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#$Date: 2019-11-25 16:36:45 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241337 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/10/4131029.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_4131029
loop_
_publ_author_name
'Liu, Qi'
'Cong, Hengjiang'
'Deng, Hexiang'
_publ_section_title
;
 Deciphering the Spatial Arrangement of Metals and Correlation to
 Reactivity in Multivariate Metal-Organic Frameworks.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13822
_journal_page_last               13825
_journal_paper_doi               10.1021/jacs.6b08724
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C144 H72 Co3 Fe3 N12 Ni3 O35'
_chemical_formula_weight         3050.60
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   31.4689(10)
_cell_length_b                   31.4689(10)
_cell_length_c                   16.8714(6)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      58.63
_cell_measurement_theta_min      2.81
_cell_volume                     14469.2(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Bruker Kappa APEX-Duo CCD'
_diffrn_radiation_monochromator  'Quazar multi-layer optics'
_diffrn_radiation_source         'Bruker I\muS'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.898
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            39191
_diffrn_reflns_point_group_measured_fraction_full 0.898
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        58.938
_diffrn_reflns_theta_max         58.938
_diffrn_reflns_theta_min         2.808
_exptl_absorpt_coefficient_mu    1.508
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.3609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/4 (Bruker,2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1543
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.624
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       0.0095(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   2.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         3571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.021
_refine_ls_R_factor_all          0.2209
_refine_ls_R_factor_gt           0.1806
_refine_ls_shift/su_max          0.000
_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          0.4663
_refine_ls_wR_factor_ref         0.4931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2496
_reflns_number_total             3571
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b08724_si_015.cif
_cod_data_source_block           I
_cod_original_cell_volume        14469.2(11)
_cod_database_code               4131029
_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'
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
Ni1 Ni 0.29639(4) 0.70361(4) 0.0000 0.0486(11) Uani 0.5 4 d S T P
Fe1 Fe 0.29639(4) 0.70361(4) 0.0000 0.0486(11) Uani 0.5 4 d S T P
Co1 Co 0.4924(8) 1.0000 0.5000 0.049(6) Uani 0.5 4 d S T P
O1 O 0.25848(18) 0.74152(18) 0.0000 0.090(4) Uani 1 4 d S T P
C1 C 0.4483(2) 0.8966(4) 0.4356(5) 0.088(4) Uani 1 2 d S T P
N1 N 0.4638(2) 0.9276(4) 0.5000 0.086(5) Uani 1 4 d S T P
O3 O 0.3333 0.6667 0.0000 0.025(3) Uani 1 12 d S T P
C3 C 0.4805(2) 0.9611(4) 0.3319(6) 0.094(4) Uani 1 2 d S T P
N2 N 0.5000 1.0000 0.3818(7) 0.079(4) Uani 1 4 d S T P
O2 O 0.3400(2) 0.74954(18) 0.0850(3) 0.0716(18) Uani 1 1 d . . .
C2 C 0.45546(19) 0.9109(4) 0.3571(6) 0.084(4) Uani 1 2 d S T P
C4 C 0.4240(2) 0.8479(4) 0.4593(7) 0.122(5) Uani 1 2 d S T P
H4 H 0.4103 0.8205 0.4264 0.146 Uiso 1 2 calc R U P
O4 O 0.4238(10) 1.0000 0.5000 0.115(9) Uani 0.5 4 d S T P
C5 C 0.4875(2) 0.9749(5) 0.2541(6) 0.121(6) Uani 1 2 d S T P
H5 H 0.4772 0.9544 0.2101 0.145 Uiso 1 2 calc R U P
C8 C 0.3712(4) 0.8188(3) 0.2048(5) 0.093(3) Uani 1 1 d . . .
H8 H 0.3396 0.8066 0.1851 0.111 Uiso 1 1 calc R U .
C7 C 0.3890(4) 0.8551(4) 0.2638(5) 0.100(3) Uani 1 1 d . . .
