#------------------------------------------------------------------------------
#$Date: 2019-11-25 16:39:04 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241345 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/10/4131037.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_4131037
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 N12 Ni6 O35, 3.36(O)'
_chemical_formula_sum            'C144 H72 Co3 N12 Ni6 O38.35'
_chemical_formula_weight         3112.78
_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                   31.7402(14)
_cell_length_b                   31.7402(14)
_cell_length_c                   16.7689(9)
_cell_measurement_reflns_used    6169
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      41.98
_cell_measurement_theta_min      2.78
_cell_volume                     14630.3(12)
_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 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0771
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            33245
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        47.819
_diffrn_reflns_theta_max         47.819
_diffrn_reflns_theta_min         2.784
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_T_max  0.7498
_exptl_absorpt_correction_T_min  0.4278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/4 (Bruker,2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.122
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       0.024(3)
_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   1.679
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2562
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.705
_refine_ls_R_factor_all          0.1849
_refine_ls_R_factor_gt           0.1586
_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          0.3819
_refine_ls_wR_factor_ref         0.4138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1850
_reflns_number_total             2562
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b08724_si_013.cif
_cod_data_source_block           I
_cod_original_cell_volume        14630.3(15)
_cod_database_code               4131037
_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   0.941
_shelx_estimated_absorpt_t_max   0.980
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 0.29701(4) 0.70299(4) 1.0000 0.0786(14) Uani 1 4 d S T P
Co1 Co 0.0000 0.5081(8) 0.5000 0.084(6) Uani 0.5 4 d S TU P
O1 O 0.25898(19) 0.74102(19) 1.0000 0.135(4) Uani 1 4 d S T P
C1 C 0.1024(4) 0.5512(2) 0.5672(7) 0.110(4) Uani 1 2 d S TU P
N1 N 0.0718(5) 0.5359(2) 0.5000 0.113(4) Uani 1 4 d S TU P
O3 O 0.3333 0.6667 1.0000 0.055(3) Uani 1 12 d S T P
C3 C 0.0404(5) 0.5202(2) 0.6674(7) 0.121(4) Uani 1 2 d S T P
N2 N 0.0000 0.5000 0.6156(8) 0.108(4) Uani 1 4 d S TU P
O2 O 0.25027(19) 0.6602(2) 0.9140(3) 0.105(2) Uani 1 1 d . . .
C2 C 0.0881(4) 0.5440(2) 0.6438(6) 0.115(4) Uani 1 2 d S TU P
C4 C 0.1512(5) 0.5756(3) 0.5440(7) 0.146(5) Uani 1 2 d S TU P
H4 H 0.1782 0.5891 0.5773 0.175 Uiso 1 2 calc R U P
O4 O 0.0000 0.5658(9) 0.5000 0.127(8) Uani 0.5 4 d S TU P
C5 C 0.0243(4) 0.5122(2) 0.7477(7) 0.144(6) Uani 1 2 d S T P
H5 H 0.0442 0.5221 0.7926 0.173 Uiso 1 2 calc R U P
O5 O 0.3333 0.6667 0.733(3) 0.41(6) Uiso 0.84(15) 6 d S . P
C8 C 0.1785(4) 0.5515(3) 0.7972(5) 0.144(4) Uani 1 1 d D . .
H8 H 0.1886 0.5313 0.8197 0.172 Uiso 1 1 calc R U .
C7 C 0.1447(4) 0.5344(4) 0.7359(6) 0.159(4) Uani 1 1 d D . .
H7 H 0.1343 0.5038 0.7141 0.191 Uiso 1 1 calc R U .
C6 C 0.1261(4) 0.56306(18) 0.7068(6) 0.116(4) Uani 1 2 d DS T P
C9 C 0.1973(4) 0.59863(19) 0.8252(6) 0.101(3) Uani 1 2 d DS T P
C10 C 0.2368(4) 0.61838(19) 0.8907(5) 0.090(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'
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 93.07(18) . 10_667
O3 Ni1 O2 93.07(18) . 19_665
O2 Ni1 O2 90.7(3) 10_667 19_665
O3 Ni1 O2 93.07(18) . 16_557
O2 Ni1 O2 89.0(3) 10_667 16_557
O2 Ni1 O2 173.9(3) 19_665 16_557
O3 Ni1 O2 93.07(18) . .
O2 Ni1 O2 173.9(3) 10_667 .
O2 Ni1 O2 89.0(3) 19_665 .
O2 Ni1 O2 90.7(3) 16_557 .
O3 Ni1 O1 180.00(7) . .
O2 Ni1 O1 86.93(17) 10_667 .
O2 Ni1 O1 86.93(18) 19_665 .
O2 Ni1 O1 86.93(17) 16_557 .
O2 Ni1 O1 86.93(17) . .
Co1 Co1 O4 180.000(15) 13_566 .
Co1 Co1 N2 82.4(7) 13_566 .
O4 Co1 N2 97.6(7) . .
