#------------------------------------------------------------------------------
#$Date: 2019-11-26 03:05:56 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242467 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/24/4132494.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_4132494
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 Hf3 O16'
_chemical_formula_weight         1342.09
_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                   20.5524(17)
_cell_length_b                   34.409(2)
_cell_length_c                   21.0160(16)
_cell_measurement_reflns_used    512
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.316
_cell_measurement_theta_min      4.574
_cell_volume                     14862.3(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            79381
_diffrn_reflns_theta_full        12.98
_diffrn_reflns_theta_max         12.98
_diffrn_reflns_theta_min         0.56
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'Light yellow'
_exptl_crystal_density_diffrn    0.600
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.791
_refine_diff_density_min         -2.069
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         5348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1910P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2391
_refine_ls_wR_factor_ref         0.2524
_reflns_number_gt                4221
_reflns_number_total             5348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b04277_si_004.cif
_cod_data_source_block           NPF-300-Hf
_cod_original_cell_volume        14862.1(19)
_cod_original_sg_symbol_H-M      Cmmm
_cod_database_code               4132494
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
Hf1 Hf 0.0000 0.070626(17) 0.5000 0.0605(4) Uani 1 4 d S
Hf2 Hf 0.08551(3) 0.0000 0.41616(2) 0.0632(4) Uani 1 2 d S
O1 O 0.0867(5) 0.0344(3) 0.5000 0.089(3) Uani 1 2 d S
O3 O 0.0643(3) 0.10376(15) 0.4380(3) 0.0646(15) Uani 1 1 d .
O2 O 0.0000 0.0348(3) 0.4147(5) 0.084(3) Uani 1 2 d S
O5 O 0.0787(5) 0.0000 0.3140(4) 0.090(3) Uani 1 2 d S
O4 O 0.1191(4) 0.05878(17) 0.3817(3) 0.087(2) Uani 1 1 d .
O6 O 0.1920(5) 0.0000 0.4218(5) 0.093(3) Uani 1 2 d S
C1 C 0.1027(7) 0.0932(3) 0.3960(5) 0.087(3) Uani 1 1 d .
C13 C 0.1397(6) 0.1249(3) 0.3588(5) 0.086(3) Uani 1 1 d .
C12 C 0.1748(6) 0.1171(3) 0.3073(4) 0.087(3) Uani 1 1 d .
H12A H 0.1816 0.0910 0.2939 0.104 Uiso 1 1 calc R
C11 C 0.2500 0.2500 0.2868(5) 0.092(5) Uani 1 2 d S
H11A H 0.2500 0.2500 0.3320 0.111 Uiso 1 2 calc SR
C10 C 0.1970(6) 0.1853(3) 0.2920(4) 0.096(4) Uani 1 1 d .
C9 C 0.2243(7) 0.2188(3) 0.1894(4) 0.110(4) Uani 1 1 d .
H9A H 0.2085 0.1972 0.1659 0.132 Uiso 1 1 calc R
C8 C 0.2015(7) 0.1481(3) 0.2733(5) 0.107(4) Uani 1 1 d .
H8A H 0.2241 0.1426 0.2349 0.128 Uiso 1 1 calc R
C7 C 0.2211(6) 0.2184(3) 0.2557(4) 0.104(4) Uani 1 1 d .
C6 C 0.1293(7) 0.1633(2) 0.3790(4) 0.097(4) Uani 1 1 d .
H6B H 0.1032 0.1689 0.4152 0.117 Uiso 1 1 calc R
C5 C 0.1575(7) 0.1919(3) 0.3456(5) 0.112(4) Uani 1 1 d .
H5B H 0.1505 0.2179 0.3588 0.134 Uiso 1 1 calc R
C4 C 0.2500 0.2500 0.1579(5) 0.105(6) Uani 1 2 d S
C3 C 0.2500 0.2500 0.0873(7) 0.170(13) Uani 1 2 d S
C2 C 0.2500 0.2500 0.0336(7) 0.151(10) 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'
Hf Hf -0.3548 4.1643 '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
O2 Hf1 O2 111.0(6) . 10_556
O2 Hf1 O1 71.05(19) . .
O2 Hf1 O1 71.05(19) 10_556 .
O2 Hf1 O1 71.05(19) . 3_556
O2 Hf1 O1 71.05(19) 10_556 3_556
O1 Hf1 O1 110.0(6) . 3_556
O2 Hf1 O3 142.16(18) . 10_556
O2 Hf1 O3 78.6(3) 10_556 10_556
O1 Hf1 O3 78.7(3) . 10_556
O1 Hf1 O3 142.84(16) 3_556 10_556
O2 Hf1 O3 78.6(3) . .
O2 Hf1 O3 142.16(18) 10_556 .
O1 Hf1 O3 78.7(3) . .
O1 Hf1 O3 142.84(16) 3_556 .
O3 Hf1 O3 73.5(3) 10_556 .
