#------------------------------------------------------------------------------
#$Date: 2019-11-23 23:02:49 +0200 (Sat, 23 Nov 2019) $
#$Revision: 235490 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/64/7236415.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_7236415
loop_
_publ_author_name
'Chandrasekhar, Pujari'
'Mukhopadhyay, Arindam'
'Savitha, Govardhan'
'Moorthy, Jarugu Narasimha'
_publ_section_title
;
 Orthogonal self-assembly of a trigonal triptycene triacid: signaling of
 exfoliation of porous 2D metal--organic layers by fluorescence and
 selective CO2 capture by the hydrogen-bonded MOF
;
_journal_issue                   11
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              5402
_journal_paper_doi               10.1039/C6TA11110F
_journal_volume                  5
_journal_year                    2017
_chemical_formula_sum            'C24 H17 Cd N3 O6 S'
_chemical_formula_weight         587.86
_chemical_name_systematic        'Tripticene triacid'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'dual - dual-space method e.g. SHELXD'
_atom_sites_solution_secondary   'dual - dual-space method e.g. SHELXD'
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-09-27 deposited with the CCDC.
2017-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.489(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.0040(14)
_cell_length_b                   41.869(5)
_cell_length_c                   17.1369(17)
_cell_measurement_reflns_used    150
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      5
_cell_volume                     9728.4(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30948
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        18.485
_diffrn_reflns_theta_max         18.485
_diffrn_reflns_theta_min         2.094
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       square
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.092
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.0012(7)
_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   2.383
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         3617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.383
_refine_ls_R_factor_all          0.1801
_refine_ls_R_factor_gt           0.1699
_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          0.4741
_refine_ls_wR_factor_ref         0.4914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2958
_reflns_number_total             3617
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ta11110f2.cif
_cod_data_source_block           Cd_TPA_DMSO
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7236415
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, 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
O1 O 0.7132(14) 0.3259(4) 0.0846(11) 0.198(8) Uani 1 1 d . . . . .
S1 S 0.1296(8) 0.5477(3) 0.7156(10) 0.384(8) Uani 1 1 d . . . . .
N1 N 0.4873(6) 0.40660(19) 0.3580(6) 0.057(2) Uani 1 1 d . . . . .
H1 H 0.5480 0.4031 0.3821 0.069 Uiso 1 1 calc R U . . .
C1 C 0.6406(18) 0.3330(4) 0.0739(14) 0.115(6) Uani 1 1 d . . . . .
O2 O 0.5844(16) 0.3280(4) -0.0024(12) 0.220(8) Uani 1 1 d . . . . .
N2 N 0.3469(7) 0.4063(2) 0.2637(5) 0.060(3) Uani 1 1 d . . . . .
C2 C 0.582(2) 0.3507(3) 0.1268(13) 0.113(5) Uani 1 1 d . . . . .
O3 O 0.3192(12) 0.7543(3) 0.5358(9) 0.170(6) Uani 1 1 d . . . . .
N3 N 0.3229(5) 0.5865(2) 0.5452(4) 0.051(2) Uani 1 1 d . . . . .
C3 C 0.4856(14) 0.3559(5) 0.1025(11) 0.138(7) Uani 1 1 d . . . . .
H3 H 0.4504 0.3489 0.0520 0.166 Uiso 1 1 calc R U . . .
C4 C 0.4380(12) 0.3717(4) 0.1521(10) 0.124(6) Uani 1 1 d . . . . .
H4 H 0.3708 0.3759 0.1345 0.149 Uiso 1 1 calc R U . . .
C5 C 0.4904(10) 0.3817(3) 0.2291(8) 0.072(3) Uani 1 1 d . . . . .
C6 C 0.5834(14) 0.3755(4) 0.2495(9) 0.113(5) Uani 1 1 d . . . . .
H6 H 0.6203 0.3820 0.2999 0.135 Uiso 1 1 calc R U . . .
C7 C 0.6325(11) 0.3586(4) 0.1971(13) 0.107(5) Uani 1 1 d . . . . .
H7 H 0.6992 0.3536 0.2140 0.129 Uiso 1 1 calc R U . . .
C8 C 0.4408(9) 0.3985(2) 0.2822(8) 0.057(3) Uani 1 1 d . . . . .
C9 C 0.3286(8) 0.4222(2) 0.3308(6) 0.051(3) Uani 1 1 d . . . . .
C10 C 0.4178(7) 0.4218(2) 0.3895(7) 0.046(3) Uani 1 1 d . . . . .
C11 C 0.4243(7) 0.4359(2) 0.4638(7) 0.049(3) Uani 1 1 d . . . . .