Co1 Co1 N2 82.4(7) 13_566 13_566
O4 Co1 N2 97.6(7) . 13_566
N2 Co1 N2 164.8(14) . 13_566
Co1 Co1 N1 82.5(7) 13_566 .
O4 Co1 N1 97.5(7) . .
N2 Co1 N1 89.02(18) . .
N2 Co1 N1 89.02(18) 13_566 .
Co1 Co1 N1 82.5(7) 13_566 13_566
O4 Co1 N1 97.4(7) . 13_566
N2 Co1 N1 89.02(19) . 13_566
N2 Co1 N1 89.02(18) 13_566 13_566
N1 Co1 N1 165.1(14) . 13_566
Co1 Co1 O4 0.000(11) 13_566 13_566
O4 Co1 O4 180.0 . 13_566
N2 Co1 O4 82.4(7) . 13_566
N2 Co1 O4 82.4(7) 13_566 13_566
N1 Co1 O4 82.5(7) . 13_566
N1 Co1 O4 82.5(7) 13_566 13_566
C2 C1 C4 123.3(11) . .
C2 C1 N1 126.2(11) . .
C4 C1 N1 110.5(11) . .
C1 N1 C1 106.5(13) 16_556 .
C1 N1 Co1 126.4(6) 16_556 13_566
C1 N1 Co1 126.4(6) . 13_566
C1 N1 Co1 126.4(6) 16_556 .
C1 N1 Co1 126.4(6) . .
Co1 N1 Co1 14.9(14) 13_566 .
Ni1 O3 Ni1 120.0 2_665 3_565
Ni1 O3 Ni1 119.997(1) 2_665 .
Ni1 O3 Ni1 119.997(1) 3_565 .
C2 C3 N2 125.2(10) . .
C2 C3 C5 125.0(11) . .
N2 C3 C5 109.8(11) . .
C3 N2 C3 104.0(13) . 4_565
C3 N2 Co1 127.6(7) . 13_566
C3 N2 Co1 127.6(7) 4_565 13_566
C3 N2 Co1 127.6(7) . .
C3 N2 Co1 127.6(7) 4_565 .
Co1 N2 Co1 15.2(14) 13_566 .
C10 O2 Ni1 133.5(6) . .
C1 C2 C3 123.8(10) . .
C1 C2 C6 118.3(9) . .
C3 C2 C6 117.9(8) . .
C1 C4 C4 106.2(7) . 16_556
C1 C4 H4 126.9 . .
C4 C4 H4 126.9 16_556 .
Co1 O4 Co1 0.000(3) . 13_566
C5 C5 C3 108.2(7) 4_565 .
C5 C5 H5 125.9 4_565 .
C3 C5 H5 125.9 . .
C9 C8 C7 120.3(7) . .
C9 C8 H8 119.8 . .
C7 C8 H8 119.8 . .
C8 C7 C6 120.0(8) . .
C8 C7 H7 120.0 . .
C6 C7 H7 120.0 . .
C7 C6 C7 119.2(10) . 21_565
C7 C6 C2 120.4(5) . .
C7 C6 C2 120.4(5) 21_565 .
C8 C9 C8 119.5(9) 21_565 .
C8 C9 C10 120.2(5) 21_565 .
C8 C9 C10 120.2(5) . .
O2 C10 O2 128.4(10) . 21_565
O2 C10 C9 115.8(5) . .
O2 C10 C9 115.8(5) 21_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O3 1.997(2) .
Ni1 O2 2.027(5) 10_667
Ni1 O2 2.027(5) 19_665
Ni1 O2 2.027(5) 16_557
Ni1 O2 2.027(5) .
Ni1 O1 2.091(11) .
Co1 Co1 0.52(5) 13_566
Co1 O4 1.83(4) .
Co1 N2 1.955(13) .
Co1 N2 1.955(13) 13_566
Co1 N1 1.989(13) .
Co1 N1 1.989(13) 13_566
Co1 O4 2.35(3) 13_566
C1 C2 1.342(14) .
C1 C4 1.397(16) .
C1 N1 1.407(13) .
N1 C1 1.407(13) 16_556
N1 Co1 1.989(13) 13_566
O3 Ni1 1.997(2) 2_665
O3 Ni1 1.997(2) 3_565
C3 C2 1.368(14) .
C3 N2 1.410(14) .
C3 C5 1.418(15) .
N2 C3 1.410(14) 4_565
N2 Co1 1.955(13) 13_566
O2 C10 1.237(6) .
C2 C6 1.487(15) .
C4 C4 1.47(3) 16_556
C4 H4 0.9300 .
O4 Co1 2.35(3) 13_566
C5 C5 1.34(2) 4_565
C5 H5 0.9300 .
C8 C9 1.385(7) .
C8 C7 1.387(8) .
C8 H8 0.9300 .
C7 C6 1.395(7) .
C7 H7 0.9300 .
C6 C7 1.395(7) 21_565
C9 C8 1.385(7) 21_565
C9 C10 1.545(14) .
C10 O2 1.237(6) 21_565