H7 H 0.3696 0.8675 0.2829 0.120 Uiso 1 1 calc R U .
C6 C 0.43616(19) 0.8723(4) 0.2934(6) 0.074(3) Uani 1 2 d S T P
C9 C 0.40047(19) 0.8009(4) 0.1757(5) 0.067(3) Uani 1 2 d S T P
C10 C 0.38156(17) 0.7631(3) 0.1087(5) 0.051(3) Uani 1 2 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'
N N 0.0311 0.0180 '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'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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
O2 Ni1 O2 176.3(3) . 10_665
O2 Ni1 O2 91.0(3) . 16
O2 Ni1 O2 88.9(3) 10_665 16
O2 Ni1 O2 88.9(3) . 19_665
O2 Ni1 O2 91.0(3) 10_665 19_665
O2 Ni1 O2 176.3(3) 16 19_665
O2 Ni1 O3 91.85(16) . .
O2 Ni1 O3 91.85(16) 10_665 .
O2 Ni1 O3 91.85(16) 16 .
O2 Ni1 O3 91.85(16) 19_665 .
O2 Ni1 O1 88.15(16) . .
O2 Ni1 O1 88.15(16) 10_665 .
O2 Ni1 O1 88.15(16) 16 .
O2 Ni1 O1 88.15(16) 19_665 .
O3 Ni1 O1 180.0 . .
Co1 Co1 N1 83.1(7) 13_676 13_676
Co1 Co1 N1 83.1(8) 13_676 .
N1 Co1 N1 166.1(15) 13_676 .
Co1 Co1 N2 83.1(7) 13_676 13_676
N1 Co1 N2 89.17(18) 13_676 13_676
N1 Co1 N2 89.17(18) . 13_676
Co1 Co1 N2 83.1(7) 13_676 .
N1 Co1 N2 89.17(18) 13_676 .
N1 Co1 N2 89.17(18) . .
N2 Co1 N2 166.3(15) 13_676 .
Co1 Co1 O4 180.000(18) 13_676 .
N1 Co1 O4 96.9(7) 13_676 .
N1 Co1 O4 96.9(7) . .
N2 Co1 O4 96.9(7) 13_676 .
N2 Co1 O4 96.9(7) . .
N1 C1 C2 125.7(10) . .
N1 C1 C4 111.1(10) . .
C2 C1 C4 123.2(10) . .
C1 N1 C1 104.3(12) . 16_556
C1 N1 Co1 127.5(6) . 13_676
C1 N1 Co1 127.5(6) 16_556 13_676
C1 N1 Co1 127.5(6) . .
C1 N1 Co1 127.5(6) 16_556 .
Ni1 O3 Ni1 120.0 . 3_565
Ni1 O3 Ni1 120.0 . 2_665
Fe1 O3 Ni1 120.0 3_565 2_665
Ni1 O3 Ni1 120.000(1) 3_565 2_665
Fe1 O3 Fe1 120.000(1) 3_565 2_665
N2 C3 C5 112.4(11) . .
N2 C3 C2 124.3(10) . .
C5 C3 C2 123.3(10) . .
C3 N2 C3 103.1(13) 4_675 .
C3 N2 Co1 128.1(6) 4_675 13_676
C3 N2 Co1 128.1(6) . 13_676
C3 N2 Co1 128.1(6) 4_675 .
C3 N2 Co1 128.1(6) . .
C10 O2 Ni1 135.3(6) . .
C1 C2 C3 123.7(9) . .
C1 C2 C6 119.2(9) . .
C3 C2 C6 117.1(9) . .
C4 C4 C1 106.8(6) 16_556 .
C4 C4 H4 126.6 16_556 .
C1 C4 H4 126.6 . .
C3 C5 C5 106.1(7) . 4_675
C3 C5 H5 127.0 . .
C5 C5 H5 127.0 4_675 .
C9 C8 C7 120.4(9) . .
