Encapsulation of N-containing compounds in a new hydrophilic Cd-based crystalline sponge via coordinative alignment method
Habib, Faiza; Tocher, Derek A.; Carmalt, Claire J.; CrystEngComm 25 (2023) 5001–5011; doi:10.1039/D3CE00592E

data_7247194
_publ_section_title
;
 Encapsulation of N-containing compounds in a new hydrophilic Cd-based
 crystalline sponge via coordinative alignment method
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              5001
_journal_page_last               5011
_journal_paper_doi               10.1039/D3CE00592E
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety
'0.33(C271.41 H216 Cd14 N34 O92), 2.17(C3 H8 O), 2.5(C3 H7 N O), 0.67(C3 H6 N O)'
_chemical_formula_sum            'C106.46 H110.99 Cd4.67 N14.5 O36'
_chemical_formula_weight         2694.13
_chemical_name_systematic
'catena- [tetrakis(\m6-4,4?4??-[1,3,5-benzenetriyltris(carbonylimino)]-trisbenzoateo)-bis(\m3-oxo)-penta(dimethlyformamide)-triaqua-hepta cadmium isopropanol'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-10-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-02-21 deposited with the CCDC.	2023-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.4290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   14.52210(10)
_cell_length_b                   42.7754(2)
_cell_length_c                   33.9548(2)
_cell_measurement_reflns_used    92410
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.3380
_cell_measurement_theta_min      3.7930
_cell_volume                     21054.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -59.00 -17.90   0.30    0.36    --  -42.62 -57.00   0.00  137
  2  \w   -112.00 -46.90   0.30    0.36    --  -42.62 -38.00 -30.00  217
  3  \w    -66.00  31.20   0.30    0.36    --  -42.62  38.00 -90.00  324
  4  \w    -64.00  28.10   0.30    0.36    --  -42.62  38.00 150.00  307
  5  \w     48.00  89.10   0.30    0.36    --   42.62-125.00-180.00  137
  6  \w     33.00  85.20   0.30    0.36    --   42.62-125.00   0.00  174
  7  \w     34.00  65.80   0.30    1.46    --  106.06 -30.00  30.00  106
  8  \w     78.00 103.80   0.30    1.46    --  106.06  61.00   0.00   86
  9  \w    113.00 164.00   0.30    1.46    --  106.06 125.00-180.00  170
 10  \w     84.00 109.80   0.30    1.46    --  106.06  45.00   0.00   86
 11  \w     81.00 106.80   0.30    1.46    --  106.06  45.00  30.00   86
 12  \w    110.80 177.70   0.30    1.46    --  106.06  77.00 150.00  223
 13  \w    117.00 177.00   0.30    1.46    --  106.06  61.00 -30.00  200
 14  \w     86.00 123.80   0.30    1.46    --  106.06 -30.00  30.00  126
 15  \w    132.00 158.10   0.30    1.46    --  106.06  61.00  30.00   87
 16  \w     97.00 175.00   0.30    1.46    --  106.06 125.00-120.00  260
 17  \w     78.00 108.00   0.30    1.46    --  106.06  61.00  30.00  100
 18  \w     85.00 126.10   0.30    1.46    --  106.06  45.00 -30.00  137
 19  \w     35.00 115.10   0.30    1.46    --  106.06 -45.00-180.00  267
 20  \w     64.00 103.00   0.30    1.46    --  106.06 -94.00 -90.00  130
 21  \w     85.00 110.80   0.30    1.46    --  106.06  61.00 -30.00   86
 22  \w     33.00  77.10   0.30    1.46    --  106.06-125.00  30.00  147
 23  \w     35.00 107.00   0.30    1.46    --  106.06 -94.00-180.00  240
 24  \w     65.00 166.10   0.30    1.46    --  106.06  15.00  90.00  337
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0179017000
_diffrn_orient_matrix_UB_12      -0.0257441000
_diffrn_orient_matrix_UB_13      -0.0303472000
_diffrn_orient_matrix_UB_21      0.0979272000
_diffrn_orient_matrix_UB_22      -0.0047082000
_diffrn_orient_matrix_UB_23      0.0190822000
_diffrn_orient_matrix_UB_31      -0.0372087000
_diffrn_orient_matrix_UB_32      -0.0247332000
_diffrn_orient_matrix_UB_33      0.0279500000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            166683
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.536
_diffrn_reflns_theta_min         3.541
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.106a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             8179
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.695
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2227
_refine_ls_number_reflns         41791
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1134P)^2^+28.2186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                37416
_reflns_number_total             41791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00592e2.cif
_cod_data_source_block           xstr1347_auto
_cod_depositor_comments
'Adding full bibliography for 7247186--7247196.cif.'
