#------------------------------------------------------------------------------
#$Date: 2019-11-03 16:15:40 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/87/4128775.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_4128775
loop_
_publ_author_name
'Zhao, Yanming'
'Qi, Shibo'
'Niu, Zheng'
'Peng, Yunlei'
'Shan, Chuan'
'Verma, Gaurav'
'Wojtas, Lukasz'
'Zhang, Zhenjie'
'Zhang, Bao'
'Feng, Yaqing'
'Chen, Yu-Sheng'
'Ma, Shengqian'
_publ_section_title
;
 Robust Corrole-Based Metal-Organic Frameworks with Rare 9-Connected
 Zr/Hf-Oxo Clusters.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14443
_journal_page_last               14450
_journal_paper_doi               10.1021/jacs.9b07700
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C120 H60 Hf6 N12 O32'
_chemical_formula_sum            'C120 H60 Hf6 N12 O32'
_chemical_formula_weight         3252.74
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   28.6282(14)
_cell_length_b                   28.6282(14)
_cell_length_c                   25.6439(12)
_cell_measurement_reflns_used    4608
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      10.83
_cell_measurement_theta_min      2.40
_cell_volume                     18201.3(15)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1905
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            218346
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        12.283
_diffrn_reflns_theta_max         12.283
_diffrn_reflns_theta_min         0.827
_diffrn_source                   synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1443 before and 0.1144 after correction.
The Ratio of minimum to maximum transmission is 0.6966.
The λ/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.594
_exptl_crystal_description       plate
_exptl_crystal_F_000             3104
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3781
_refine_ls_number_restraints     616
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0879
_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)+(0.1380P)²+68.2968P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2468
_refine_ls_wR_factor_ref         0.3126
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2238
_reflns_number_total             3781
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b07700_si_003.cif
_cod_data_source_block           zym_3_0m_sq
_cod_original_cell_volume        18201(2)
_cod_database_code               4128775
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: Hf1(0.5) O3(0.5) O4(0.5) C12(0.5) C17(0.5) C16(0.5) H16(0.5)
 C15(0.5) H15(0.5) C14(0.5) C19(0.5) H19(0.5) C18(0.5) H18(0.5) C20(0.5)
 N22(0.5) C23(0.5) C24(0.5) H24(0.5) C25(0.5) H25(0.5) C21(0.5) C26(0.5)
 C27(0.5) H27(0.5) C28(0.5) H28(0.5) C29(0.5) N30(0.5) C31(0.25) C32(0.25)
 C33(0.25) H33(0.25) C34(0.25) H34(0.25) C35(0.25) C36(0.25) H36(0.25)
 C37(0.25) H37(0.25) O39(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C15(H15), C19(H19), C18(H18), C24(H24), C25(H25), C27(H27),
 C28(H28), C33(H33), C34(H34), C36(H36), C37(H37)
;
_olex2_submission_special_instructions 'No special instructions were received'
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'
'-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
Hf1 Hf 0.73739(5) 0.33403(6) 0.69417(4) 0.1281(7) Uani 0.5 1 d . . . A -1
O2 O 0.666667 0.333333 0.6658(7) 0.138(5) Uani 1 6 d S T P . .
O3 O 0.6686(8) 0.2609(9) 0.7194(9) 0.181(9) Uani 0.5 1 d . . . A -1
O4 O 0.7779(9) 0.2801(10) 0.7001(6) 0.223(11) Uani 0.5 1 d . . . A -1
O11 O 0.7678(4) 0.3839(2) 0.6243(3) 0.145(3) Uani 1 2 d S T P . .
C12 C 0.7493(10) 0.4157(10) 0.6064(8) 0.144(6) Uani 0.5 1 d . . . A -1
O13 O 0.7159(2) 0.4317(5) 0.6251(3) 0.145(4) Uani 1 2 d S T P . .
