#------------------------------------------------------------------------------
#$Date: 2019-10-29 01:28:21 +0200 (Tue, 29 Oct 2019) $
#$Revision: 220315 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/29/4002940.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_4002940
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                   31.2164(8)
_cell_length_b                   31.216
_cell_length_c                   33.3866(11)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      44.6962
_cell_measurement_theta_min      2.6469
_cell_volume                     28174.9(12)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            3876
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        44.848
_diffrn_reflns_theta_max         44.848
_diffrn_reflns_theta_min         2.647
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.364
_exptl_absorpt_correction_T_max  0.7488
_exptl_absorpt_correction_T_min  0.3279
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Dark-red
_exptl_crystal_density_diffrn    0.337
_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         0.295
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.026
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.470
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         3876
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.475
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0401
_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          0.1133
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2979
_reflns_number_total             3876
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm9b02582_si_003.cif
_cod_data_source_block           PCN-168-298K
_cod_original_cell_volume        28175.3(17)
_cod_database_code               4002940
_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 0.40190(2) 0.71637(2) 0.0000 0.0332(3) Uani 1 2 d S T P
C14 C 0.5000 1.0000 -0.2500 0.0361(10) Uani 1 4 d S T P
O4 O 0.47536(8) 0.76970(8) 0.0000 0.0726(7) Uani 1 2 d S T P
O3 O 0.3333 0.6667 0.0000 0.0272(7) Uani 1 6 d S T P
O1 O 0.39547(6) 0.75776(6) -0.04238(4) 0.0579(5) Uani 1 1 d . . .
C10 C 0.45404(8) 0.96966(8) -0.22512(5) 0.0395(6) Uani 1 1 d . U .
C5 C 0.38949(10) 0.87019(9) -0.14663(6) 0.0584(7) Uani 1 1 d . . .
C8 C 0.39928(10) 0.90825(9) -0.17771(6) 0.0587(7) Uani 1 1 d . . .
C2 C 0.36939(9) 0.79824(8) -0.08775(6) 0.0455(6) Uani 1 1 d . U .
C9 C 0.44531(8) 0.93355(8) -0.19680(6) 0.0455(6) Uani 1 1 d . U .
H9 H 0.4700 0.9262 -0.1906 0.055 Uiso 1 1 calc R U .
O2 O 0.31636(6) 0.73692(6) -0.04317(5) 0.0611(5) Uani 1 1 d . . .
C1 C 0.36024(10) 0.76159(8) -0.05558(6) 0.0366(6) Uani 1 1 d . U .
C11 C 0.41793(10) 0.98052(9) -0.23518(6) 0.0604(7) Uani 1 1 d . . .
C3 C 0.41646(12) 0.83100(12) -0.09900(8) 0.1086(11) Uani 1 1 d . . .
H3 H 0.4425 0.8293 -0.0872 0.130 Uiso 1 1 calc R U .
C13 C 0.36348(11) 0.92069(11) -0.18706(7) 0.0974(10) Uani 1 1 d . . .
H13 H 0.3331 0.9047 -0.1740 0.117 Uiso 1 1 calc R U .
C6 C 0.34166(11) 0.83721(12) -0.13470(8) 0.1099(12) Uani 1 1 d . . .
H6 H 0.3154 0.8388 -0.1463 0.132 Uiso 1 1 calc R U .
C7 C 0.33236(10) 0.80199(11) -0.10590(8) 0.1006(11) Uani 1 1 d . . .
H7 H 0.2998 0.7801 -0.0986 0.121 Uiso 1 1 calc R U .
C4 C 0.42653(10) 0.86686(11) -0.12768(9) 0.1046(11) Uani 1 1 d . . .
H4 H 0.4593 0.8892 -0.1342 0.126 Uiso 1 1 calc R U .
C12 C 0.37231(11) 0.95673(11) -0.21571(8) 0.0963(10) Uani 1 1 d . . .
