#------------------------------------------------------------------------------
#$Date: 2019-09-25 12:22:59 +0300 (Wed, 25 Sep 2019) $
#$Revision: 218826 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/42/7124223.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_7124223
loop_
_publ_author_name
'Drake, Hannah'
'Day, Gregory S.'
'Vali, Shaik Waseem'
'Xiao, Zhifeng'
'Banerjee, Sayan'
'Li, Jialuo'
'Joseph, Elizabeth'
'Kuszynski, Jason E.'
'Perry, Zachary'
'Kirchon, Angelo'
'Ozdemir, Osman'
'Lindahl, Paul'
'Zhou, Hong-Cai'
_publ_section_title
;
 The Thermally Induced Decarboxylation Mechanism of a Mixed-Oxidation
 State Carboxylate-Based Iron Metal-Organic Framework
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04555D
_journal_year                    2019
_chemical_formula_moiety         'C48 H29.639 Fe6 N6 O31.82'
_chemical_formula_sum            'C48 H29.64 Fe6 N6 O31.82'
_chemical_formula_weight         1534.64
_chemical_name_common            PCN-250
_chemical_name_systematic
'catena-[hexakis(m-5,5'-((E)-diazenediyl)bis(benzene-1,3-dicarboxylato))-tetrakis(m-oxo)-dodeca-aqua-dodeca-iron unknown solvate]'
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_Hall           'P -4n 2 3'
_space_group_name_H-M_alt        'P -4 3 n'
_symmetry_space_group_name_Hall  'P -4n 2 3'
_symmetry_space_group_name_H-M   'P -4 3 n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-09-08
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.08.16 svn.r3652 for OlexSys, GUI svn.r5895)
;
_audit_update_record
;
2019-09-12 deposited with the CCDC.    2019-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9389(7)
_cell_length_b                   21.9389(7)
_cell_length_c                   21.9389(7)
_cell_measurement_reflns_used    9472
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      28
_cell_measurement_theta_min      0.5
_cell_volume                     10559.5(6)
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.1112
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            104626
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         28.268
_diffrn_reflns_theta_min         1.346
_diffrn_source                   'Advanced Light Source, Beamline 12.2.1'
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.965
_exptl_crystal_description       block
_exptl_crystal_F_000             3081
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.007(19)
_refine_ls_extinction_coef       0.0044(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         4054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0263
_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)+(0.0455P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.851
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3680
_reflns_number_total             4054
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc04555d2.cif
_cod_data_source_block           pcn-250_beforeactivation
_cod_original_cell_volume        10559.5(10)
_cod_database_code               7124223
_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.
;
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.914
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.99276
 0.00724
2. Others
 Sof(O6)=Sof(H6A)=Sof(H6B)=FVAR(1)
3.a Rotating group:
 O6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C8(H8)
;
_platon_squeeze_special_details
;
A solvent mask was calculated and 993 electrons were
found in a volume of 6055Å^3 in 1 void per unit cell.
This is consistent with the presence of 
6[C3H7NO(N,N-dimethylformamide] per Formula Unit 
which account for 960 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_original_sample_id PCN-250_BeforeActivation
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y+1/2, -x+1/2, -z+1/2'
'-x, -y, z'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, z+1/2, -y+1/2'
'x, -y, -z'
'-x+1/2, -z+1/2, y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-x, y, -z'
'z+1/2, -y+1/2, -x+1/2'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, y+1/2, x+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 0.73995(2) 0.31990(2) 0.19632(2) 0.01694(12) Uani 1 1 d . . .
O1 O 0.74063(8) 0.25937(8) 0.25937(8) 0.0152(5) Uani 1 3 d S T P
O4 O 1.10775(8) 0.25549(10) 0.24900(9) 0.0298(5) Uani 1 1 d . . .
O5 O 1.14940(8) 0.29618(11) 0.16591(9) 0.0326(5) Uani 1 1 d . . .
O3 O 0.87494(9) 0.27366(10) 0.26235(9) 0.0307(5) Uani 1 1 d . . .
O2 O 0.82956(8) 0.31301(11) 0.18083(10) 0.0342(5) Uani 1 1 d . . .
C1 C 0.87515(11) 0.29305(13) 0.20907(13) 0.0228(5) Uani 1 1 d . . .
C2 C 1.10522(11) 0.27917(12) 0.19751(13) 0.0222(5) Uani 1 1 d . . .
C3 C 1.04322(12) 0.28752(15) 0.16891(13) 0.0283(6) Uani 1 1 d . . .