C17 C 0.7803(3) 0.4533(3) 0.4411(4) 0.129(6) Uani 0.5 1 d . . . A -1
C16 C 0.7515(3) 0.4719(3) 0.4698(4) 0.142(6) Uani 0.5 1 d . . . A -1
H16 H 0.737505 0.491984 0.453165 0.171 Uiso 0.5 1 calc R . . A -1
C15 C 0.7433(4) 0.4608(4) 0.5229(4) 0.140(6) Uani 0.5 1 d . . . A -1
H15 H 0.723726 0.473399 0.542539 0.168 Uiso 0.5 1 calc R . . A -1
C14 C 0.7637(5) 0.4314(4) 0.5474(5) 0.139(6) Uani 0.5 1 d . . . A -1
C19 C 0.7924(5) 0.4131(5) 0.5181(4) 0.134(6) Uani 0.5 1 d . . . A -1
H19 H 0.806434 0.393051 0.534713 0.161 Uiso 0.5 1 calc R . . A -1
C18 C 0.8009(5) 0.4240(4) 0.4649(4) 0.135(6) Uani 0.5 1 d . . . A -1
H18 H 0.820487 0.411400 0.445213 0.162 Uiso 0.5 1 calc R . . A -1
C20 C 0.7857(5) 0.4638(9) 0.3815(6) 0.127(6) Uani 0.5 1 d . . . A -1
N22 N 0.7444(6) 0.4676(4) 0.3017(4) 0.138(7) Uani 0.5 1 d . . . A -1
C23 C 0.6938(6) 0.4411(5) 0.2792(5) 0.139(7) Uani 0.5 1 d . . . A -1
C24 C 0.6571(4) 0.4104(3) 0.3184(6) 0.138(7) Uani 0.5 1 d . . . A -1
H24 H 0.619311 0.387977 0.313879 0.165 Uiso 0.5 1 calc R . . A -1
C25 C 0.6830(4) 0.4175(3) 0.3616(5) 0.136(7) Uani 0.5 1 d . . . A -1
H25 H 0.666912 0.400984 0.393861 0.163 Uiso 0.5 1 calc R . . A -1
C21 C 0.7381(5) 0.4531(3) 0.3540(4) 0.128(6) Uani 0.5 1 d . . . A -1
C26 C 0.8388(5) 0.4874(4) 0.3607(5) 0.141(6) Uani 0.5 1 d . . . A -1
C27 C 0.8890(5) 0.5078(3) 0.3847(4) 0.147(7) Uani 0.5 1 d . . . A -1
H27 H 0.895203 0.511182 0.421218 0.177 Uiso 0.5 1 calc R . . A -1
C28 C 0.9253(5) 0.5210(3) 0.3500(5) 0.163(8) Uani 0.5 1 d . . . A -1
H28 H 0.962673 0.535826 0.356814 0.195 Uiso 0.5 1 calc R . . A -1
C29 C 0.9017(6) 0.5104(3) 0.3000(4) 0.143(7) Uani 0.5 1 d . . . A -1
N30 N 0.8473(5) 0.4893(4) 0.3073(4) 0.125(5) Uani 0.5 1 d . . . A -1
C31 C 0.9261(9) 0.5202(10) 0.250000 0.142(8) Uani 0.5 2 d S T P . .
C32 C 0.9860(6) 0.5355(4) 0.250000 0.144(8) Uani 0.5 2 d S T P A .
C33 C 1.0011(6) 0.5022(3) 0.2758(2) 0.152(9) Uani 0.25 1 d . . . A -1
H33 H 0.974701 0.470852 0.293532 0.183 Uiso 0.25 1 calc R . . A -1
C34 C 1.0548(6) 0.5147(4) 0.2757(2) 0.159(10) Uani 0.25 1 d . . . A -1
H34 H 1.064919 0.491957 0.293304 0.191 Uiso 0.25 1 calc R . . A -1
C35 C 1.0935(6) 0.5603(5) 0.250000 0.178(9) Uani 0.5 2 d S T P . .
C36 C 1.0780(6) 0.5937(5) 0.2241(3) 0.158(10) Uani 0.25 1 d . . . A -1
H36 H 1.104314 0.625001 0.206365 0.189 Uiso 0.25 1 calc R . . A -1
C37 C 1.0242(6) 0.5812(4) 0.2241(3) 0.153(9) Uani 0.25 1 d . . . A -1
H37 H 1.013922 0.603883 0.206571 0.184 Uiso 0.25 1 calc R . . A -1
C38 C 1.1539(9) 0.5770(4) 0.250000 0.181(9) Uani 1 4 d S T P A .