H12 H 0.3481 0.9648 -0.2217 0.116 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 O1 95.24(5) . 16
O3 Fe1 O1 95.23(5) . .
O1 Fe1 O1 90.47(9) 16 .
O3 Fe1 O2 94.51(5) . 5_565
O1 Fe1 O2 170.25(6) 16 5_565
O1 Fe1 O2 88.24(7) . 5_565
O3 Fe1 O2 94.51(5) . 14_565
O1 Fe1 O2 88.24(7) 16 14_565
O1 Fe1 O2 170.25(6) . 14_565
O2 Fe1 O2 91.40(10) 5_565 14_565
O3 Fe1 O4 179.94(7) . .
O1 Fe1 O4 84.72(7) 16 .
O1 Fe1 O4 84.72(7) . .
O2 Fe1 O4 85.54(7) 5_565 .
O2 Fe1 O4 85.54(7) 14_565 .
C10 C14 C10 101.06(17) 4_675 11_554
C10 C14 C10 114.31(15) 4_675 7_674
C10 C14 C10 113.35(14) 11_554 7_674
C10 C14 C10 113.35(14) 4_675 .
C10 C14 C10 114.31(15) 11_554 .
C10 C14 C10 101.06(17) 7_674 .
Fe1 O3 Fe1 120.002(2) 3_665 .
Fe1 O3 Fe1 120.000(1) 3_665 14_565
Fe1 O3 Fe1 119.998(1) . 14_565
C1 O1 Fe1 133.95(14) . .
C11 C10 C9 121.00(19) . .
C11 C10 C14 110.51(17) . .
C9 C10 C14 128.43(19) . .
C4 C5 C6 116.7(2) . .
C4 C5 C8 122.6(2) . .
C6 C5 C8 120.6(2) . .
C13 C8 C9 118.8(2) . .
C13 C8 C5 120.4(2) . .
C9 C8 C5 120.7(2) . .
C7 C2 C3 117.3(2) . .
C7 C2 C1 122.9(2) . .
C3 C2 C1 119.8(2) . .
C10 C9 C8 119.8(2) . .
C1 O2 Fe1 133.32(14) . 3_665
O1 C1 O2 124.58(19) . .
O1 C1 C2 119.4(2) . .
O2 C1 C2 116.0(2) . .
C10 C11 C12 120.1(2) . .
C10 C11 C11 108.90(13) . 7_674
C12 C11 C11 130.95(14) . 7_674
C2 C3 C4 121.5(2) . .
C8 C13 C12 121.1(2) . .
C7 C6 C5 120.9(2) . .
C2 C7 C6 122.0(2) . .
C5 C4 C3 121.5(2) . .
C13 C12 C11 119.1(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O3 1.9150(4) .
Fe1 O1 1.9925(15) 16
Fe1 O1 1.9927(15) .
Fe1 O2 2.0138(16) 5_565
Fe1 O2 2.0138(16) 14_565
Fe1 O4 2.053(2) .
C14 C10 1.512(2) 4_675
C14 C10 1.512(2) 11_554
C14 C10 1.512(2) 7_674
C14 C10 1.512(2) .
O3 Fe1 1.9150(4) 3_665
O3 Fe1 1.9150(4) 14_565
O1 C1 1.245(2) .
C10 C11 1.371(3) .
C10 C9 1.390(3) .
C5 C4 1.367(3) .
C5 C6 1.382(3) .
C5 C8 1.490(3) .
C8 C13 1.389(3) .
C8 C9 1.400(3) .
C2 C7 1.361(3) .
C2 C3 1.358(3) .
C2 C1 1.489(3) .
O2 C1 1.260(2) .
O2 Fe1 2.0138(16) 3_665
C11 C12 1.394(3) .
C11 C11 1.445(4) 7_674
C3 C4 1.385(3) .
C13 C12 1.395(3) .
C6 C7 1.378(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 -0.006 -0.004 23517 4338 ' '
