#------------------------------------------------------------------------------
#$Date: 2019-10-29 01:28:21 +0200 (Tue, 29 Oct 2019) $
#$Revision: 220315 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/29/4002939.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_4002939
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                   31.3244(10)
_cell_length_b                   31.324
_cell_length_c                   33.2713(13)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      46.3049
_cell_measurement_theta_min      3.1162
_cell_volume                     28272.3(14)
_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      250(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4208
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        46.412
_diffrn_reflns_theta_max         46.412
_diffrn_reflns_theta_min         2.656
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  0.7491
_exptl_absorpt_correction_T_min  0.3386
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Dark-red
_exptl_crystal_density_diffrn    0.335
_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         0.351
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.028
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.524
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         4208
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.528
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0431
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3369
_reflns_number_total             4208
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm9b02582_si_003.cif
_cod_data_source_block           PCN-168-250K
_cod_original_cell_volume        28273(2)
_cod_database_code               4002939
_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 0.40166(2) 0.71604(2) 0.0000 0.0268(2) Uani 1 2 d S T P
C14 C 0.5000 1.0000 -0.2500 0.0299(10) Uani 1 4 d S T P
O4 O 0.47462(7) 0.76846(8) 0.0000 0.0602(6) Uani 1 2 d S T P
O3 O 0.3333 0.6667 0.0000 0.0262(7) Uani 1 6 d S T P
O2 O 0.39490(6) 0.75740(5) -0.04287(4) 0.0496(5) Uani 1 1 d . . .
C10 C 0.45402(7) 0.96940(7) -0.22502(5) 0.0318(5) Uani 1 1 d . U .
C8 C 0.39902(8) 0.90868(8) -0.17764(6) 0.0483(7) Uani 1 1 d . . .
C2 C 0.36948(8) 0.79804(8) -0.08781(5) 0.0367(6) Uani 1 1 d . . .
C5 C 0.39000(9) 0.87052(8) -0.14642(6) 0.0502(7) Uani 1 1 d . . .
O1 O 0.31650(5) 0.73668(6) -0.04328(4) 0.0539(5) Uani 1 1 d . . .
C1 C 0.35971(9) 0.76161(7) -0.05578(6) 0.0304(5) Uani 1 1 d . U .
C11 C 0.41798(9) 0.98067(8) -0.23465(6) 0.0485(6) Uani 1 1 d . . .
C9 C 0.44528(7) 0.93349(7) -0.19665(5) 0.0367(6) Uani 1 1 d . U .
H9 H 0.4699 0.9259 -0.1902 0.044 Uiso 1 1 calc R U .
C13 C 0.36409(10) 0.92145(10) -0.18690(7) 0.0738(8) Uani 1 1 d . . .
H13 H 0.3336 0.9058 -0.1735 0.089 Uiso 1 1 calc R U .
C3 C 0.41660(11) 0.83005(11) -0.09975(8) 0.0947(10) Uani 1 1 d . . .
H3 H 0.4428 0.8277 -0.0883 0.114 Uiso 1 1 calc R U .
C4 C 0.42663(10) 0.86602(11) -0.12853(9) 0.0990(11) Uani 1 1 d . . .
H4 H 0.4595 0.8878 -0.1358 0.119 Uiso 1 1 calc R U .
C7 C 0.33266(10) 0.80232(11) -0.10514(8) 0.0970(11) Uani 1 1 d . . .
H7 H 0.2999 0.7808 -0.0973 0.116 Uiso 1 1 calc R U .
C12 C 0.37280(9) 0.95666(10) -0.21540(7) 0.0748(8) Uani 1 1 d . . .
H12 H 0.3482 0.9644 -0.2218 0.090 Uiso 1 1 calc R U .
C6 C 0.34218(10) 0.83771(11) -0.13418(8) 0.1040(12) Uani 1 1 d . . .
H6 H 0.3158 0.8395 -0.1458 0.125 Uiso 1 1 calc R U .
