4 152.2(3) . 3_565 ?
O1 Zr1A O3 78.7(3) . . ?
O2 Zr1A O3 151.4(3) 3_565 . ?
O2 Zr1A O3 87.6(3) . . ?
O4 Zr1A O3 82.2(3) 3_565 . ?
O1 Zr1A C1 148.8(3) . . ?
O2 Zr1A C1 99.6(4) 3_565 . ?
O2 Zr1A C1 76.3(4) . . ?
O4 Zr1A C1 131.4(4) 3_565 . ?
O3 Zr1A C1 108.0(4) . . ?
O1 Zr1A C2 148.9(4) . . ?
O2 Zr1A C2 76.1(4) 3_565 . ?
O2 Zr1A C2 100.5(4) . . ?
O4 Zr1A C2 105.5(4) 3_565 . ?
O3 Zr1A C2 132.2(4) . . ?
C1 Zr1A C2 33.45(9) . . ?
O1 Zr1A C5 153.9(4) . . ?
O2 Zr1A C5 128.4(3) 3_565 . ?
O2 Zr1A C5 90.3(4) . . ?
O4 Zr1A C5 113.1(4) 3_565 . ?
O3 Zr1A C5 80.3(3) . . ?
C1 Zr1A C5 31.89(19) . . ?
C2 Zr1A C5 52.9(2) . . ?
O1 Zr1A C3 154.1(4) . . ?
O2 Zr1A C3 90.5(4) 3_565 . ?
O2 Zr1A C3 128.5(3) . . ?
O4 Zr1A C3 79.2(3) 3_565 . ?
O3 Zr1A C3 112.1(4) . . ?
C1 Zr1A C3 52.7(2) . . ?
C2 Zr1A C3 31.45(18) . . ?
C5 Zr1A C3 50.72(19) . . ?
O1 Zr1A C4 157.6(3) . . ?
O2 Zr1A C4 120.3(4) 3_565 . ?
O2 Zr1A C4 120.2(4) . . ?
O4 Zr1A C4 84.5(4) 3_565 . ?
O3 Zr1A C4 84.0(3) . . ?
C1 Zr1A C4 51.3(2) . . ?
C2 Zr1A C4 51.1(2) . . ?
C5 Zr1A C4 29.95(13) . . ?
C3 Zr1A C4 29.81(12) . . ?
O1 Zr1A Zr1A 36.51(14) . 3_565 ?
O2 Zr1A Zr1A 37.8(2) 3_565 3_565 ?
O2 Zr1A Zr1A 85.7(2) . 3_565 ?
O4 Zr1A Zr1A 75.0(2) 3_565 3_565 ?
O3 Zr1A Zr1A 113.7(2) . 3_565 ?
C1 Zr1A Zr1A 133.5(3) . 3_565 ?
C2 Zr1A Zr1A 113.8(3) . 3_565 ?
C5 Zr1A Zr1A 165.20(13) . 3_565 ?
C3 Zr1A Zr1A 122.8(4) . 3_565 ?
C4 Zr1A Zr1A 150.1(4) . 3_565 ?
O1 Zr1A Zr1A 36.51(14) . 2_665 ?
O2 Zr1A Zr1A 85.8(2) 3_565 2_665 ?
O2 Zr1A Zr1A 37.7(2) . 2_665 ?
O4 Zr1A Zr1A 114.6(2) 3_565 2_665 ?
O3 Zr1A Zr1A 76.2(2) . 2_665 ?
C1 Zr1A Zr1A 114.0(3) . 2_665 ?
C2 Zr1A Zr1A 134.2(3) . 2_665 ?
C5 Zr1A Zr1A 122.4(4) . 2_665 ?
C3 Zr1A Zr1A 165.34(13) . 2_665 ?
C4 Zr1A Zr1A 149.8(4) . 2_665 ?
Zr1A Zr1A Zr1A 60.0 3_565 2_665 ?
Zr1A O1 Zr1A 107.0(3) . 2_665 ?
Zr1A O1 Zr1A 107.0(3) . 3_565 ?