O2 Hf1 O3 142.16(18) . 3_556
O2 Hf1 O3 78.6(3) 10_556 3_556
O1 Hf1 O3 142.84(16) . 3_556
O1 Hf1 O3 78.7(3) 3_556 3_556
O3 Hf1 O3 74.7(3) 10_556 3_556
O3 Hf1 O3 116.9(3) . 3_556
O2 Hf1 O3 78.6(3) . 12
O2 Hf1 O3 142.16(18) 10_556 12
O1 Hf1 O3 142.84(16) . 12
O1 Hf1 O3 78.7(3) 3_556 12
O3 Hf1 O3 116.9(3) 10_556 12
O3 Hf1 O3 74.7(3) . 12
O3 Hf1 O3 73.5(3) 3_556 12
O2 Hf1 Hf2 35.59(14) . 2
O2 Hf1 Hf2 91.3(2) 10_556 2
O1 Hf1 Hf2 90.8(3) . 2
O1 Hf1 Hf2 35.45(15) 3_556 2
O3 Hf1 Hf2 167.24(15) 10_556 2
O3 Hf1 Hf2 111.65(15) . 2
O3 Hf1 Hf2 111.25(17) 3_556 2
O3 Hf1 Hf2 75.88(14) 12 2
O2 Hf1 Hf2 35.59(14) . .
O2 Hf1 Hf2 91.3(2) 10_556 .
O1 Hf1 Hf2 35.45(16) . .
O1 Hf1 Hf2 90.8(3) 3_556 .
O3 Hf1 Hf2 111.25(17) 10_556 .
O3 Hf1 Hf2 75.88(14) . .
O3 Hf1 Hf2 167.24(14) 3_556 .
O3 Hf1 Hf2 111.65(15) 12 .
Hf2 Hf1 Hf2 60.698(19) 2 .
O2 Hf1 Hf2 91.3(2) . 10_556
O2 Hf1 Hf2 35.59(14) 10_556 10_556
O1 Hf1 Hf2 35.45(16) . 10_556
O1 Hf1 Hf2 90.8(3) 3_556 10_556
O3 Hf1 Hf2 75.88(14) 10_556 10_556
O3 Hf1 Hf2 111.25(17) . 10_556
O3 Hf1 Hf2 111.65(15) 3_556 10_556
O3 Hf1 Hf2 167.24(14) 12 10_556
Hf2 Hf1 Hf2 91.363(18) 2 10_556
Hf2 Hf1 Hf2 60.869(16) . 10_556
O2 Hf1 Hf2 91.3(2) . 9_556
O2 Hf1 Hf2 35.59(14) 10_556 9_556
O1 Hf1 Hf2 90.8(3) . 9_556
O1 Hf1 Hf2 35.45(15) 3_556 9_556
O3 Hf1 Hf2 111.65(15) 10_556 9_556
O3 Hf1 Hf2 167.24(15) . 9_556
O3 Hf1 Hf2 75.88(14) 3_556 9_556
O3 Hf1 Hf2 111.25(17) 12 9_556
Hf2 Hf1 Hf2 60.869(16) 2 9_556
Hf2 Hf1 Hf2 91.363(19) . 9_556
Hf2 Hf1 Hf2 60.698(19) 10_556 9_556
O1 Hf2 O1 67.8(5) . 11
O1 Hf2 O2 109.6(4) . 2
O1 Hf2 O2 73.0(3) 11 2
O1 Hf2 O2 73.0(3) . .
O1 Hf2 O2 109.6(4) 11 .
O2 Hf2 O2 68.6(4) 2 .
O1 Hf2 O5 146.0(2) . .
O1 Hf2 O5 146.0(2) 11 .
O2 Hf2 O5 86.1(4) 2 .
O2 Hf2 O5 86.1(4) . .
O1 Hf2 O6 86.8(4) . .
O1 Hf2 O6 86.8(4) 11 .
O2 Hf2 O6 145.6(2) 2 .
O2 Hf2 O6 145.6(2) . .
O5 Hf2 O6 96.8(4) . .
O1 Hf2 O4 76.3(3) . .
O1 Hf2 O4 139.7(3) 11 .
O2 Hf2 O4 138.9(3) 2 .
O2 Hf2 O4 75.1(3) . .
O5 Hf2 O4 72.5(2) . .
O6 Hf2 O4 73.2(2) . .
O1 Hf2 O4 139.7(3) . 11
O1 Hf2 O4 76.3(3) 11 11
O2 Hf2 O4 75.1(3) 2 11
O2 Hf2 O4 138.9(3) . 11
O5 Hf2 O4 72.5(2) . 11
O6 Hf2 O4 73.2(2) . 11
O4 Hf2 O4 127.3(3) . 11
O1 Hf2 Hf1 88.5(3) . 9_556
O1 Hf2 Hf1 36.5(2) 11 9_556
O2 Hf2 Hf1 36.5(2) 2 9_556
O2 Hf2 Hf1 89.0(3) . 9_556
O5 Hf2 Hf1 118.21(18) . 9_556
O6 Hf2 Hf1 118.50(16) . 9_556
O4 Hf2 Hf1 160.64(16) . 9_556
O4 Hf2 Hf1 72.02(16) 11 9_556
O1 Hf2 Hf1 36.5(2) . .
