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#$Date: 2019-11-25 15:58:50 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241266 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/09/4130926.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_4130926
loop_
_publ_author_name
'Zhao, Xiang'
'Bu, Xianhui'
'Nguyen, Edward T.'
'Zhai, Quan-Guo'
'Mao, Chengyu'
'Feng, Pingyun'
_publ_section_title
;
 Multivariable Modular Design of Pore Space Partition.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15102
_journal_page_last               15105
_journal_paper_doi               10.1021/jacs.6b07901
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C30 H6 Cu3 Fe3 N9 O20'
_chemical_formula_sum            'C30 H6 Cu3 Fe3 N9 O20'
_chemical_formula_weight         1170.61
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.7672(7)
_cell_length_b                   15.7672(7)
_cell_length_c                   16.6814(8)
_cell_measurement_reflns_used    6088
_cell_measurement_temperature    174(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.44
_cell_volume                     3591.5(3)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      174(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART Apex diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22353
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.348
_diffrn_reflns_theta_min         1.927
_exptl_absorpt_coefficient_mu    1.514
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/3
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_description       block
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.086
_refine_diff_density_max         2.918
_refine_diff_density_min         -2.597
_refine_diff_density_rms         0.228
_refine_ls_extinction_coef       0.005(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   2.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         1708
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      3.233
_refine_ls_R_factor_all          0.1328
_refine_ls_R_factor_gt           0.1196
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3559
_refine_ls_wR_factor_ref         0.3647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1397
_reflns_number_total             1708
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b07901_si_002.cif
_cod_data_source_block           CPM-516
_cod_original_cell_volume        3591.5(4)
_cod_database_code               4130926
_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.
;
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
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
Fe1 Fe 0.74206(5) 0.48411(10) 0.7500 0.0196(6) Uani 1 4 d S T P
O1 O 0.6667 0.3333 0.7500 0.0101(17) Uani 1 12 d S T P
O2 O 0.8370(3) 0.4883(3) 0.6596(3) 0.0479(13) Uani 1 1 d . . .
C1 C 0.8633(6) 0.4316(3) 0.6333(4) 0.0350(17) Uani 1 2 d S T P
C3 C 0.9696(7) 0.5607(6) 0.5327(5) 0.069(3) Uani 1 1 d . . .
C2 C 0.9345(7) 0.4672(3) 0.5644(5) 0.043(2) Uani 1 2 d S T P
N2 N 0.9404(9) 0.7945(9) 0.7500 0.090(3) Uani 1 2 d S TU P
N1 N 0.8217(4) 0.6434(7) 0.7500 0.035(2) Uani 1 4 d S T P
C4 C 0.9090(13) 0.7002(8) 0.7500 0.108(6) Uani 1 2 d S T P
H4A H 0.9531 0.6774 0.7500 0.130 Uiso 1 2 calc R U P
Cu1 Cu 1.07467(12) 0.92533(12) 0.7500 0.1418(19) Uani 1 4 d S TU P
O3 O 1.0000 1.0000 0.7500 0.1382(13) Uani 1 12 d S TU P
O6 O 0.9340(11) 0.6201(11) 0.5604(9) 0.092(4) Uani 0.5 1 d . U P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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 91.55(12) . .
O1 Fe1 O2 91.55(12) . 20_655
O2 Fe1 O2 88.3(3) . 20_655
O1 Fe1 O2 91.55(12) . 11_656
O2 Fe1 O2 176.9(2) . 11_656
O2 Fe1 O2 91.6(3) 20_655 11_656
O1 Fe1 O2 91.55(12) . 16_557
O2 Fe1 O2 91.6(3) . 16_557
O2 Fe1 O2 176.9(2) 20_655 16_557
O2 Fe1 O2 88.3(3) 11_656 16_557
O1 Fe1 N1 180.0 . .
O2 Fe1 N1 88.45(12) . .
O2 Fe1 N1 88.45(12) 20_655 .
O2 Fe1 N1 88.45(12) 11_656 .
O2 Fe1 N1 88.45(12) 16_557 .
Fe1 O1 Fe1 120.000(1) . 3_665
Fe1 O1 Fe1 120.0 . 2_655
Fe1 O1 Fe1 120.0 3_665 2_655
C1 O2 Fe1 136.2(4) . .
O2 C1 O2 125.5(7) . 21
O2 C1 C2 117.3(3) . .
O2 C1 C2 117.3(3) 21 .
C3 C3 O6 118.4(7) 9_766 .
C3 C3 C2 120.7(3) 9_766 .
O6 C3 C2 120.4(8) . .
C3 C2 C3 118.4(7) 21 .
C3 C2 C1 120.8(3) 21 .
C3 C2 C1 120.8(3) . .
C4 N2 N2 100.9(11) . 20_655
C4 N2 Cu1 137.8(12) . .
N2 N2 Cu1 121.3(3) 20_655 .
C4 N1 C4 100.2(18) . 20_655
C4 N1 Fe1 129.9(9) . .
C4 N1 Fe1 129.9(9) 20_655 .
N1 C4 N2 119.0(18) . .
N1 C4 C4 39.9(9) . 20_655
N2 C4 C4 79.1(11) . 20_655
O3 Cu1 N2 88.7(3) . 19_775
O3 Cu1 N2 88.7(3) . .
N2 Cu1 N2 177.4(7) 19_775 .
Cu1 O3 Cu1 120.0 . 3_675
Cu1 O3 Cu1 120.000(1) . 2_765
Cu1 O3 Cu1 120.000(1) 3_675 2_765
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 2.0588(13) .
Fe1 O2 2.102(4) .
Fe1 O2 2.102(4) 20_655
Fe1 O2 2.102(4) 11_656
Fe1 O2 2.102(4) 16_557
Fe1 N1 2.175(10) .
O1 Fe1 2.0589(13) 3_665
O1 Fe1 2.0589(13) 2_655
O2 C1 1.238(5) .
C1 O2 1.238(5) 21
C1 C2 1.505(9) .
C3 C3 1.372(12) 9_766
C3 O6 1.389(15) .
C3 C2 1.394(7) .
C2 C3 1.394(7) 21
N2 C4 1.311(16) .
N2 N2 1.36(2) 20_655
N2 Cu1 2.091(12) .
N1 C4 1.210(17) .
N1 C4 1.210(16) 20_655
C4 C4 1.86(4) 20_655
Cu1 O3 2.039(3) .
Cu1 N2 2.091(12) 19_775
O3 Cu1 2.039(3) 3_675
O3 Cu1 2.039(3) 2_765
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 -0.022 -0.015 -0.002 1907 626 ' '
