#------------------------------------------------------------------------------
#$Date: 2019-10-29 01:28:21 +0200 (Tue, 29 Oct 2019) $
#$Revision: 220315 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/29/4002938.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_4002938
loop_
_publ_author_name
'Pang, Jiandong'
'Wu, Mingyan'
'Qin, Jun-Sheng'
'Liu, Caiping'
'Lollar, Christina T.'
'Yuan, Daqiang'
'Hong, Maochun'
'Zhou, Hong-Cai'
_publ_section_title
;
 Solvent-Assisted, Thermally Triggered Structural Transformation in
 Flexible Mesoporous Metal--Organic Frameworks
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.9b02582
_journal_year                    2019
_chemical_formula_sum            'C53 H32.67 Fe2 O10.67'
_chemical_formula_weight         951.82
_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_Hall           '-P 6 2c'
_space_group_name_H-M_alt        'P 6/m c c'
_symmetry_space_group_name_Hall  '-P 6 2c'
_symmetry_space_group_name_H-M   'P 6/m c c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   31.4730(7)
_cell_length_b                   31.473
_cell_length_c                   33.1372(10)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      43.6998
_cell_measurement_theta_min      2.6669
_cell_volume                     28426.5(11)
_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, 2014)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(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  0.0000
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            3676
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        43.752
_diffrn_reflns_theta_max         43.752
_diffrn_reflns_theta_min         2.667
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_T_max  0.7486
_exptl_absorpt_correction_T_min  0.3017
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Dark-red
_exptl_crystal_density_diffrn    0.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod-like
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         3676
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0521
_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)+(0.1010P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2896
_reflns_number_total             3676
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm9b02582_si_003.cif
_cod_data_source_block           PCN-168-200K
_cod_original_cell_volume        28426.4(15)
_cod_database_code               4002938
_shelx_shelxl_version_number     2014/7
_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+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-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-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'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
Fe1 Fe 0.28426(2) 0.59861(2) 0.0000 0.0158(3) Uani 1 2 d S T P
O1 O 0.39506(8) 0.63786(9) 0.04313(6) 0.0328(7) Uani 1 1 d . . .
O2 O 0.31666(9) 0.57988(8) 0.04321(7) 0.0372(7) Uani 1 1 d . . .
O3 O 0.3333 0.6667 0.0000 0.0152(12) Uani 1 6 d S T P
O4 O 0.23220(10) 0.52593(10) 0.0000 0.0386(9) Uani 1 2 d S T P
C1 C 0.35999(15) 0.59844(13) 0.05589(11) 0.0194(9) Uani 1 1 d . . .
C2 C 0.37005(14) 0.57249(13) 0.08748(10) 0.0192(9) Uani 1 1 d . . .
C3 C 0.33406(17) 0.53187(19) 0.10463(14) 0.0750(14) Uani 1 1 d . . .
H3 H 0.3011 0.5208 0.0969 0.090 Uiso 1 1 calc R U .
C4 C 0.34351(18) 0.50484(16) 0.13400(14) 0.0880(15) Uani 1 1 d . . .
H4 H 0.3169 0.4760 0.1452 0.106 Uiso 1 1 calc R U .
C5 C 0.39034(14) 0.51953(14) 0.14660(10) 0.0285(9) Uani 1 1 d . . .
C6 C 0.42586(16) 0.56098(18) 0.12976(15) 0.0717(13) Uani 1 1 d . . .
H6 H 0.4590 0.5734 0.1379 0.086 Uiso 1 1 calc R U .
C7 C 0.41492(19) 0.58622(15) 0.10040(14) 0.0714(13) Uani 1 1 d . . .
H7 H 0.4414 0.6150 0.0891 0.086 Uiso 1 1 calc R U .
C8 C 0.40004(12) 0.49131(13) 0.17736(10) 0.0286(9) Uani 1 1 d . . .
C9 C 0.36480(13) 0.44413(15) 0.18651(11) 0.0474(11) Uani 1 1 d . . .
H9 H 0.3341 0.4297 0.1730 0.057 Uiso 1 1 calc R U .
C10 C 0.37332(14) 0.41702(13) 0.21513(12) 0.0521(11) Uani 1 1 d . . .
H10 H 0.3485 0.3845 0.2214 0.062 Uiso 1 1 calc R U .
C11 C 0.41929(13) 0.43830(12) 0.23494(9) 0.0305(9) Uani 1 1 d . . .
