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#$Date: 2019-11-25 16:35:57 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241334 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/10/4131026.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_4131026
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 Co4.8 N12 Ni4.2 O35'
_chemical_formula_weight         3059.58
_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                   31.963(3)
_cell_length_b                   31.963(3)
_cell_length_c                   16.7135(16)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      43.07
_cell_measurement_theta_min      2.76
_cell_volume                     14787(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0814
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            34126
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        43.842
_diffrn_reflns_theta_max         43.842
_diffrn_reflns_theta_min         1.596
_exptl_absorpt_coefficient_mu    1.328
_exptl_absorpt_correction_T_max  0.7486
_exptl_absorpt_correction_T_min  0.4462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/4 (Bruker,2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1547
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.694
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       0.0052(10)
_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   1.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.899
_refine_ls_R_factor_all          0.1686
_refine_ls_R_factor_gt           0.1526
_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          0.4214
_refine_ls_wR_factor_ref         0.4375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1748
_reflns_number_total             2203
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b08724_si_016.cif
_cod_data_source_block           I
_cod_original_cell_volume        14788(3)
_cod_original_formula_sum        'C144 H72 Co4.80 N12 Ni4.20 O35'
_cod_database_code               4131026
_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 0.29720(4) 0.70280(4) 0.5000 0.0498(17) Uani 0.7 4 d S T P
O1 O 0.2588(2) 0.7412(2) 0.5000 0.107(5) Uani 1 4 d S T P
C1 C 0.1026(5) 0.5513(2) 0.0667(9) 0.095(5) Uani 1 2 d S T P
N1 N 0.0716(5) 0.5358(3) 0.0000 0.089(5) Uani 1 4 d S T P
Co1 Co 0.0000 0.5000 0.0000 0.078(2) Uani 1 8 d S T P
Co2 Co 0.29720(4) 0.70280(4) 0.5000 0.0498(17) Uani 0.3 4 d S T P
O3 O 0.3333 0.6667 0.5000 0.022(4) Uani 1 12 d S T P
C3 C 0.0390(5) 0.5195(2) 0.1673(8) 0.091(5) Uani 1 2 d S T P
N2 N 0.0000 0.5000 0.1155(9) 0.083(5) Uani 1 4 d S T P
O2 O 0.2500(2) 0.6603(2) 0.4127(4) 0.076(2) Uani 1 1 d . . .
C2 C 0.0875(5) 0.5438(3) 0.1442(10) 0.088(5) Uani 1 2 d S T P
C5 C 0.0247(5) 0.5123(2) 0.2464(9) 0.106(6) Uani 1 2 d S T P
H5 H 0.0447 0.5224 0.2910 0.127 Uiso 1 2 calc R U P
C4 C 0.1497(5) 0.5749(3) 0.0423(8) 0.139(7) Uani 1 2 d S T P
H4 H 0.1768 0.5884 0.0753 0.166 Uiso 1 2 calc R U P
O4 O 0.0000 0.5647(10) 0.0000 0.110(9) Uani 0.5 4 d S T P
C7 C 0.1440(4) 0.5343(4) 0.2381(7) 0.116(4) Uani 1 1 d . . .
H7 H 0.1323 0.5032 0.2184 0.139 Uiso 1 1 calc R U .
C6 C 0.1254(5) 0.5627(2) 0.2075(9) 0.087(5) Uani 1 2 d S T P
C9 C 0.1964(4) 0.5982(2) 0.3250(7) 0.073(4) Uani 1 2 d S T P
C10 C 0.2371(4) 0.6185(2) 0.3899(7) 0.061(4) Uani 1 2 d S T P
C8 C 0.1784(4) 0.5512(4) 0.2956(7) 0.107(4) Uani 1 1 d . . .
H8 H 0.1901 0.5318 0.3154 0.129 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'
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'
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
O3 Ni1 O2 93.64(17) . 10_666
O3 Ni1 O2 93.64(17) . 16_556
O2 Ni1 O2 88.8(3) 10_666 16_556
O3 Ni1 O2 93.64(17) . 19_665
O2 Ni1 O2 90.8(3) 10_666 19_665
O2 Ni1 O2 172.7(3) 16_556 19_665
O3 Ni1 O2 93.64(17) . .
O2 Ni1 O2 172.7(3) 10_666 .
O2 Ni1 O2 90.8(3) 16_556 .
O2 Ni1 O2 88.8(3) 19_665 .
O3 Ni1 O1 180.00(7) . .
O2 Ni1 O1 86.36(17) 10_666 .
O2 Ni1 O1 86.36(17) 16_556 .
O2 Ni1 O1 86.36(17) 19_665 .
O2 Ni1 O1 86.36(17) . .
C2 C1 C4 125.1(12) . .
C2 C1 N1 124.6(12) . .
C4 C1 N1 110.3(13) . .
C1 N1 C1 104.8(15) . 16
C1 N1 Co1 127.6(7) . .
