#------------------------------------------------------------------------------
#$Date: 2019-11-03 12:12:47 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221360 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/82/4128231.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_4128231
loop_
_publ_author_name
'Wei, Yong-Sheng'
'Zhang, Mei'
'Kitta, Mitsunori'
'Liu, Zheng'
'Horike, Satoshi'
'Xu, Qiang'
_publ_section_title
;
 A Single-Crystal Open-Capsule Metal-Organic Framework.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7906
_journal_page_last               7916
_journal_paper_doi               10.1021/jacs.9b02417
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.5(C88 H40 Fe6 N14 O26)'
_chemical_formula_sum            'C44 H20 Fe3 N7 O13'
_chemical_formula_weight         1022.22
_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'
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.8853(4)
_cell_length_b                   16.8853(4)
_cell_length_c                   14.8612(5)
_cell_measurement_reflns_used    5842
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.9790
_cell_measurement_theta_min      2.3850
_cell_volume                     3669.46(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13573
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_min         1.954
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.925
_exptl_crystal_description       plate
_exptl_crystal_F_000             1030
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1387
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0416
_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)+(0.0930P)²+1.3982P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1318
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1232
_reflns_number_total             1387
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b02417_si_003.cif
_cod_data_source_block           Fe-MIL-88B-tpy
_cod_original_cell_volume        3669.5(2)
_cod_database_code               4128231
_shelxl_version_number           2013-2
_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, All N(H,H,H) groups
2. Shared sites
{N3, C8}
3. Restrained distances
 N1-C3
 1.5 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(N3) = Uanis(C8)
5. Others
 Fixed Sof: N1(0.25) H1A(0.16667) H1B(0.16667) H1C(0.16667) C8(0.16667)
 H8(0.16667) N3(0.08333)
6.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8)
6.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_platon_squeeze_void_probe_radius 1.20
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
Fe1 Fe 0.73150(2) 0.46300(3) 0.2500 0.0227(2) Uani 1 4 d S T P . .
O1 O 0.6667 0.3333 0.2500 0.0183(8) Uani 1 12 d S T P . .
O2 O 0.65389(12) 0.47678(11) 0.34577(13) 0.0577(6) Uani 1 1 d . . . . .
N1 N 0.3977(10) 0.3095(6) 0.4708(11) 0.116(5) Uani 0.25 1 d D U . . .
H1A H 0.3483 0.2887 0.5077 0.140 Uiso 0.1667 1 calc GR . . . .
H1B H 0.4355 0.2895 0.4912 0.140 Uiso 0.1667 1 calc GR . . . .
H1C H 0.3788 0.2881 0.4141 0.140 Uiso 0.1667 1 calc GR . . . .
N2 N 0.80643(11) 0.6129(2) 0.2500 0.0364(8) Uani 1 4 d S T P . .
C1 C 0.57402(11) 0.42598(11) 0.3724(2) 0.0418(7) Uani 1 2 d S T P . .
C2 C 0.53633(13) 0.46367(13) 0.4391(3) 0.0548(10) Uani 1 2 d S T P . .
C3 C 0.4479(2) 0.4115(2) 0.4698(3) 0.1027(16) Uani 1 1 d D . . . .
C4 C 0.8974(3) 0.6617(3) 0.2500 0.0694(13) Uani 1 2 d S T P . .
H4 H 0.9303 0.6295 0.2500 0.083 Uiso 1 2 calc RS T P . .
C5 C 0.9469(2) 0.7560(3) 0.2500 0.0766(15) Uani 1 2 d S T P . .
H5 H 1.0119 0.7868 0.2500 0.092 Uiso 1 2 calc RS T P . .
C6 C 0.90253(15) 0.8051(3) 0.2500 0.0463(11) Uani 1 4 d S T P A .
C7 C 0.95340(16) 0.9068(3) 0.2500 0.0465(11) Uani 1 4 d S T P . .
C8 C 0.9059(3) 0.95295(14) 0.2500 0.0473(11) Uani 0.6667 4 d S T P A 1
H8 H 0.8409 0.9205 0.2500 0.057 Uiso 0.6667 4 calc RS T P A 1
N3 N 0.9059(3) 0.95295(14) 0.2500 0.0473(11) Uani 0.3333 4 d S T P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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 Fe1 O2 95.71(5) . 16_556
O1 Fe1 O2 95.71(5) . 20_655
O1 Fe1 O2 95.71(5) . .
O1 Fe1 O2 95.71(5) . 11_655
O1 Fe1 N2 180.0 . .
O2 Fe1 O2 168.58(10) 16_556 20_655
O2 Fe1 O2 89.30(12) 16_556 .
O2 Fe1 O2 89.29(12) 20_655 11_655
O2 Fe1 O2 89.57(12) . 20_655
O2 Fe1 O2 89.57(12) 16_556 11_655
O2 Fe1 O2 168.58(10) . 11_655
O2 Fe1 N2 84.29(5) 16_556 .
O2 Fe1 N2 84.29(5) 11_655 .
O2 Fe1 N2 84.29(5) 20_655 .
