#------------------------------------------------------------------------------
#$Date: 2020-01-28 01:44:48 +0200 (Tue, 28 Jan 2020) $
#$Revision: 247267 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/40/4134050.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_4134050
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            'C45 H27 Mg2.25 N3 O13 Ti0.75'
_chemical_formula_weight         908.43
_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                   17.234(4)
_cell_length_b                   17.234(4)
_cell_length_c                   14.537(3)
_cell_measurement_temperature    296(2)
_cell_volume                     3739.2(14)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20380
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.327
_diffrn_reflns_theta_min         1.364
_exptl_absorpt_coefficient_mu    0.149
_exptl_crystal_density_diffrn    0.807
_exptl_crystal_F_000             931
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0405
_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          0.1509
_refine_ls_wR_factor_ref         0.1602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                969
_reflns_number_total             1319
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b12924_si_002.cif
_cod_data_source_block           pacs_Mg2Ti_bdc_tpbz
_cod_original_cell_volume        3739.2(19)
_cod_database_code               4134050
_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 0.26819(3) 0.73181(3) 0.750000 0.0162(4) Uani 0.748(8) 4 d S T P A 1
Ti01 Ti 0.26819(3) 0.73181(3) 0.750000 0.0162(4) Uani 0.252(8) 4 d S T P A 2
O1 O 0.333333 0.666667 0.750000 0.0223(11) Uani 1 12 d S T P . .
O11 O 0.17872(11) 0.65365(11) 0.65247(12) 0.0409(6) Uani 1 1 d . . . . .
C12 C 0.0721(2) 0.53605(11) 0.5609(2) 0.0382(9) Uani 1 2 d S T P . .
C13 C 0.0355(2) 0.44951(17) 0.5305(2) 0.0701(11) Uani 1 1 d . . . . .
H13 H 0.058727 0.414198 0.551139 0.084 Uiso 1 1 calc R U . . .
N21 N 0.19140(11) 0.80860(11) 0.750000 0.0288(9) Uani 1 4 d S T P . .
C22 C 0.0551(2) 0.8124(3) 0.750000 0.093(2) Uani 1 2 d S T P . .
H22 H -0.007213 0.779349 0.750000 0.111 Uiso 1 2 calc R U P A .
C23 C 0.09714(14) 0.90286(14) 0.750000 0.0355(12) Uani 1 4 d S T P A .
C24 C 0.04723(14) 0.95277(14) 0.750000 0.0364(12) Uani 1 4 d S T P . .
C25 C -0.04650(14) 0.9070(3) 0.750000 0.0388(12) Uani 1 4 d S T P A .
H25 H -0.077662 0.844678 0.750000 0.047 Uiso 1 4 calc R U P . .
C21 C 0.1039(2) 0.7684(3) 0.750000 0.0828(19) Uani 1 2 d S T P A .
H21 H 0.072307 0.706070 0.750000 0.099 Uiso 1 2 calc R U P . .
C11 C 0.1497(2) 0.57486(10) 0.6269(2) 0.0294(8) 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 94.77(5) . 10_666
O1 Mg01 O11 94.77(5) . 19_665
O11 Mg01 O11 88.55(11) 10_666 19_665
O1 Mg01 O11 94.77(5) . 16_557
O11 Mg01 O11 90.66(11) 10_666 16_557
O11 Mg01 O11 170.46(10) 19_665 16_557
O1 Mg01 O11 94.77(5) . .
O11 Mg01 O11 170.46(10) 10_666 .
O11 Mg01 O11 90.66(11) 19_665 .
O11 Mg01 O11 88.55(11) 16_557 .
O1 Mg01 N21 180.00(3) . .
O11 Mg01 N21 85.23(5) 10_666 .
O11 Mg01 N21 85.23(5) 19_665 .
O11 Mg01 N21 85.23(5) 16_557 .
O11 Mg01 N21 85.23(5) . .