C12 C 0.45433(10) 0.48525(11) 0.22546(9) 0.0191(8) Uani 1 1 d . . .
C13 C 0.44542(11) 0.51166(11) 0.19698(10) 0.0211(8) Uani 1 1 d . U .
H13 H 0.4704 0.5441 0.1906 0.025 Uiso 1 1 calc R U .
C14 C 0.5000 0.5000 0.2500 0.0136(15) Uani 1 4 d S T 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'
Fe Fe -1.1336 3.1974 '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 Fe1 O2 94.84(7) . .
O3 Fe1 O2 94.84(7) . 16
O2 Fe1 O2 90.89(13) . 16
O3 Fe1 O1 95.13(7) . 14_565
O2 Fe1 O1 170.03(9) . 14_565
O2 Fe1 O1 88.41(9) 16 14_565
O3 Fe1 O1 95.13(7) . 5_565
O2 Fe1 O1 88.42(9) . 5_565
O2 Fe1 O1 170.03(9) 16 5_565
O1 Fe1 O1 90.55(12) 14_565 5_565
O3 Fe1 O4 179.72(9) . .
O2 Fe1 O4 84.96(9) . .
O2 Fe1 O4 84.96(9) 16 .
O1 Fe1 O4 85.07(9) 14_565 .
O1 Fe1 O4 85.07(9) 5_565 .
C1 O1 Fe1 133.6(2) . 3_665
C1 O2 Fe1 133.9(2) . .
Fe1 O3 Fe1 119.998(1) 14_565 .
Fe1 O3 Fe1 119.998(1) 14_565 3_665
Fe1 O3 Fe1 120.003(1) . 3_665
O1 C1 O2 124.2(3) . .
O1 C1 C2 117.9(3) . .
O2 C1 C2 118.0(3) . .
C7 C2 C3 115.4(3) . .
C7 C2 C1 123.0(4) . .
C3 C2 C1 121.5(4) . .
C2 C3 C4 122.2(4) . .
C5 C4 C3 121.3(4) . .
C6 C5 C4 115.7(3) . .
C6 C5 C8 123.2(4) . .
C4 C5 C8 121.1(4) . .
C5 C6 C7 121.1(4) . .
C2 C7 C6 124.3(4) . .
C9 C8 C13 118.7(3) . .
C9 C8 C5 120.3(3) . .
C13 C8 C5 121.0(3) . .
C8 C9 C10 121.1(3) . .
C9 C10 C11 119.5(3) . .
C12 C11 C10 119.1(3) . .
C12 C11 C11 109.29(19) . 9
C10 C11 C11 131.6(2) . 9
C11 C12 C13 120.8(3) . .
C11 C12 C14 109.8(3) . .
C13 C12 C14 129.4(3) . .
C12 C13 C8 120.8(3) . .
C12 C14 C12 101.9(3) 10_665 4_665
C12 C14 C12 114.8(2) 10_665 9
C12 C14 C12 112.1(2) 4_665 9
C12 C14 C12 112.1(2) 10_665 .
C12 C14 C12 114.8(2) 4_665 .
C12 C14 C12 101.9(3) 9 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O3 1.9145(6) .
Fe1 O2 2.010(2) .
Fe1 O2 2.010(2) 16
Fe1 O1 2.011(2) 14_565
Fe1 O1 2.011(2) 5_565
Fe1 O4 2.042(3) .
O1 C1 1.252(3) .
O1 Fe1 2.011(2) 3_665
O2 C1 1.257(4) .
O3 Fe1 1.9147(6) 14_565
O3 Fe1 1.9145(6) 3_665
C1 C2 1.457(4) .
C2 C7 1.325(5) .
C2 C3 1.339(5) .
C3 C4 1.419(5) .
C4 C5 1.371(5) .
C5 C6 1.343(5) .
C5 C8 1.480(4) .
C6 C7 1.404(5) .
C8 C9 1.371(4) .
C8 C13 1.399(4) .
C9 C10 1.389(4) .
C10 C11 1.415(4) .
C11 C12 1.367(4) .
C11 C11 1.439(6) 9
C12 C13 1.376(4) .
C12 C14 1.508(3) .
C14 C12 1.508(3) 10_665
C14 C12 1.508(3) 4_665
C14 C12 1.508(3) 9
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 -0.003 -0.005 -0.004 23995 10133 ' '
