#------------------------------------------------------------------------------
#$Date: 2020-01-28 01:44:48 +0200 (Tue, 28 Jan 2020) $
#$Revision: 247267 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/40/4134052.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_4134052
loop_
_publ_author_name
'Yang, Huajun'
'Wang, Yanxiang'
'Krishna, Rajamani'
'Jia, Xiaoxia'
'Wang, Yong'
'Hong, Anh N.'
'Dang, Candy'
'Castillo, Henry E.'
'Bu, Xianhui'
'Feng, Pingyun'
_publ_section_title
;
 Pore-Space-Partition-Enabled Exceptional Ethane Uptake and
 Ethane-Selective Ethane--Ethylene Separation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b12924
_journal_year                    2020
_chemical_formula_sum            'C42 H24 Mg2.22 N6 O13 Ti0.78'
_chemical_formula_weight         912.00
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   17.014(12)
_cell_length_b                   17.014(12)
_cell_length_c                   14.838(10)
_cell_measurement_temperature    296(2)
_cell_volume                     3720(4)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17564
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.458
_diffrn_reflns_theta_min         1.948
_exptl_absorpt_coefficient_mu    0.154
_exptl_crystal_density_diffrn    0.814
_exptl_crystal_F_000             932
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0338
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1061
_reflns_number_total             1324
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b12924_si_002.cif
_cod_data_source_block           MgTi_bdc_tpt
_cod_original_cell_volume        3720(6)
_cod_database_code               4134052
_shelx_shelxl_version_number     2016/6
_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+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mg01 Mg 0.73248(3) 0.26752(3) 0.750000 0.0161(3) Uani 0.732(7) 4 d S T P A 1
Ti01 Ti 0.73248(3) 0.26752(3) 0.750000 0.0161(3) Uani 0.268(7) 4 d S T P A 2
O1 O 0.666667 0.333333 0.750000 0.0230(8) Uani 1 12 d S T P . .
O11 O 0.65389(8) 0.17683(8) 0.65444(9) 0.0380(4) Uani 1 1 d . . . . .
C12 C 0.53565(8) 0.07130(17) 0.56157(17) 0.0363(7) Uani 1 2 d S T P . .
C13 C 0.58725(13) 0.03531(16) 0.53084(16) 0.0629(8) Uani 1 1 d . . . . .
H13 H 0.646343 0.058563 0.551631 0.076 Uiso 1 1 calc R U . . .
N21 N 0.81042(9) 0.18958(9) 0.750000 0.0294(7) Uani 1 4 d S T P . .
C21 C 0.76767(17) 0.09887(17) 0.750000 0.0458(8) Uani 1 2 d S T P A .
H21 H 0.704557 0.067350 0.750000 0.055 Uiso 1 2 calc R U P . .
N22 N 1.04653(9) 0.09307(19) 0.750000 0.0468(9) Uani 1 4 d S T P . .
C23 C 0.90536(11) 0.09464(11) 0.750000 0.0403(9) Uani 1 4 d S T P A .
C24 C 0.95579(11) 0.04421(11) 0.750000 0.0424(10) Uani 1 4 d S T P . .
C22 C 0.81169(17) 0.04926(17) 0.750000 0.0541(9) Uani 1 2 d S T P . .
H22 H 0.778712 -0.013831 0.750000 0.065 Uiso 1 2 calc R U P A .
C11 C 0.57400(7) 0.14801(15) 0.62855(15) 0.0277(6) Uani 1 2 d S T P A .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Mg Mg 0.0486 0.0363 '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'
Ti Ti 0.2776 0.4457 '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 Mg01 O11 95.04(4) . .
O1 Mg01 O11 95.04(4) . 10_666
O11 Mg01 O11 169.91(8) . 10_666
O1 Mg01 O11 95.04(4) . 19_665
O11 Mg01 O11 90.44(10) . 19_665
O11 Mg01 O11 88.67(10) 10_666 19_665
O1 Mg01 O11 95.04(4) . 16_557
O11 Mg01 O11 88.67(10) . 16_557
O11 Mg01 O11 90.44(10) 10_666 16_557
O11 Mg01 O11 169.91(8) 19_665 16_557
O1 Mg01 N21 180.00(2) . .
O11 Mg01 N21 84.96(4) . .
O11 Mg01 N21 84.96(4) 10_666 .
O11 Mg01 N21 84.96(4) 19_665 .
O11 Mg01 N21 84.96(4) 16_557 .