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 94.89(4) . .
O3 Fe1 O2 94.89(5) . 16
O2 Fe1 O2 90.51(9) . 16
O3 Fe1 O1 94.59(4) . 5_565
O2 Fe1 O1 88.20(6) . 5_565
O2 Fe1 O1 170.50(6) 16 5_565
O3 Fe1 O1 94.59(4) . 14_565
O2 Fe1 O1 170.50(6) . 14_565
O2 Fe1 O1 88.20(6) 16 14_565
O1 Fe1 O1 91.52(10) 5_565 14_565
O3 Fe1 O4 179.75(6) . .
O2 Fe1 O4 85.28(6) . .
O2 Fe1 O4 85.28(6) 16 .
O1 Fe1 O4 85.24(6) 5_565 .
O1 Fe1 O4 85.24(6) 14_565 .
C10 C14 C10 113.59(13) 11_554 7_674
C10 C14 C10 113.69(14) 11_554 .
C10 C14 C10 101.42(15) 7_674 .
C10 C14 C10 101.42(15) 11_554 4_675
C10 C14 C10 113.69(14) 7_674 4_675
C10 C14 C10 113.59(13) . 4_675
Fe1 O3 Fe1 120.002(3) 3_665 .
Fe1 O3 Fe1 120.000(1) 3_665 14_565
Fe1 O3 Fe1 119.998(1) . 14_565
C1 O2 Fe1 134.05(13) . .
C11 C10 C9 120.75(18) . .
C11 C10 C14 110.54(15) . .
C9 C10 C14 128.69(17) . .
C13 C8 C9 119.2(2) . .
C13 C8 C5 121.8(2) . .
C9 C8 C5 118.9(2) . .
C7 C2 C3 117.7(2) . .
C7 C2 C1 121.7(2) . .
C3 C2 C1 120.5(2) . .
C4 C5 C6 116.7(2) . .
C4 C5 C8 123.5(2) . .
C6 C5 C8 119.8(2) . .
C1 O1 Fe1 134.13(13) . 3_665
O1 C1 O2 123.86(19) . .
O1 C1 C2 117.7(2) . .
O2 C1 C2 118.4(2) . .
C10 C11 C12 119.94(18) . .
C10 C11 C11 108.74(11) . 7_674
C12 C11 C11 131.32(13) . 7_674
C10 C9 C8 119.04(19) . .
C12 C13 C8 121.4(2) . .
C2 C3 C4 121.3(2) . .
C5 C4 C3 121.7(2) . .
C2 C7 C6 121.5(2) . .
C13 C12 C11 119.6(2) . .
C7 C6 C5 121.2(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O3 1.9138(4) .
Fe1 O2 2.0080(14) .
Fe1 O2 2.0081(14) 16
Fe1 O1 2.0100(14) 5_565
Fe1 O1 2.0100(14) 14_565
Fe1 O4 2.041(2) .
C14 C10 1.5177(19) 11_554
C14 C10 1.5177(19) 7_674
C14 C10 1.5178(19) .
C14 C10 1.5178(19) 4_675
O3 Fe1 1.9139(4) 3_665
O3 Fe1 1.9139(4) 14_565
O2 C1 1.250(2) .
C10 C11 1.378(3) .
C10 C9 1.387(2) .
C8 C13 1.375(3) .
C8 C9 1.406(3) .
C8 C5 1.500(3) .
C2 C7 1.355(3) .
C2 C3 1.365(3) .
C2 C1 1.477(3) .
C5 C4 1.361(3) .
C5 C6 1.388(3) .
O1 C1 1.248(2) .
O1 Fe1 2.0100(14) 3_665
C11 C12 1.384(3) .
C11 C11 1.464(4) 7_674
C13 C12 1.374(3) .
C3 C4 1.390(3) .
C7 C6 1.386(3) .
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 23595 4103 ' '
