#------------------------------------------------------------------------------
#$Date: 2020-01-28 01:44:48 +0200 (Tue, 28 Jan 2020) $
#$Revision: 247267 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/40/4134048.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_4134048
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 Co2.06 N6 O13 Ti0.94'
_chemical_formula_weight         987.09
_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                   16.871(3)
_cell_length_b                   16.871(3)
_cell_length_c                   14.955(2)
_cell_measurement_temperature    296(2)
_cell_volume                     3686.4(10)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19495
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        23.254
_diffrn_reflns_theta_max         23.254
_diffrn_reflns_theta_min         1.949
_exptl_absorpt_coefficient_mu    0.599
_exptl_crystal_density_diffrn    0.889
_exptl_crystal_F_000             997
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0427
_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          0.1439
_refine_ls_wR_factor_ref         0.1493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                869
_reflns_number_total             1037
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b12924_si_002.cif
_cod_data_source_block           pacs_CoTi_bdc_tpt
_cod_original_cell_volume        3686.3(12)
_cod_database_code               4134048
_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
Co01 Co 0.26587(3) 0.53175(6) 0.250000 0.0188(4) Uani 0.69(2) 4 d S T P A 1
Ti01 Ti 0.26587(3) 0.53175(6) 0.250000 0.0188(4) Uani 0.31(2) 4 d S T P A 2
O1 O 0.333333 0.666667 0.250000 0.0208(15) Uani 1 12 d S T P . .
O11 O 0.34679(16) 0.52259(15) 0.34498(16) 0.0405(8) Uani 1 1 d . . . . .
C12 C 0.46462(16) 0.53538(16) 0.4380(3) 0.0342(12) Uani 1 2 d S T P . .
C13 C 0.5524(3) 0.5874(3) 0.4693(3) 0.0646(15) Uani 1 1 d . . . . .
H13 H 0.588569 0.647025 0.448827 0.078 Uiso 1 1 calc R U . . .
N21 N 0.19064(16) 0.3813(3) 0.250000 0.0259(12) Uani 1 4 d S T P . .
C21 C 0.0990(3) 0.3331(3) 0.250000 0.0437(14) Uani 1 2 d S T P A .
H21 H 0.067293 0.365073 0.250000 0.052 Uiso 1 2 calc R U P . .
N22 N -0.0470(2) 0.0470(2) 0.250000 0.0494(18) Uani 1 4 d S T P . .
C23 C 0.0950(2) 0.1900(4) 0.250000 0.0404(18) Uani 1 4 d S T P A .
C24 C 0.0444(2) 0.0888(5) 0.250000 0.043(2) Uani 1 4 d S T P . .
C22 C 0.0490(3) 0.2385(3) 0.250000 0.0541(17) Uani 1 2 d S T P . .
H22 H -0.014658 0.207994 0.250000 0.065 Uiso 1 2 calc R U P A .
C11 C 0.42625(15) 0.57375(15) 0.3711(3) 0.0276(11) 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'
Co Co 0.3494 0.9721 '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 Co01 O11 93.78(7) . .
O1 Co01 O11 93.78(7) . 11
O11 Co01 O11 172.44(13) . 11
O1 Co01 O11 93.78(7) . 16_556
O11 Co01 O11 88.87(15) . 16_556
O11 Co01 O11 90.63(15) 11 16_556
O1 Co01 O11 93.78(7) . 20
O11 Co01 O11 90.63(15) . 20
O11 Co01 O11 88.87(15) 11 20
O11 Co01 O11 172.44(13) 16_556 20
O1 Co01 N21 180.00(5) . .
O11 Co01 N21 86.22(7) . .
O11 Co01 N21 86.22(7) 11 .
O11 Co01 N21 86.22(7) 16_556 .
O11 Co01 N21 86.22(7) 20 .
O1 Ti01 O11 93.78(7) . .
O1 Ti01 O11 93.78(7) . 11
O11 Ti01 O11 172.44(13) . 11
O1 Ti01 O11 93.78(7) . 16_556
O11 Ti01 O11 88.87(15) . 16_556
O11 Ti01 O11 90.63(15) 11 16_556
O1 Ti01 O11 93.78(7) . 20
O11 Ti01 O11 90.63(15) . 20
O11 Ti01 O11 88.87(15) 11 20
O11 Ti01 O11 172.44(13) 16_556 20
O1 Ti01 N21 180.00(5) . .
O11 Ti01 N21 86.22(7) . .
O11 Ti01 N21 86.22(7) 11 .
O11 Ti01 N21 86.22(7) 16_556 .
O11 Ti01 N21 86.22(7) 20 .
Co01 O1 Co01 120.0 3_565 2_665
Co01 O1 Co01 120.0 3_565 .
Co01 O1 Co01 120.0 2_665 .
C11 O11 Co01 134.6(2) . .
C11 O11 Ti01 134.6(2) . .
C13 C12 C13 118.5(4) . 19_665
C13 C12 C11 120.8(2) . .
C13 C12 C11 120.8(2) 19_665 .
C12 C13 C13 120.8(2) . 7_556
C12 C13 H13 119.6 . .
C13 C13 H13 119.6 7_556 .
C21 N21 C21 116.7(5) . 20
C21 N21 Ti01 121.7(3) . .
C21 N21 Ti01 121.7(3) 20 .
C21 N21 Co01 121.7(3) . .
C21 N21 Co01 121.7(3) 20 .
N21 C21 C22 123.6(4) . .
N21 C21 H21 118.2 . .
C22 C21 H21 118.2 . .
C24 N22 C24 114.4(7) . 2
C22 C23 C22 118.3(6) . 20
C22 C23 C24 120.9(3) . .
C22 C23 C24 120.9(3) 20 .
N22 C24 N22 125.6(7) 3 .
N22 C24 C23 117.2(3) 3 .
N22 C24 C23 117.2(3) . .
C23 C22 C21 119.0(4) . .
C23 C22 H22 120.5 . .
C21 C22 H22 120.5 . .
O11 C11 O11 125.4(4) 19_665 .
O11 C11 C12 117.27(19) 19_665 .
O11 C11 C12 117.27(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co01 O1 1.9712(9) .
Co01 O11 2.029(2) .
Co01 O11 2.029(2) 11
Co01 O11 2.029(2) 16_556
Co01 O11 2.029(2) 20
Co01 N21 2.199(5) .
Ti01 O1 1.9712(9) .
Ti01 O11 2.029(2) .
Ti01 O11 2.029(2) 11
Ti01 O11 2.029(2) 16_556
Ti01 O11 2.029(2) 20
Ti01 N21 2.199(5) .
O11 C11 1.240(3) .
C12 C13 1.372(4) .
C12 C13 1.372(4) 19_665
C12 C11 1.503(6) .
C13 C13 1.374(7) 7_556
C13 H13 0.9300 .
N21 C21 1.339(5) .
N21 C21 1.339(5) 20
C21 C22 1.384(7) .
C21 H21 0.9300 .
N22 C24 1.337(4) .
N22 C24 1.337(4) 2
C23 C22 1.381(6) .
C23 C22 1.381(6) 20
C23 C24 1.478(9) .
C22 H22 0.9300 .