C1 N1 Co1 127.6(7) 16 .
N2 Co1 N2 180.0 . 13_565
N1 Co1 N1 180.0 13_565 .
N2 Co1 O4 90.0 . 13_565
N2 Co1 O4 90.0 13_565 13_565
N1 Co1 O4 89.996(2) 13_565 13_565
N1 Co1 O4 90.000(2) . 13_565
N2 Co1 O4 90.0 . .
N2 Co1 O4 90.0 13_565 .
N1 Co1 O4 90.004(2) 13_565 .
N1 Co1 O4 90.000(2) . .
O4 Co1 O4 180.0 13_565 .
Co2 O3 Co2 120.000(1) 3_565 2_665
Ni1 O3 Ni1 120.000(1) 3_565 2_665
Ni1 O3 Ni1 120.000(1) 3_565 .
Ni1 O3 Ni1 120.0 2_665 .
C5 C3 N2 112.1(12) . .
C5 C3 C2 122.7(13) . .
N2 C3 C2 125.2(12) . .
C3 N2 C3 102.5(14) 4_565 .
C3 N2 Co1 128.8(7) 4_565 .
C3 N2 Co1 128.8(7) . .
C10 O2 Ni1 132.0(7) . .
C1 C2 C3 123.8(13) . .
C1 C2 C6 117.5(12) . .
C3 C2 C6 118.7(13) . .
C5 C5 C3 106.7(8) 4_565 .
C5 C5 H5 126.7 4_565 .
C3 C5 H5 126.7 . .
C1 C4 C4 107.3(8) . 16
C1 C4 H4 126.3 . .
C4 C4 H4 126.3 16 .
C8 C7 C6 121.4(11) . .
C8 C7 H7 119.3 . .
C6 C7 H7 119.3 . .
C7 C6 C7 118.0(13) 21_565 .
C7 C6 C2 121.0(6) 21_565 .
C7 C6 C2 121.0(6) . .
C8 C9 C8 120.1(12) . 21_565
O2 C10 O2 130.2(11) . 21_565
O2 C10 C9 114.9(6) . .
O2 C10 C9 114.9(6) 21_565 .
C7 C8 C9 119.6(10) . .
C7 C8 H8 120.2 . .
C9 C8 H8 120.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O3 2.000(2) .
Ni1 O2 2.049(7) 10_666
Ni1 O2 2.049(7) 16_556
Ni1 O2 2.049(7) 19_665
Ni1 O2 2.049(7) .
Ni1 O1 2.128(12) .
C1 C2 1.361(18) .
C1 C4 1.367(16) .
C1 N1 1.406(14) .
N1 C1 1.406(14) 16
N1 Co1 1.983(15) .
Co1 N2 1.930(16) .
Co1 N2 1.930(16) 13_565
Co1 N1 1.982(15) 13_565
Co1 O4 2.07(3) 13_565
Co1 O4 2.07(3) .
O3 Co2 2.000(2) 3_565
O3 Co2 2.000(2) 2_665
O3 Ni1 2.000(2) 3_565
O3 Ni1 2.000(2) 2_665
C3 C5 1.380(17) .
C3 N2 1.383(16) .
C3 C2 1.399(17) .
N2 C3 1.383(16) 4_565
O2 C10 1.244(7) .
C2 C6 1.490(18) .
C5 C5 1.37(3) 4_565
C5 H5 0.9300 .
C4 C4 1.42(3) 16
C4 H4 0.9300 .
C7 C8 1.353(14) .
C7 C6 1.406(12) .
C7 H7 0.9300 .
C6 C7 1.406(12) 21_565
C9 C8 1.402(10) .
C9 C8 1.402(10) 21_565
C9 C10 1.563(17) .
C10 O2 1.244(7) 21_565
C8 H8 0.9300 .
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
C4 C1 C2 C3 180.000(6) . .
C5 C3 C2 C1 180.000(5) . .
C2 C3 C5 C5 179.995(5) . 4_565
C8 C7 C6 C7 0(2) . 21_565
C8 C7 C6 C2 179.9(12) . .
C1 C2 C6 C7 89.7(11) . 21_565
C3 C2 C6 C7 -90.3(11) . 21_565
C1 C2 C6 C7 -89.7(11) . .
C3 C2 C6 C7 90.3(11) . .
Ni1 O2 C10 O2 -1.7(19) . 21_565
Ni1 O2 C10 C9 175.1(6) . .
C8 C9 C10 O2 -179.1(10) . .
C8 C9 C10 O2 1.7(15) 21_565 .
C8 C9 C10 O2 -1.7(16) . 21_565
C8 C9 C10 O2 179.1(10) 21_565 21_565
C6 C7 C8 C9 -0.5(19) . .
C8 C9 C8 C7 1(2) 21_565 .
C10 C9 C8 C7 -178.5(10) . .
