#------------------------------------------------------------------------------
#$Date: 2019-11-25 16:37:53 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241341 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/10/4131033.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_4131033
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         'C72 H39 Mg3 N6 O16'
_chemical_formula_sum            'C72 H39 Mg3 N6 O16'
_chemical_formula_weight         1317.02
_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-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   31.848(8)
_cell_length_b                   31.848(8)
_cell_length_c                   16.883(5)
_cell_measurement_reflns_used    6951
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      2.58
_cell_volume                     14830(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'ADSC Quantum Q315r software (ADSC, 2009)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.812
_diffrn_measured_fraction_theta_max 0.812
_diffrn_measurement_device_type  'ADSC Q315r CCD area-detector'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1839
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.812
_diffrn_reflns_Laue_measured_fraction_max 0.812
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            46259
_diffrn_reflns_point_group_measured_fraction_full 0.812
_diffrn_reflns_point_group_measured_fraction_max 0.812
_diffrn_reflns_theta_full        20.807
_diffrn_reflns_theta_max         20.807
_diffrn_reflns_theta_min         1.477
_exptl_absorpt_coefficient_mu    0.027
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1354
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.063(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.327
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         2439
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.343
_refine_ls_R_factor_all          0.1427
_refine_ls_R_factor_gt           0.1214
_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          0.3293
_refine_ls_wR_factor_ref         0.3516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1622
_reflns_number_total             2439
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b08724_si_006.cif
_cod_data_source_block           I
_cod_original_cell_volume        14830(8)
_cod_database_code               4131033
_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   0.998
_shelx_estimated_absorpt_t_max   1.000
_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'
'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
Mg1 Mg 0.29738(4) 0.59475(8) 0.5000 0.0731(11) Uani 1 4 d S T P
O1 O 0.25861(11) 0.5172(2) 0.5000 0.133(3) Uani 1 4 d S T P
C1 C 0.0404(2) 0.52020(11) 0.1723(6) 0.101(2) Uani 1 2 d S T P
N1 N 0.0000 0.5000 0.1184(6) 0.107(3) Uani 1 4 d S T P
H1 H 0.0000 0.5000 0.0674 0.128 Uiso 1 4 calc R U P
O2 O 0.24971(10) 0.59004(10) 0.4134(2) 0.1008(13) Uani 1 1 d . . .
C2 C 0.0881(2) 0.54405(11) 0.1423(5) 0.105(3) Uani 1 2 d S T P
N2 N 0.0740(3) 0.53699(14) 0.0000 0.101(3) Uani 1 4 d S T P
C10 C 0.23570(19) 0.61785(10) 0.3893(4) 0.080(2) Uani 1 2 d S T P
C3 C 0.1026(3) 0.55129(14) 0.0652(6) 0.115(3) Uani 1 2 d S T P
O3 O 0.3333 0.6667 0.5000 0.051(2) Uani 1 12 d S T P
C9 C 0.19831(19) 0.59915(9) 0.3248(5) 0.093(2) Uani 1 2 d DS TU P
C6 C 0.1270(2) 0.56352(10) 0.2083(5) 0.107(2) Uani 1 2 d DS TU P
C5 C 0.1527(2) 0.57635(11) 0.0394(5) 0.126(3) Uani 1 2 d S TU P
H5 H 0.1799 0.5899 0.0720 0.151 Uiso 1 2 calc R U P
C8 C 0.1799(2) 0.55344(18) 0.2941(4) 0.132(2) Uani 1 1 d D U .
H8 H 0.1929 0.5345 0.3110 0.158 Uiso 1 1 calc R U .
C7 C 0.1433(2) 0.5346(2) 0.2396(5) 0.151(3) Uani 1 1 d D U .
H7 H 0.1295 0.5024 0.2240 0.181 Uiso 1 1 calc R U .
C4 C 0.0249(2) 0.51244(12) 0.2513(7) 0.124(3) Uani 1 2 d S T P
H4 H 0.0447 0.5224 0.2958 0.148 Uiso 1 2 calc R U P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
Mg Mg 0.0486 0.0363 '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 Mg1 O2 93.62(10) . .
O3 Mg1 O2 93.63(10) . 11_556
O2 Mg1 O2 172.8(2) . 11_556
O3 Mg1 O2 93.63(10) . 20
O2 Mg1 O2 89.03(19) . 20
O2 Mg1 O2 90.51(19) 11_556 20
O3 Mg1 O2 93.63(10) . 16_556
O2 Mg1 O2 90.51(19) . 16_556
O2 Mg1 O2 89.03(19) 11_556 16_556
O2 Mg1 O2 172.7(2) 20 16_556
O3 Mg1 O1 180.00(15) . .