H11 H 0.4837 0.4367 0.5029 0.059 Uiso 1 1 calc R U . . .
C12 C 0.3405(7) 0.44853(19) 0.4772(5) 0.039(3) Uani 1 1 d . . . . .
C13 C 0.2499(6) 0.44888(19) 0.4176(6) 0.040(3) Uani 1 1 d . . . . .
C14 C 0.2420(7) 0.4351(2) 0.3438(6) 0.050(3) Uani 1 1 d . . . . .
H14 H 0.1826 0.4344 0.3047 0.060 Uiso 1 1 calc R U . . .
C15 C 0.3325(6) 0.4657(2) 0.5568(6) 0.044(3) Uani 1 1 d . . . . .
H15 H 0.3947 0.4661 0.5986 0.053 Uiso 1 1 calc R U . . .
C16 C 0.2941(6) 0.4982(2) 0.5293(5) 0.038(3) Uani 1 1 d . . . . .
C17 C 0.3418(6) 0.5271(2) 0.5579(5) 0.042(3) Uani 1 1 d . . . . .
H17 H 0.4028 0.5273 0.5951 0.051 Uiso 1 1 calc R U . . .
C18 C 0.2945(6) 0.5547(3) 0.5284(4) 0.039(3) Uani 1 1 d . . . . .
C19 C 0.2500 0.6044(4) 0.5000 0.045(4) Uani 1 2 d S T P . .
C20 C 0.2500 0.6372(5) 0.5000 0.059(4) Uani 1 2 d S T P . .
C21 C 0.3324(10) 0.6556(3) 0.5360(8) 0.094(4) Uani 1 1 d . . . . .
H21 H 0.3906 0.6451 0.5611 0.112 Uiso 1 1 calc R U . . .
C22 C 0.3318(11) 0.6884(5) 0.5362(9) 0.106(4) Uani 1 1 d . . . . .
H22 H 0.3887 0.6995 0.5617 0.128 Uiso 1 1 calc R U . . .
C23 C 0.2500 0.7048(5) 0.5000 0.093(7) Uani 1 2 d S T P . .
C24 C 0.2500 0.7394(11) 0.5000 0.139(13) Uani 1 2 d S T P . .
O4 O 0.2295(16) 0.5542(6) 0.741(2) 0.384(8) Uani 1 1 d . . . . .
C26 C 0.016(2) 0.5574(9) 0.725(3) 0.384(8) Uani 1 1 d . . . . .
H26A H 0.0168 0.5791 0.7430 0.575 Uiso 1 1 calc R U . . .
H26B H -0.0020 0.5434 0.7625 0.575 Uiso 1 1 calc R U . . .
H26C H -0.0300 0.5554 0.6730 0.575 Uiso 1 1 calc R U . . .
Cd1 Cd 0.8658(3) 0.30378(9) 0.1021(3) 0.091(2) Uani 0.353(11) 1 d . . P A 1
O5A O 0.8551(16) 0.2742(5) 0.2158(11) 0.091(2) Uani 0.353(11) 1 d . . P A 1
O6A O 1.0233(17) 0.2889(6) 0.1375(12) 0.091(2) Uani 0.353(11) 1 d . . P A 1
Cd2 Cd 0.8114(9) 0.30244(8) 0.0488(7) 0.246(6) Uani 0.647(11) 1 d . . P A 2
O5B O 0.755(2) 0.2595(5) 0.2023(15) 0.246(6) Uani 0.647(11) 1 d . . P A 2
O6B O 0.970(3) 0.3030(4) 0.1789(19) 0.246(6) Uani 0.647(11) 1 d . . P A 2
C25 C 0.140(2) 0.5149(9) 0.670(3) 0.384(8) Uani 1 1 d . . . . .
H25A H 0.0757 0.5062 0.6472 0.575 Uiso 1 1 calc R U . . .
H25B H 0.1726 0.5189 0.6279 0.575 Uiso 1 1 calc R U . . .
H25C H 0.1781 0.4999 0.7077 0.575 Uiso 1 1 calc R U . . .
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'
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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
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
C1 O1 Cd2 148(2) . .
C1 O1 Cd1 172.4(19) . .
C1 O1 Cd2 92.8(17) . 2_655
Cd2 O1 Cd2 55.6(8) . 2_655
O4 S1 C25 96.6(15) . .
O4 S1 C26 145.5(17) . .
C25 S1 C26 117.1(18) . .
C8 N1 C10 106.0(8) . .
C8 N1 H1 127.0 . .
C10 N1 H1 127.0 . .
O1 C1 O2 115.7(18) . .
