#------------------------------------------------------------------------------
#$Date: 2019-11-25 16:37:24 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241339 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/10/4131031.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_4131031
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_moiety         'C144 H72 Co3 Fe6 N12 O35, 4(O0.50)'
_chemical_formula_sum            'C144 H72 Co3 Fe6 N12 O37'
_chemical_formula_weight         3074.02
_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                   31.350(2)
_cell_length_b                   31.350(2)
_cell_length_c                   16.9103(11)
_cell_measurement_reflns_used    2317
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      38.86
_cell_measurement_theta_min      2.82
_cell_volume                     14393.2(16)
_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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker Kappa APEX-Duo CCD'
_diffrn_measurement_method       'ω scans'
_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  0.1375
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            23710
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        43.986
_diffrn_reflns_theta_max         43.986
_diffrn_reflns_theta_min         1.627
_exptl_absorpt_coefficient_mu    2.005
_exptl_absorpt_correction_T_max  0.7498
_exptl_absorpt_correction_T_min  0.4316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/4 (Bruker,2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1553
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.708
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         2113
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.713
_refine_ls_R_factor_all          0.2269
_refine_ls_R_factor_gt           0.1848
_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          0.4234
_refine_ls_wR_factor_ref         0.4482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1453
_reflns_number_total             2113
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b08724_si_010.cif
_cod_data_source_block           I
_cod_original_cell_volume        14393(2)
_cod_database_code               4131031
_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.
;
_shelx_estimated_absorpt_t_min   0.889
_shelx_estimated_absorpt_t_max   0.961
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
Fe1 Fe 0.29796(7) 0.70204(7) 0.5000 0.0454(17) Uani 1 4 d S T P
Co1 Co 0.0000 0.4923(13) 0.0000 0.049(8) Uani 0.5 4 d S TU P
O1 O 0.3333 0.6667 0.5000 0.049(7) Uani 1 12 d S T P
C1 C 0.0400(7) 0.5200(4) 0.1656(10) 0.071(6) Uani 1 2 d S TU P
N1 N 0.0000 0.5000 0.1166(12) 0.068(6) Uani 1 4 d S TU P
C3 C 0.1027(8) 0.5513(4) 0.0646(10) 0.080(6) Uani 1 2 d S TU P
O3 O 0.2606(3) 0.7394(3) 0.5000 0.078(5) Uani 1 4 d S T P
N2 N 0.0741(7) 0.5370(3) 0.0000 0.074(7) Uani 1 4 d S T P
O2 O 0.2503(3) 0.6605(3) 0.4153(4) 0.068(3) Uani 1 1 d . . .
C2 C 0.0884(6) 0.5442(3) 0.1424(9) 0.073(6) Uani 1 2 d DS TU P
C4 C 0.0244(6) 0.5122(3) 0.2457(11) 0.092(7) Uani 1 2 d S TU P
H4 H 0.0447 0.5223 0.2900 0.110 Uiso 1 2 calc R U P
O4 O 0.0000 0.4298(10) 0.0000 0.042(8) Uani 0.5 4 d S TU P
C5 C 0.1535(9) 0.5768(4) 0.0391(10) 0.103(8) Uani 1 2 d S TU P
H5 H 0.1811 0.5906 0.0717 0.124 Uiso 1 2 calc R U P
O5 O 0.3333 0.6667 0.171(8) 0.35(6) Uiso 0.5 6 d S . P
C7 C 0.1459(6) 0.5353(5) 0.2362(8) 0.116(7) Uani 1 1 d D . .
H7 H 0.1344 0.5038 0.2158 0.140 Uiso 1 1 calc R U .
C6 C 0.1277(5) 0.5639(3) 0.2073(8) 0.082(7) Uani 1 2 d DS T P
C9 C 0.1979(6) 0.5990(3) 0.3239(9) 0.062(6) Uani 1 2 d DS T P
C8 C 0.1807(5) 0.5525(4) 0.2949(8) 0.105(6) Uani 1 1 d D . .
H8 H 0.1925 0.5327 0.3149 0.126 Uiso 1 1 calc R U .
C10 C 0.2359(7) 0.6179(3) 0.3897(10) 0.055(5) Uani 1 2 d S TU 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'
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 94.8(3) . .
O1 Fe1 O2 94.8(3) . 10_666
O2 Fe1 O2 170.4(5) . 10_666
O1 Fe1 O2 94.8(3) . 19_665
O2 Fe1 O2 88.3(5) . 19_665
O2 Fe1 O2 90.9(5) 10_666 19_665
O1 Fe1 O2 94.8(3) . 16_556
O2 Fe1 O2 90.9(5) . 16_556
O2 Fe1 O2 88.3(5) 10_666 16_556
O2 Fe1 O2 170.5(5) 19_665 16_556
O1 Fe1 O3 180.00(12) . .