Zr1A O1 Zr1A 107.0(3) 2_665 3_565 ?
Zr1A O2 Zr1A 104.6(3) 2_665 . ?
Zr1A O2 H2O 127.7 2_665 . ?
Zr1A O2 H2O 127.7 . . ?
C6 O3 Zr1A 126.1(7) . . ?
C6 O4 Zr1A 127.3(7) . 2_665 ?
C2 C1 C5 108.0 . . ?
C2 C1 Zr1A 74.3(7) . . ?
C5 C1 Zr1A 82.2(3) . . ?
C2 C1 H1 126.0 . . ?
C5 C1 H1 126.0 . . ?
Zr1A C1 H1 110.3 . . ?
C1 C2 C3 108.0 . . ?
C1 C2 Zr1A 72.3(7) . . ?
C3 C2 Zr1A 82.9(3) . . ?
C1 C2 H2 126.0 . . ?
C3 C2 H2 126.0 . . ?
Zr1A C2 H2 111.3 . . ?
C2 C3 C4 108.0 . . ?
C2 C3 Zr1A 65.67(12) . . ?
C4 C3 Zr1A 79.2(5) . . ?
C2 C3 H3 126.0 . . ?
C4 C3 H3 126.0 . . ?
Zr1A C3 H3 120.6 . . ?
C5 C4 C3 108.0 . . ?
C5 C4 Zr1A 69.4(5) . . ?
C3 C4 Zr1A 71.0(5) . . ?
C5 C4 H4 126.0 . . ?
C3 C4 H4 126.0 . . ?
Zr1A C4 H4 125.2 . . ?
C4 C5 C1 108.0 . . ?
C4 C5 Zr1A 80.6(5) . . ?
C1 C5 Zr1A 65.94(14) . . ?
C4 C5 H5 126.0 . . ?
C1 C5 H5 126.0 . . ?
Zr1A C5 H5 119.0 . . ?
O4 C6 O3 125.8(9) . . ?
O4 C6 C7 114.9(11) . . ?
O3 C6 C7 119.3(10) . . ?
C8 C7 C6 120.4(12) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 127.0(18) . . ?
C7 C8 H8 116.5 . . ?
C9 C8 H8 116.5 . . ?
C10 C9 C14 120.0 . . ?
C10 C9 C8 117(3) . . ?
C14 C9 C8 123(3) . . ?
F1 C10 C9 132(3) . . ?
F1 C10 C11 108(3) . . ?
C9 C10 C11 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C9 120.0 . . ?
C13 C14 H14 120.0 . . ?
C9 C14 H14 120.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1A O1 2.083(4) . ?
Zr1A O2 2.113(8) 3_565 ?
Zr1A O2 2.119(7) . ?
Zr1A O4 2.192(8) 3_565 ?
Zr1A O3 2.196(8) . ?
Zr1A C1 2.454(11) . ?
Zr1A C2 2.480(11) . ?
Zr1A C5 2.663(17) . ?
Zr1A C3 2.701(16) . ?
Zr1A C4 2.806(11) . ?
Zr1A Zr1A 3.3478(15) 3_565 ?
Zr1A Zr1A 3.3479(15) 2_665 ?
O2 H2O 0.9500 . ?
O3 C6 1.278(14) . ?
O4 C6 1.262(14) . ?
C1 C2 1.4200 . ?
C1 C5 1.4200 . ?
C1 H1 0.9500 . ?
C2 C3 1.4200 . ?
C2 H2 0.9500 . ?
C3 C4 1.4200 . ?
C3 H3 0.9500 . ?
C4 C5 1.4200 . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.489(14) . ?
C7 C8 1.345(17) . ?
C7 H7 0.9500 . ?
C8 C9 1.471(19) . ?
C8 H8 0.9500 . ?
C9 C10 1.3900 . ?
C9 C14 1.3900 . ?
C10 F1 1.31(2) . ?
C10 C11 1.3900 . ?
C11 C12 1.3900 . ?
C11 H11 0.9500 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