O1 Mg01 Mg01 30.0 . 3_665
O11 Mg01 Mg01 73.81(4) . 3_665
O11 Mg01 Mg01 115.53(4) 10_666 3_665
O11 Mg01 Mg01 115.53(4) 19_665 3_665
O11 Mg01 Mg01 73.81(4) 16_557 3_665
N21 Mg01 Mg01 150.0 . 3_665
O1 Mg01 Mg01 30.0 . 2_655
O11 Mg01 Mg01 115.53(4) . 2_655
O11 Mg01 Mg01 73.81(4) 10_666 2_655
O11 Mg01 Mg01 73.81(4) 19_665 2_655
O11 Mg01 Mg01 115.53(4) 16_557 2_655
N21 Mg01 Mg01 150.0 . 2_655
Mg01 Mg01 Mg01 60.0 3_665 2_655
O1 Ti01 O11 95.04(4) . .
O1 Ti01 O11 95.04(4) . 10_666
O11 Ti01 O11 169.91(8) . 10_666
O1 Ti01 O11 95.04(4) . 19_665
O11 Ti01 O11 90.44(10) . 19_665
O11 Ti01 O11 88.67(10) 10_666 19_665
O1 Ti01 O11 95.04(4) . 16_557
O11 Ti01 O11 88.67(10) . 16_557
O11 Ti01 O11 90.44(10) 10_666 16_557
O11 Ti01 O11 169.91(8) 19_665 16_557
O1 Ti01 N21 180.00(2) . .
O11 Ti01 N21 84.96(4) . .
O11 Ti01 N21 84.96(4) 10_666 .
O11 Ti01 N21 84.96(4) 19_665 .
O11 Ti01 N21 84.96(4) 16_557 .
Mg01 O1 Mg01 120.0 . 3_665
Ti01 O1 Mg01 120.000(1) . 2_655
Mg01 O1 Mg01 120.000(1) . 2_655
Mg01 O1 Mg01 120.000(1) 3_665 2_655
C11 O11 Mg01 133.28(12) . .
C11 O11 Ti01 133.28(12) . .
C13 C12 C13 118.9(2) 20_655 .
C13 C12 C11 120.57(11) 20_655 .
C13 C12 C11 120.57(11) . .
C12 C13 C13 120.57(11) . 8_556
C12 C13 H13 119.7 . .
C13 C13 H13 119.7 8_556 .
C21 N21 C21 116.2(3) . 19_665
C21 N21 Ti01 121.90(14) . .
C21 N21 Ti01 121.90(14) 19_665 .
C21 N21 Mg01 121.90(14) . .
C21 N21 Mg01 121.90(14) 19_665 .
N21 C21 C22 123.9(2) . .
N21 C21 H21 118.1 . .
C22 C21 H21 118.1 . .
C24 N22 C24 114.9(3) 3_765 .
C22 C23 C22 117.9(3) . 19_665
C22 C23 C24 121.03(16) . .
C22 C23 C24 121.03(16) 19_665 .
N22 C24 N22 125.1(3) 2_645 .
N22 C24 C23 117.46(17) 2_645 .
N22 C24 C23 117.46(17) . .
C21 C22 C23 119.1(2) . .
C21 C22 H22 120.5 . .
C23 C22 H22 120.5 . .
O11 C11 O11 125.6(2) 20_655 .
O11 C11 C12 117.20(10) 20_655 .
O11 C11 C12 117.20(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg01 O1 1.9395(15) .
Mg01 O11 2.0288(15) .
Mg01 O11 2.0288(15) 10_666
Mg01 O11 2.0288(15) 19_665
Mg01 O11 2.0288(15) 16_557
Mg01 N21 2.297(3) .
Mg01 Mg01 3.359(3) 3_665
Mg01 Mg01 3.359(3) 2_655
Ti01 O1 1.9395(15) .
Ti01 O11 2.0288(15) .
Ti01 O11 2.0288(15) 10_666
Ti01 O11 2.0288(15) 19_665
Ti01 O11 2.0288(15) 16_557
Ti01 N21 2.297(3) .
O11 C11 1.2527(17) .
C12 C13 1.375(2) 20_655
C12 C13 1.375(2) .
C12 C11 1.505(3) .
C13 C13 1.386(4) 8_556
C13 H13 0.9300 .
N21 C21 1.337(3) .
N21 C21 1.337(3) 19_665
C21 C22 1.380(4) .
C21 H21 0.9300 .
N22 C24 1.338(2) 3_765
N22 C24 1.338(2) .
C23 C22 1.380(3) .
C23 C22 1.380(3) 19_665
C23 C24 1.486(5) .
C22 H22 0.9300 .