O1 C1 C2 133(3) . .
O2 C1 C2 112(2) . .
O1 C1 Cd2 64.7(13) . 2_655
O2 C1 Cd2 51.2(9) . 2_655
C2 C1 Cd2 163(2) . 2_655
C1 O2 Cd2 98.7(14) . 2_655
C1 O2 Cd1 125.8(14) . 2_655
C8 N2 C9 107.2(8) . .
C7 C2 C3 122.3(17) . .
C7 C2 C1 115(2) . .
C3 C2 C1 123(2) . .
C24 O3 Cd2 121(3) . 3_455
C24 O3 Cd1 143(2) . 3_455
C19 N3 C18 106.0(8) . .
C2 C3 C4 119.8(16) . .
C2 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
C3 C4 C5 120.3(15) . .
C3 C4 H4 119.9 . .
C5 C4 H4 119.9 . .
C6 C5 C4 116.8(14) . .
C6 C5 C8 122.3(12) . .
C4 C5 C8 120.8(13) . .
C5 C6 C7 122.4(15) . .
C5 C6 H6 118.8 . .
C7 C6 H6 118.8 . .
C2 C7 C6 118.3(14) . .
C2 C7 H7 120.9 . .
C6 C7 H7 120.9 . .
N2 C8 N1 112.6(9) . .
N2 C8 C5 125.0(12) . .
N1 C8 C5 122.4(11) . .
C10 C9 C14 123.2(9) . .
C10 C9 N2 105.6(9) . .
C14 C9 N2 131.1(10) . .
N1 C10 C11 131.7(10) . .
N1 C10 C9 108.5(9) . .
C11 C10 C9 119.9(9) . .
C12 C11 C10 117.5(8) . .
C12 C11 H11 121.3 . .
C10 C11 H11 121.3 . .
C11 C12 C13 122.5(8) . .
C11 C12 C15 125.3(9) . .
C13 C12 C15 112.1(8) . .
C14 C13 C12 120.8(8) . .
C14 C13 C15 125.1(9) . 2_556
C12 C13 C15 114.1(9) . 2_556
C13 C14 C9 116.0(9) . .
C13 C14 H14 122.0 . .
C9 C14 H14 122.0 . .
C16 C15 C13 106.0(6) . 2_556
C16 C15 C12 104.0(7) . .
C13 C15 C12 105.3(7) 2_556 .
C16 C15 H15 113.6 . .
C13 C15 H15 113.6 2_556 .
C12 C15 H15 113.6 . .
C16 C16 C17 120.8(5) 2_556 .
C16 C16 C15 114.5(5) 2_556 .
C17 C16 C15 124.7(7) . .
C18 C17 C16 117.1(8) . .
C18 C17 H17 121.5 . .
C16 C17 H17 121.5 . .
C17 C18 C18 122.1(5) . 2_556
C17 C18 N3 130.1(8) . .
C18 C18 N3 107.8(4) 2_556 .
N3 C19 N3 112.3(13) 2_556 .
N3 C19 C20 123.9(6) 2_556 .
N3 C19 C20 123.9(6) . .
C19 C20 C21 123.4(8) . 2_556
C19 C20 C21 123.4(8) . .
C21 C20 C21 113.2(17) 2_556 .
C22 C21 C20 123.2(14) . .
C22 C21 H21 118.4 . .
C20 C21 H21 118.4 . .
C23 C22 C21 120.8(15) . .
C23 C22 H22 119.6 . .
C21 C22 H22 119.6 . .
C22 C23 C22 119(2) 2_556 .
C22 C23 C24 120.6(10) 2_556 .
C22 C23 C24 120.6(10) . .
O3 C24 O3 117(4) 2_556 .
O3 C24 C23 122(2) 2_556 .
O3 C24 C23 122(2) . .
S1 C26 H26A 109.5 . .
S1 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
S1 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
O6A Cd1 O2 81.9(8) . 2_655
O6A Cd1 O1 169.3(8) . .
O2 Cd1 O1 100.2(7) 2_655 .
O6A Cd1 O5A 83.7(8) . .
O2 Cd1 O5A 165.6(9) 2_655 .
O1 Cd1 O5A 94.1(7) . .