O2 Fe1 N2 84.29(5) . .
Fe1 O1 Fe1 120.0 3_665 2_655
Fe1 O1 Fe1 120.0 2_655 .
Fe1 O1 Fe1 120.0 3_665 .
C1 O2 Fe1 133.11(16) . .
H1A N1 H1B 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
C3 N1 H1A 109.5 . .
C3 N1 H1B 109.5 . .
C3 N1 H1C 109.5 . .
C4 N2 Fe1 122.39(19) 20_655 .
C4 N2 Fe1 122.39(19) . .
C4 N2 C4 115.2(4) . 20_655
O2 C1 O2 124.5(3) . 19_665
O2 C1 C2 117.76(13) 19_665 .
O2 C1 C2 117.76(13) . .
C3 C2 C1 120.50(16) . .
C3 C2 C1 120.50(16) 19_665 .
C3 C2 C3 119.0(3) 19_665 .
C2 C3 N1 123.3(6) . .
C2 C3 C3 120.51(16) . 7_556
C3 C3 N1 112.4(5) 7_556 .
N2 C4 H4 118.0 . .
N2 C4 C5 124.0(3) . .
C5 C4 H4 118.0 . .
C4 C5 H5 120.0 . .
C6 C5 C4 120.0(3) . .
C6 C5 H5 120.0 . .
C5 C6 C5 116.7(4) . 20_655
C5 C6 C7 121.7(2) . .
C5 C6 C7 121.7(2) 20_655 .
C8 C7 C6 119.5(2) . .
C8 C7 C6 119.5(2) 2_765 .
C8 C7 C8 120.9(4) . 2_765
N3 C7 C6 119.5(2) 2_765 .
C7 C8 C7 119.1(4) . 3_675
C7 C8 H8 120.5 . .
C7 C8 H8 120.5 3_675 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 1.8961(5) .
Fe1 O2 2.0254(15) .
Fe1 O2 2.0254(15) 11_655
Fe1 O2 2.0253(15) 16_556
Fe1 O2 2.0254(15) 20_655
Fe1 N2 2.192(3) .
O1 Fe1 1.8960(5) 3_665
O1 Fe1 1.8960(5) 2_655
O2 C1 1.247(2) .
N1 H1A 0.9100 .
N1 H1B 0.9100 .
N1 H1C 0.9100 .
N1 C3 1.492(8) .
N2 C4 1.332(4) 20_655
N2 C4 1.332(4) .
C1 O2 1.247(2) 19_665
C1 C2 1.483(4) .
C2 C3 1.378(3) 19_665
C2 C3 1.378(3) .
C3 C3 1.393(5) 7_556
C4 H4 0.9500 .
C4 C5 1.380(5) .
C5 H5 0.9500 .
C5 C6 1.368(4) .
C6 C5 1.368(4) 20_655
C6 C7 1.488(6) .
C7 C8 1.370(3) 2_765
C7 C8 1.370(3) .
C7 N3 1.370(3) 2_765
C8 C7 1.369(3) 3_675
C8 H8 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Fe1 O2 C1 O2 5.1(6) . 19_665
Fe1 O2 C1 C2 -173.8(3) . .
Fe1 N2 C4 C5 180.0 . .
O2 Fe1 O1 Fe1 -135.07(6) . 3_665
O2 Fe1 O1 Fe1 -44.93(6) 20_655 3_665
O2 Fe1 O1 Fe1 135.07(6) 20_655 2_655
O2 Fe1 O1 Fe1 -135.07(6) 11_655 2_655
O2 Fe1 O1 Fe1 44.93(6) 11_655 3_665
O2 Fe1 O1 Fe1 -44.93(6) 16_556 2_655
O2 Fe1 O1 Fe1 135.07(6) 16_556 3_665
O2 Fe1 O1 Fe1 44.93(6) . 2_655
O2 C1 C2 C3 -178.7(4) 19_665 19_665
O2 C1 C2 C3 0.3(6) . 19_665
O2 C1 C2 C3 178.7(4) . .
O2 C1 C2 C3 -0.3(6) 19_665 .
N2 C4 C5 C6 0.0 . .
C1 C2 C3 N1 25.4(11) . .
C1 C2 C3 C3 -177.9(6) . 7_556
C3 C2 C3 N1 -156.1(9) 19_665 .
C3 C2 C3 C3 0.6(11) 19_665 7_556
C4 N2 C4 C5 0.0 20_655 .
C4 C5 C6 C5 0.0 . 20_655
C4 C5 C6 C7 180.0 . .
C5 C6 C7 C8 180.0 20_655 2_765
C5 C6 C7 C8 180.0 . .
C5 C6 C7 C8 0.0 . 2_765
C5 C6 C7 C8 0.0 20_655 .
C5 C6 C7 N3 180.0 20_655 2_765
C5 C6 C7 N3 0.0 . 2_765
C6 C7 C8 C7 180.0 . 3_675
C8 C7 C8 C7 0.0 2_765 3_675
N3 C7 C8 C7 0.0 2_765 3_675
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.010 -0.009 -0.008 1672 374 ' '