O2 Fe1 O3 85.2(3) . .
O2 Fe1 O3 85.2(3) 10_666 .
O2 Fe1 O3 85.2(3) 19_665 .
O2 Fe1 O3 85.2(3) 16_556 .
Co1 Co1 O4 180.000(10) 13_565 .
Co1 Co1 N1 83.0(12) 13_565 .
O4 Co1 N1 97.0(12) . .
Co1 Co1 N1 83.0(12) 13_565 13_565
O4 Co1 N1 97.0(12) . 13_565
N1 Co1 N1 166(2) . 13_565
Co1 Co1 N2 83.1(11) 13_565 .
O4 Co1 N2 96.9(12) . .
N1 Co1 N2 89.2(3) . .
N1 Co1 N2 89.2(3) 13_565 .
Co1 Co1 N2 83.1(12) 13_565 13_565
O4 Co1 N2 96.9(12) . 13_565
N1 Co1 N2 89.2(3) . 13_565
N1 Co1 N2 89.2(3) 13_565 13_565
N2 Co1 N2 166(2) . 13_565
Fe1 O1 Fe1 119.997(1) . 3_565
Fe1 O1 Fe1 120.0 . 2_665
Fe1 O1 Fe1 120.007(1) 3_565 2_665
N1 C1 C2 126.0(15) . .
N1 C1 C4 110.0(18) . .
C2 C1 C4 124.0(16) . .
C1 N1 C1 105(2) . 4_565
C1 N1 Co1 127.1(11) . .
C1 N1 Co1 127.1(11) 4_565 .
C1 N1 Co1 127.1(11) . 13_565
C1 N1 Co1 127.1(11) 4_565 13_565
Co1 N1 Co1 14(2) . 13_565
N2 C3 C2 128.2(18) . .
N2 C3 C5 108.0(17) . .
C2 C3 C5 123.8(16) . .
C3 N2 C3 109(2) . 16
C3 N2 Co1 125.1(11) . .
C3 N2 Co1 125.1(11) 16 .
C3 N2 Co1 125.1(11) . 13_565
C3 N2 Co1 125.1(11) 16 13_565
Co1 N2 Co1 14(2) . 13_565
C10 O2 Fe1 133.8(11) . .
C1 C2 C3 123.0(14) . .
C1 C2 C6 117.6(11) . .
C3 C2 C6 119.4(13) . .
C4 C4 C1 107.4(11) 4_565 .
C4 C4 H4 126.3 4_565 .
C1 C4 H4 126.3 . .
C5 C5 C3 107.3(10) 16 .
C5 C5 H5 126.3 16 .
C3 C5 H5 126.3 . .
C6 C7 C8 120.6(9) . .
C6 C7 H7 119.7 . .
C8 C7 H7 119.7 . .
C7 C6 C7 119.1(13) 21_565 .
C7 C6 C2 120.4(6) 21_565 .
C7 C6 C2 120.4(6) . .
C8 C9 C8 120.6(12) . 21_565
C8 C9 C10 119.7(6) . .
C8 C9 C10 119.7(6) 21_565 .
C9 C8 C7 119.5(9) . .
C9 C8 H8 120.2 . .
C7 C8 H8 120.2 . .
O2 C10 O2 124.5(18) . 21_565
O2 C10 C9 117.7(9) . .
O2 C10 C9 117.7(9) 21_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 1.921(4) .
Fe1 O2 2.009(8) .
Fe1 O2 2.009(8) 10_666
Fe1 O2 2.009(8) 19_665
Fe1 O2 2.009(8) 16_556
Fe1 O3 2.029(16) .
Co1 Co1 0.48(8) 13_565
Co1 O4 1.96(6) .
Co1 N1 1.99(2) .
Co1 N1 1.99(2) 13_565
Co1 N2 2.026(19) .
Co1 N2 2.026(19) 13_565
O1 Fe1 1.921(4) 3_565
O1 Fe1 1.921(4) 2_665
C1 N1 1.367(19) .
C1 C2 1.37(2) .
C1 C4 1.42(2) .
N1 C1 1.367(19) 4_565
N1 Co1 1.99(2) 13_565
C3 N2 1.341(19) .
C3 C2 1.37(2) .
C3 C5 1.45(2) .
N2 C3 1.341(19) 16
N2 Co1 2.026(19) 13_565
O2 C10 1.253(10) .
C2 C6 1.530(15) .
C4 C4 1.33(3) 4_565
C4 H4 0.9300 .
C5 C5 1.32(3) 16
C5 H5 0.9300 .
C7 C6 1.370(9) .
C7 C8 1.372(10) .
C7 H7 0.9300 .
C6 C7 1.370(9) 21_565
C9 C8 1.366(9) .
C9 C8 1.366(9) 21_565
C9 C10 1.52(2) .
C8 H8 0.9300 .
C10 O2 1.253(10) 21_565