O1 Mg01 Mg01 30.0 . 3_565
O11 Mg01 Mg01 73.53(5) 10_666 3_565
O11 Mg01 Mg01 73.53(5) 19_665 3_565
O11 Mg01 Mg01 115.32(5) 16_557 3_565
O11 Mg01 Mg01 115.32(5) . 3_565
N21 Mg01 Mg01 150.0 . 3_565
O1 Mg01 Mg01 30.0 . 2_665
O11 Mg01 Mg01 115.32(5) 10_666 2_665
O11 Mg01 Mg01 115.32(5) 19_665 2_665
O11 Mg01 Mg01 73.53(5) 16_557 2_665
O11 Mg01 Mg01 73.53(5) . 2_665
N21 Mg01 Mg01 149.999(1) . 2_665
Mg01 Mg01 Mg01 60.0 3_565 2_665
O1 Ti01 O11 94.77(5) . 10_666
O1 Ti01 O11 94.77(5) . 19_665
O11 Ti01 O11 88.55(11) 10_666 19_665
O1 Ti01 O11 94.77(5) . 16_557
O11 Ti01 O11 90.66(11) 10_666 16_557
O11 Ti01 O11 170.46(10) 19_665 16_557
O1 Ti01 O11 94.77(5) . .
O11 Ti01 O11 170.46(10) 10_666 .
O11 Ti01 O11 90.66(11) 19_665 .
O11 Ti01 O11 88.55(11) 16_557 .
O1 Ti01 N21 180.00(3) . .
O11 Ti01 N21 85.23(5) 10_666 .
O11 Ti01 N21 85.23(5) 19_665 .
O11 Ti01 N21 85.23(5) 16_557 .
O11 Ti01 N21 85.23(5) . .
Mg01 O1 Mg01 120.0 2_665 3_565
Mg01 O1 Mg01 120.0 2_665 .
Mg01 O1 Mg01 120.0 3_565 .
C11 O11 Mg01 133.52(16) . .
C11 O11 Ti01 133.52(16) . .
C13 C12 C13 118.3(3) . 21_565
C13 C12 C11 120.86(15) . .
C13 C12 C11 120.86(15) 21_565 .
C12 C13 C13 120.86(15) . 9_556
C12 C13 H13 119.6 . .
C13 C13 H13 119.6 9_556 .
C21 N21 C21 114.7(4) . 19_665
C21 N21 Ti01 122.7(2) . .
C21 N21 Ti01 122.7(2) 19_665 .
C21 N21 Mg01 122.7(2) . .
C21 N21 Mg01 122.7(2) 19_665 .
C23 C22 C21 120.6(4) . .
C23 C22 H22 119.7 . .
C21 C22 H22 119.7 . .
C22 C23 C22 115.4(4) 19_665 .
C22 C23 C24 122.3(2) 19_665 .
C22 C23 C24 122.3(2) . .
C25 C24 C25 118.5(4) . 2_675
C25 C24 C23 120.8(2) . .
C25 C24 C23 120.8(2) 2_675 .
C24 C25 C24 121.5(4) . 3_465
C24 C25 H25 119.2 . .
C24 C25 H25 119.2 3_465 .
N21 C21 C22 124.4(4) . .
N21 C21 H21 117.8 . .
C22 C21 H21 117.8 . .
O11 C11 O11 125.5(3) 21_565 .
O11 C11 C12 117.24(13) 21_565 .
O11 C11 C12 117.24(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg01 O1 1.9445(11) .
Mg01 O11 2.0310(15) 10_666
Mg01 O11 2.0310(15) 19_665
Mg01 O11 2.0310(15) 16_557
Mg01 O11 2.0310(15) .
Mg01 N21 2.292(3) .
Mg01 Mg01 3.3679(19) 3_565
Mg01 Mg01 3.3679(19) 2_665
Ti01 O1 1.9445(11) .
Ti01 O11 2.0310(15) 10_666
Ti01 O11 2.0310(15) 19_665
Ti01 O11 2.0310(15) 16_557
Ti01 O11 2.0310(15) .
Ti01 N21 2.292(3) .
O11 C11 1.246(2) .
C12 C13 1.370(3) .
C12 C13 1.370(3) 21_565
C12 C11 1.505(4) .
C13 C13 1.381(5) 9_556
C13 H13 0.9300 .
N21 C21 1.307(4) .
N21 C21 1.307(4) 19_665
C22 C23 1.351(4) .
C22 C21 1.386(5) .
C22 H22 0.9300 .
C23 C24 1.490(6) .
C24 C25 1.399(3) .
C24 C25 1.399(3) 2_675
C25 H25 0.9300 .
C21 H21 0.9300 .