O39 O 1.1790(5) 0.5721(8) 0.2866(4) 0.166(11) Uani 0.5 1 d . . . A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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'
Hf Hf -0.5166 2.4839 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0004 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0017 0.0018 '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 O4 142.1(6) . .
O2 Hf1 O11 78.0(5) . .
O3 Hf1 O2 71.9(6) . .
O3 Hf1 O4 81.5(9) . .
O3 Hf1 O11 139.5(6) . .
O11 Hf1 O4 108.4(5) . .
C12 O11 Hf1 124.2(11) . .
O11 C12 C14 112.7(12) . .
O13 C12 O11 134.4(17) . .
O13 C12 C14 112.2(12) . .
C16 C17 C20 117.9(11) . .
C18 C17 C16 120.7(11) . .
C18 C17 C20 121.3(11) . .
C15 C16 C17 119.6(11) . .
C14 C15 C16 120.5(11) . .
C15 C14 C12 118.6(10) . .
C15 C14 C19 119.3(11) . .
C19 C14 C12 122.0(10) . .
C18 C19 C14 120.8(12) . .
C17 C18 C19 119.2(12) . .
C21 C20 C17 116.9(11) . .
C26 C20 C17 116.2(11) . .
C26 C20 C21 126.6(14) . .
C23 N22 C21 107.2(11) . .
N22 C23 C24 107.2(10) . .
C25 C24 C23 109.0(8) . .
C24 C25 C21 110.1(9) . .
N22 C21 C20 116.6(12) . .
N22 C21 C25 106.4(10) . .
C25 C21 C20 134.2(12) . .
C27 C26 C20 131.8(12) . .
N30 C26 C20 120.9(13) . .
N30 C26 C27 107.1(10) . .
C28 C27 C26 109.6(9) . .
C27 C28 C29 109.8(8) . .
C28 C29 C31 130.0(14) . .
N30 C29 C28 106.7(9) . .
N30 C29 C31 123.3(13) . .
C29 N30 C26 106.9(11) . .
C29 C31 C32 115.1(10) . .
C33 C32 C31 119.0(8) . .
C37 C32 C31 120.7(9) . .
C37 C32 C33 120.3(8) . .
C34 C33 C32 120.0(7) . .
C35 C34 C33 120.3(8) . .
C34 C35 C36 119.3(9) . .
C34 C35 C38 122.3(8) . .
C35 C35 C34 57.2(5) 21 .
C35 C35 C36 146.9(3) 21 .
C35 C35 C38 75.5(5) 21 .
C36 C35 C38 118.3(7) . .
C37 C36 C35 120.5(8) . .
C32 C37 C36 119.5(9) . .
C35 C38 C35 29.0(10) 21 .
O39 C38 C35 112.8(11) 12 .
O39 C38 C35 112.8(11) . 21
O39 C38 C35 126.1(11) . .
O39 C38 C35 126.1(11) 12 21
O39 C38 O39 119(2) . 12
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hf1 O2 2.142(7) .
Hf1 O3 2.135(19) .
Hf1 O4 2.36(2) .
Hf1 O11 2.181(7) .
O11 C12 1.344(13) .
C12 O13 1.338(12) .
C12 C14 1.57(2) .
C17 C16 1.393(9) .
C17 C18 1.386(9) .
C17 C20 1.550(18) .
C16 C15 1.392(9) .
C15 C14 1.389(9) .
C14 C19 1.394(9) .
C19 C18 1.394(9) .
C20 C21 1.425(15) .
C20 C26 1.421(15) .
N22 C23 1.381(15) .
N22 C21 1.389(13) .
C23 C24 1.401(14) .
C24 C25 1.291(18) .
C25 C21 1.400(12) .
C26 C27 1.396(14) .
C26 N30 1.388(14) .
C27 C28 1.271(17) .
C28 C29 1.410(14) .
C29 N30 1.372(14) .
C29 C31 1.420(14) .
C31 C32 1.54(2) .
C32 C33 1.397(9) .
C32 C37 1.384(9) .
C33 C34 1.392(9) .
C34 C35 1.384(9) .
C35 C35 0.78(3) 21
C35 C36 1.407(9) .
C35 C38 1.55(2) .
C36 C37 1.395(10) .
C38 O39 1.229(14) .
C38 O39 1.229(14) 12