O1 Hf2 Hf1 88.5(3) 11 .
O2 Hf2 Hf1 89.0(3) 2 .
O2 Hf2 Hf1 36.5(2) . .
O5 Hf2 Hf1 118.21(18) . .
O6 Hf2 Hf1 118.50(16) . .
O4 Hf2 Hf1 72.02(16) . .
O4 Hf2 Hf1 160.64(16) 11 .
Hf1 Hf2 Hf1 88.637(18) 9_556 .
O1 Hf2 Hf2 90.6(3) . 2
O1 Hf2 Hf2 90.6(3) 11 2
O2 Hf2 Hf2 34.3(2) 2 2
O2 Hf2 Hf2 34.3(2) . 2
O5 Hf2 Hf2 86.3(3) . 2
O6 Hf2 Hf2 176.9(3) . 2
O4 Hf2 Hf2 107.8(2) . 2
O4 Hf2 Hf2 107.8(2) 11 2
Hf1 Hf2 Hf2 59.651(10) 9_556 2
Hf1 Hf2 Hf2 59.651(10) . 2
O1 Hf2 Hf2 33.9(2) . 10_556
O1 Hf2 Hf2 33.9(2) 11 10_556
O2 Hf2 Hf2 90.8(3) 2 10_556
O2 Hf2 Hf2 90.8(3) . 10_556
O5 Hf2 Hf2 176.3(3) . 10_556
O6 Hf2 Hf2 86.9(3) . 10_556
O4 Hf2 Hf2 108.73(16) . 10_556
O4 Hf2 Hf2 108.73(16) 11 10_556
Hf1 Hf2 Hf2 59.565(8) 9_556 10_556
Hf1 Hf2 Hf2 59.565(8) . 10_556
Hf2 Hf2 Hf2 90.0 2 10_556
Hf2 O1 Hf2 112.2(5) . 10_556
Hf2 O1 Hf1 108.1(3) . .
Hf2 O1 Hf1 108.1(3) 10_556 .
C1 O3 Hf1 131.3(5) . .
Hf2 O2 Hf2 111.4(4) . 2
Hf2 O2 Hf1 107.9(3) . .
Hf2 O2 Hf1 107.9(3) 2 .
C1 O4 Hf2 132.8(6) . .
O3 C1 O4 127.7(8) . .
O3 C1 C13 118.0(8) . .
O4 C1 C13 114.1(9) . .
C12 C13 C6 121.3(9) . .
C12 C13 C1 122.5(8) . .
C6 C13 C1 116.0(9) . .
C13 C12 C8 118.4(9) . .
C7 C11 C7 124.5(11) . 6
C8 C10 C5 115.3(9) . .
C8 C10 C7 124.7(9) . .
C5 C10 C7 119.2(9) . .
C4 C9 C7 120.6(9) . .
C10 C8 C12 123.6(9) . .
C9 C7 C11 115.9(8) . .
C9 C7 C10 123.1(8) . .
C11 C7 C10 120.5(8) . .
C5 C6 C13 117.8(9) . .
C6 C5 C10 123.4(9) . .
C9 C4 C9 122.1(11) 6 .
C9 C4 C3 118.9(6) 6 .
C9 C4 C3 118.9(6) . .
C2 C3 C4 180.000(2) . .
C3 C2 C2 180.000(2) . 13
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hf1 O2 2.174(8) .
Hf1 O2 2.174(8) 10_556
Hf1 O1 2.175(8) .
Hf1 O1 2.175(8) 3_556
Hf1 O3 2.178(5) 10_556
Hf1 O3 2.178(5) .
Hf1 O3 2.178(5) 3_556
Hf1 O3 2.178(5) 12
Hf1 Hf2 3.4784(6) 2
Hf1 Hf2 3.4784(6) .
Hf1 Hf2 3.4784(6) 10_556
Hf1 Hf2 3.4784(6) 9_556
Hf2 O1 2.122(6) .
Hf2 O1 2.122(6) 11
Hf2 O2 2.128(5) 2
Hf2 O2 2.128(5) .
Hf2 O5 2.152(9) .
Hf2 O6 2.191(10) .
Hf2 O4 2.257(6) .
Hf2 O4 2.257(6) 11
Hf2 Hf1 3.4784(6) 9_556
Hf2 Hf2 3.5150(12) 2
Hf2 Hf2 3.5240(9) 10_556
O1 Hf2 2.122(6) 10_556
O3 C1 1.238(12) .
O2 Hf2 2.128(5) 2
O4 C1 1.269(11) .
C1 C13 1.541(13) .
C13 C12 1.330(13) .
C13 C6 1.404(12) .
C12 C8 1.395(13) .
C11 C7 1.401(10) .
C11 C7 1.401(10) 6
C10 C8 1.341(14) .
C10 C5 1.408(14) .
C10 C7 1.457(12) .
C9 C4 1.368(11) .
C9 C7 1.396(13) .
C6 C5 1.339(13) .
C4 C9 1.368(11) 6
C4 C3 1.485(18) .
C3 C2 1.128(17) .
C2 C2 1.41(3) 13