O2 Mg1 O1 86.38(10) . .
O2 Mg1 O1 86.37(10) 11_556 .
O2 Mg1 O1 86.37(10) 20 .
O2 Mg1 O1 86.37(10) 16_556 .
O3 Mg1 Mg1 30.0 . 2_665
O2 Mg1 Mg1 113.91(10) . 2_665
O2 Mg1 Mg1 72.79(10) 11_556 2_665
O2 Mg1 Mg1 72.79(10) 20 2_665
O2 Mg1 Mg1 113.91(10) 16_556 2_665
O1 Mg1 Mg1 150.0 . 2_665
O3 Mg1 Mg1 30.0 . 3_565
O2 Mg1 Mg1 72.80(10) . 3_565
O2 Mg1 Mg1 113.91(10) 11_556 3_565
O2 Mg1 Mg1 113.91(10) 20 3_565
O2 Mg1 Mg1 72.80(10) 16_556 3_565
O1 Mg1 Mg1 150.001(1) . 3_565
Mg1 Mg1 Mg1 60.0 2_665 3_565
C4 C1 C2 128.8(7) . .
C4 C1 N1 111.4(6) . .
C2 C1 N1 119.7(9) . .
C1 N1 C1 101.5(10) 4_565 .
C1 N1 H1 129.2 4_565 .
C1 N1 H1 129.2 . .
C10 O2 Mg1 134.0(3) . .
C3 C2 C1 128.1(7) . .
C3 C2 C6 119.0(6) . .
C1 C2 C6 112.9(7) . .
C3 N2 C3 108.7(11) . 16
O2 C10 O2 126.4(6) 21_565 .
O2 C10 C9 116.8(3) 21_565 .
O2 C10 C9 116.8(3) . .
N2 C3 C2 127.3(8) . .
N2 C3 C5 108.2(9) . .
C2 C3 C5 124.5(7) . .
Mg1 O3 Mg1 120.000(1) 3_565 2_665
Mg1 O3 Mg1 120.0 3_565 .
Mg1 O3 Mg1 120.000(1) 2_665 .
C8 C9 C8 116.1(6) . 21_565
C8 C9 C10 121.9(3) . .
C8 C9 C10 121.9(3) 21_565 .
C7 C6 C7 119.1(7) . 21_565
C7 C6 C2 120.4(3) . .
C7 C6 C2 120.4(3) 21_565 .
C5 C5 C3 107.5(5) 16 .
C5 C5 H5 126.3 16 .
C3 C5 H5 126.3 . .
C7 C8 C9 122.6(5) . .
C7 C8 H8 118.7 . .
C9 C8 H8 118.7 . .
C8 C7 C6 119.5(5) . .
C8 C7 H7 120.3 . .
C6 C7 H7 120.3 . .
C4 C4 C1 107.8(4) 4_565 .
C4 C4 H4 126.1 4_565 .
C1 C4 H4 126.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg1 O3 1.983(2) .
Mg1 O2 2.058(3) .
Mg1 O2 2.058(3) 11_556
Mg1 O2 2.058(3) 20
Mg1 O2 2.058(3) 16_556
Mg1 O1 2.139(7) .
Mg1 Mg1 3.435(4) 2_665
Mg1 Mg1 3.435(4) 3_565
C1 C4 1.402(13) .
C1 C2 1.409(9) .
C1 N1 1.439(11) .
N1 C1 1.439(11) 4_565
N1 H1 0.8600 .
O2 C10 1.243(4) .
C2 C3 1.361(11) .
C2 C6 1.547(10) .
N2 C3 1.355(9) .
N2 C3 1.355(9) 16
C10 O2 1.243(4) 21_565
C10 C9 1.500(9) .
C3 C5 1.449(11) .
O3 Mg1 1.983(2) 3_565
O3 Mg1 1.983(2) 2_665
C9 C8 1.371(6) .
C9 C8 1.371(6) 21_565
C6 C7 1.369(7) .
C6 C7 1.369(7) 21_565
C5 C5 1.332(18) 16
C5 H5 0.9300 .
C8 C7 1.367(7) .
C8 H8 0.9300 .
C7 H7 0.9300 .
C4 C4 1.372(13) 4_565
C4 H4 0.9300 .