O6A Cd1 O3 91.2(7) . 3_544
O2 Cd1 O3 97.5(6) 2_655 3_544
O1 Cd1 O3 98.9(7) . 3_544
O5A Cd1 O3 82.5(6) . 3_544
O1 Cd2 O3 127.4(8) . 3_544
O1 Cd2 Cd2 75.0(8) . 2_655
O3 Cd2 Cd2 88.2(7) 3_544 2_655
O1 Cd2 O2 118.7(8) . 2_655
O3 Cd2 O2 113.4(7) 3_544 2_655
Cd2 Cd2 O2 101.9(7) 2_655 2_655
O1 Cd2 O1 98.6(8) . 2_655
O3 Cd2 O1 107.2(7) 3_544 2_655
Cd2 Cd2 O1 49.4(5) 2_655 2_655
O2 Cd2 O1 52.6(6) 2_655 2_655
O1 Cd2 C1 110.3(7) . 2_655
O3 Cd2 C1 110.8(6) 3_544 2_655
Cd2 Cd2 C1 71.8(7) 2_655 2_655
O2 Cd2 C1 30.1(7) 2_655 2_655
O1 Cd2 C1 22.5(5) 2_655 2_655
O1 Cd2 O6B 103.8(9) . .
O3 Cd2 O6B 92.4(7) 3_544 .
Cd2 Cd2 O6B 178.9(5) 2_655 .
O2 Cd2 O6B 78.7(9) 2_655 .
O1 Cd2 O6B 131.2(7) 2_655 .
C1 Cd2 O6B 108.8(8) 2_655 .
O1 Cd2 O5B 72.6(6) . .
O3 Cd2 O5B 66.1(5) 3_544 .
Cd2 Cd2 O5B 108.3(6) 2_655 .
O2 Cd2 O5B 149.7(10) 2_655 .
O1 Cd2 O5B 157.6(8) 2_655 .
C1 Cd2 O5B 176.8(5) 2_655 .
O6B Cd2 O5B 71.1(8) . .
S1 C25 H25A 109.5 . .
S1 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
S1 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C1 1.03(2) .
O1 Cd2 1.911(16) .
O1 Cd1 2.279(18) .
O1 Cd2 2.43(2) 2_655
S1 O4 1.39(2) .
S1 C25 1.60(3) .
S1 C26 1.68(3) .
N1 C8 1.342(12) .
N1 C10 1.380(12) .
N1 H1 0.8600 .
C1 O2 1.36(2) .
C1 C2 1.56(2) .
C1 Cd2 2.687(17) 2_655
O2 Cd2 2.119(17) 2_655
O2 Cd1 2.242(15) 2_655
N2 C8 1.315(12) .
N2 C9 1.407(12) .
C2 C7 1.280(18) .
C2 C3 1.32(2) .
O3 C24 1.186(19) .
O3 Cd2 2.034(15) 3_455
O3 Cd1 2.374(15) 3_455
N3 C19 1.345(10) .
N3 C18 1.398(12) .
C3 C4 1.37(2) .
C3 H3 0.9300 .
C4 C5 1.403(17) .
C4 H4 0.9300 .
C5 C6 1.289(17) .
C5 C8 1.457(16) .
C6 C7 1.44(2) .
C6 H6 0.9300 .
C7 H7 0.9300 .
C9 C10 1.394(12) .
C9 C14 1.395(13) .
C10 C11 1.386(13) .
C11 C12 1.359(13) .
C11 H11 0.9300 .
C12 C13 1.416(11) .
C12 C15 1.570(13) .
C13 C14 1.369(12) .
C13 C15 1.507(12) 2_556
C14 H14 0.9300 .
C15 C16 1.493(12) .
C15 C13 1.507(12) 2_556
C15 H15 0.9800 .
C16 C16 1.382(16) 2_556
C16 C17 1.411(12) .
C17 C18 1.366(12) .
C17 H17 0.9300 .
C18 C18 1.377(15) 2_556
C19 N3 1.344(10) 2_556
C19 C20 1.37(2) .
C20 C21 1.396(15) 2_556
C20 C21 1.396(15) .
C21 C22 1.37(2) .
C21 H21 0.9300 .
C22 C23 1.346(16) .
C22 H22 0.9300 .
C23 C22 1.346(16) 2_556
C23 C24 1.45(4) .
C24 O3 1.186(19) 2_556
C26 H26A 0.9600 .
C26 H26B 0.9600 .
C26 H26C 0.9600 .
Cd1 O6A 2.22(2) .
Cd1 O2 2.242(15) 2_655
Cd1 O5A 2.35(2) .
Cd1 O3 2.374(15) 3_544
Cd2 O3 2.034(15) 3_544
Cd2 Cd2 2.08(3) 2_655
Cd2 O2 2.119(17) 2_655
Cd2 O1 2.43(2) 2_655
Cd2 C1 2.687(17) 2_655
Cd2 O6B 2.73(4) .
Cd2 O5B 3.44(2) .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