C4 C 1.04051(13) 0.2963(2) 0.10686(14) 0.0452(9) Uani 1 1 d . . .
H4 H 1.076878 0.297894 0.083413 0.054 Uiso 1 1 calc R U .
C6 C 0.93141(13) 0.3034(2) 0.11272(15) 0.0481(10) Uani 1 1 d . . .
H6 H 0.893258 0.310081 0.093371 0.058 Uiso 1 1 calc R U .
C8 C 0.99015(12) 0.28463(14) 0.20294(13) 0.0267(6) Uani 1 1 d . . .
H8 H 0.992064 0.276205 0.245374 0.032 Uiso 1 1 calc R U .
C7 C 0.93393(12) 0.29410(15) 0.17492(13) 0.0290(6) Uani 1 1 d . . .
C5 C 0.98406(14) 0.3029(2) 0.07879(15) 0.0565(13) Uani 1 1 d . . .
O6 O 0.73803(12) 0.38496(10) 0.12948(11) 0.0375(7) Uani 0.970(6) 1 d . . P
H6A H 0.758949 0.424265 0.128673 0.056 Uiso 0.970(6) 1 d R U P
H6B H 0.716360 0.384660 0.090498 0.056 Uiso 0.970(6) 1 d R U P
N1 N 0.97671(12) 0.3071(2) 0.01396(13) 0.0719(13) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0037 0.0017 '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 0.3621 0.8896 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0070 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0123 0.0065 '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 O4 96.57(8) . 2_565
O1 Fe1 O5 93.19(9) . 21_455
O1 Fe1 O3 97.23(8) . 15_656
O1 Fe1 O2 93.59(9) . .
O1 Fe1 O6 179.16(12) . .
O4 Fe1 O3 166.13(7) 2_565 15_656
O4 Fe1 O6 83.17(9) 2_565 .
O5 Fe1 O4 89.80(9) 21_455 2_565
O5 Fe1 O3 90.79(9) 21_455 15_656
O5 Fe1 O6 86.02(10) 21_455 .
O3 Fe1 O6 83.05(9) 15_656 .
O2 Fe1 O4 89.69(10) . 2_565
O2 Fe1 O5 173.22(8) . 21_455
O2 Fe1 O3 88.10(9) . 15_656
O2 Fe1 O6 87.21(9) . .
Fe1 O1 Fe1 119.985(4) . 15_656
Fe1 O1 Fe1 119.985(4) 16_665 15_656
Fe1 O1 Fe1 119.985(4) . 16_665
C2 O4 Fe1 130.17(17) . 4_645
C2 O5 Fe1 134.67(18) . 21
C1 O3 Fe1 129.58(17) . 16_665
C1 O2 Fe1 136.50(18) . .
O3 C1 O2 125.5(2) . .
O3 C1 C7 118.7(2) . .
O2 C1 C7 115.8(3) . .
O4 C2 O5 126.4(2) . .
O4 C2 C3 117.9(2) . .
O5 C2 C3 115.6(2) . .
C4 C3 C2 117.9(2) . .
C4 C3 C8 120.2(2) . .
C8 C3 C2 121.9(2) . .
C3 C4 C5 119.4(3) . .
C5 C6 C7 120.0(3) . .
C3 C8 C7 120.0(3) . .
C6 C7 C1 117.6(2) . .
C6 C7 C8 119.6(3) . .
C8 C7 C1 122.8(3) . .
C4 C5 N1 123.1(3) . .
C6 C5 C4 120.6(3) . .
C6 C5 N1 116.2(3) . .
N1 N1 C5 114.4(3) 9_755 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 1.9177(3) .
Fe1 O4 2.019(2) 2_565
Fe1 O5 2.0176(19) 21_455
Fe1 O3 2.031(2) 15_656
Fe1 O2 2.0007(18) .
Fe1 O6 2.0467(19) .
O4 C2 1.244(3) .
O5 C2 1.249(4) .
O3 C1 1.244(3) .
O2 C1 1.255(3) .
C1 C7 1.492(4) .
C2 C3 1.509(3) .
C3 C4 1.376(4) .
C3 C8 1.385(4) .
C4 C5 1.391(4) .
C6 C7 1.381(4) .
C6 C5 1.374(4) .
C8 C7 1.394(4) .
C5 N1 1.434(4) .
N1 N1 1.192(5) 9_755
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 -0.062 -0.046 -0.045 6055 993 '24 C3H7NO'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.99276
2 0.00724