C9 C8 H8 119.8 . .
C7 C8 H8 119.8 . .
C6 C7 C8 118.9(9) . .
C6 C7 H7 120.5 . .
C8 C7 H7 120.5 . .
C7 C6 C7 121.1(10) . 20
C7 C6 C2 119.4(5) . .
C7 C6 C2 119.4(5) 20 .
C8 C9 C8 120.2(10) . 20
C8 C9 C10 119.9(5) . .
C8 C9 C10 119.9(5) 20 .
O2 C10 O2 127.1(9) . 20
O2 C10 C9 116.5(5) . .
O2 C10 C9 116.5(5) 20 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.010(5) .
Ni1 O2 2.010(5) 10_665
Ni1 O2 2.010(5) 16
Ni1 O2 2.010(5) 19_665
Ni1 O3 2.013(2) .
Ni1 O1 2.066(10) .
Co1 Co1 0.48(5) 13_676
Co1 N1 1.987(12) 13_676
Co1 N1 1.987(12) .
Co1 N2 2.008(12) 13_676
Co1 N2 2.008(12) .
Co1 O4 2.16(4) .
C1 N1 1.377(12) .
C1 C2 1.380(14) .
C1 C4 1.385(15) .
N1 C1 1.377(12) 16_556
N1 Co1 1.987(12) 13_676
O3 Fe1 2.013(2) 3_565
O3 Ni1 2.013(2) 3_565
O3 Ni1 2.013(2) 2_665
O3 Fe1 2.013(2) 2_665
C3 N2 1.355(13) .
C3 C5 1.366(15) .
C3 C2 1.431(14) .
N2 C3 1.355(13) 4_675
N2 Co1 2.008(12) 13_676
O2 C10 1.224(6) .
C2 C6 1.505(13) .
C4 C4 1.37(2) 16_556
C4 H4 0.9300 .
C5 C5 1.37(3) 4_675
C5 H5 0.9300 .
C8 C9 1.385(9) .
C8 C7 1.405(10) .
C8 H8 0.9300 .
C7 C6 1.393(11) .
C7 H7 0.9300 .
C6 C7 1.393(11) 20
C9 C8 1.385(9) 20
C9 C10 1.530(13) .
C10 O2 1.224(6) 20
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C2 C1 N1 C1 180.004(2) . 16_556
C2 C1 N1 Co1 -8.8(9) . 13_676
C4 C1 N1 Co1 171.2(9) . 13_676
C2 C1 N1 Co1 8.8(9) . .
C4 C1 N1 Co1 -171.2(9) . .
C5 C3 N2 C3 0.005(8) . 4_675
C5 C3 N2 Co1 -171.3(9) . 13_676
C2 C3 N2 Co1 8.7(9) . 13_676
C5 C3 N2 Co1 171.3(9) . .
C2 C3 N2 Co1 -8.7(9) . .
N1 C1 C2 C6 180.000(6) . .
C5 C3 C2 C1 180.000(8) . .
N1 C1 C4 C4 -0.004(5) . 16_556
C2 C1 C4 C4 179.996(6) . 16_556
C9 C8 C7 C6 -0.9(15) . .
C8 C7 C6 C7 1.7(19) . 20
C8 C7 C6 C2 -179.5(9) . .
C1 C2 C6 C7 90.6(9) . .
C3 C2 C6 C7 -89.4(9) . .
C1 C2 C6 C7 -90.6(9) . 20
C3 C2 C6 C7 89.4(9) . 20
C7 C8 C9 C8 0.2(18) . 20
C7 C8 C9 C10 -177.1(9) . .
Ni1 O2 C10 O2 -2.1(16) . 20
Ni1 O2 C10 C9 178.3(6) . .
C8 C9 C10 O2 -1.5(13) . .
C8 C9 C10 O2 -178.8(9) 20 .
C8 C9 C10 O2 178.8(9) . 20
C8 C9 C10 O2 1.5(13) 20 20