_cod_original_formula_sum        'C106.46 H110.99 Cd4.67 N14.50 O36'
_cod_database_code               7247194
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C136H50N9O50Cd7
_shelx_estimated_absorpt_t_max   0.836
_shelx_estimated_absorpt_t_min   0.371
_diffrn_oxdiff_digest_frames
;
01ece87772522c83f1401e692601c9fe0f000304a39
;
_diffrn_oxdiff_digest_hkl
;
01142e2733dbdfc727b8b2c3b862b5d86cd676
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C161-C162
 1.5 with sigma of 0.02
 C165-C166
 1.5 with sigma of 0.02
 C164-C165
 1.5 with sigma of 0.02
 N1-C1 = N21-C147 = N21-C146 = N20B-C158 = N20B-C159 = N18-C140 = N18-C141 =
 N19-C143 = N19-C144 = N22-C137 = N22-C138 = N13A-C98A = N13A-C99A = N12-C102 =
 N12-C103 = N17-C135 = N17-C136
 1.45 with sigma of 0.002
 N22-C139 = N12-C101 = N19-C145 = N18-C142 = N20B-C160
 1.34 with sigma of 0.002
 O46-C134 = O35-C97 = O32-C101 = O47-C139 = O57-C145 = O48-C142 = O50-C148 =
 O1-C3 = O5-C6
 1.23 with sigma of 0.002
 C169-C167 = C168-C167 = C166-C165 = C165-C164 = C163-C162 = C162-C161 = C157-
 C155 = C157-C156 = C153-C152 = C154-C153 = C151-C150 = C150-C149
 1.54 with sigma of 0.002
 O56-C167 = O55-C165 = O54-C162 = O52-C153 = O51-C150 = O49-C157
 1.23 with sigma of 0.002
 C166-C164
 2.5 with sigma of 0.002
 O49-C157 = O52-C153 = O54-C162 = O55-C165 = O56-C167 = O51-C150
 1.34 with sigma of 0.002
 O51-C150 = O56-C167 = O55-C165 = O54-C162 = O52-C153 = O49-C157
 1.34 with sigma of 0.002
 C97-H97
 0.98 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C97) \\sim Ueq, Uanis(N13A) \\sim Ueq, Uanis(C99A) \\sim Ueq, Uanis(C98A)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C138) \\sim Ueq, Uanis(N22) \\sim Ueq, Uanis(C137) \\sim Ueq, Uanis(C139)
\\sim Ueq, Uanis(O47) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C159) \\sim Ueq, Uanis(N20B) \\sim Ueq, Uanis(C158) \\sim Ueq,
Uanis(C160) \\sim Ueq, Uanis(O53) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C162) \\sim Ueq, Uanis(C161) \\sim Ueq, Uanis(C163) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(O52) \\sim Ueq, Uanis(C153) \\sim Ueq, Uanis(C152) \\sim Ueq, Uanis(C154)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C150) \\sim Ueq, Uanis(C151) \\sim Ueq, Uanis(C149) \\sim Ueq, Uanis(O51)
\\sim Ueq, Uanis(C157) \\sim Ueq, Uanis(O49) \\sim Ueq, Uanis(C155) \\sim Ueq,
Uanis(C156) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N13A) = Uanis(C97) = Uanis(C99A) = Uanis(C98A)
Uanis(C166) = Uanis(C165) = Uanis(C164) = Uanis(O55)
Uanis(C154) = Uanis(C153) = Uanis(C152) = Uanis(O52)
Uanis(N2) = Uanis(C6) = Uanis(C5) = Uanis(C4)
Uanis(C3) = Uanis(N1) = Uanis(C1) = Uanis(C2)
Uanis(C167) = Uanis(C169) = Uanis(C168) = Uanis(O56)
Uanis(C100) = Uanis(O34)
Uanis(O33) = Uanis(C100) = Uanis(O34)
4. Others
 Fixed Sof: Cd5(0.85) O49(0.5) H49(0.5) C155(0.5) H15A(0.5) H15B(0.5)
 H15C(0.5) C157(0.5) H157(0.5) C156(0.5) H15D(0.5) H15E(0.5) H15F(0.5)
 O56(0.75) H56A(0.75) C169(0.75) H16B(0.75) H16C(0.75) H16D(0.75) C167(0.75)
 H167(0.75) C168(0.75) H16E(0.75) H16F(0.75) H16G(0.75) O55(0.5) H55(0.5)
 C165(0.5) H165(0.5) C164(0.5) H16H(0.5) H16I(0.5) H16J(0.5) C166(0.5)
 H16K(0.5) H16L(0.5) H16M(0.5) O52(0.5) H52(0.5) C154(0.5) H15G(0.5) H15H(0.5)
 H15I(0.5) C153(0.5) H153(0.5) C152(0.5) H15J(0.5) H15K(0.5) H15L(0.5) O51(0.5)
 H51(0.5) O50(0.75) N21(0.75) C149(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C150(0.5)
 H150(0.5) C147(0.75) H14D(0.75) H14E(0.75) H14F(0.75) C146(0.75) H14G(0.75)
 H14H(0.75) H14I(0.75) C148(0.75) H148(0.75) C151(0.5) H15M(0.5) H15N(0.5)
 H15O(0.5) O54(0.5) H54A(0.5) C162(0.5) H162(0.5) C161(0.5) H16N(0.5) H16O(0.5)
 H16P(0.5) C163(0.5) H16Q(0.5) H16R(0.5) H16S(0.5) Cd5B(0.15)
5.a Ternary CH refined with riding coordinates:
 C157(H157), C167(H167), C165(H165), C153(H153), C150(H150), C162(H162)
5.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N9(H9), N14(H14), N3(H3), N4(H4), N10(H10), N15(H15), N8(H8),
 N11(H11), N7(H7), N16(H16), N6(H6), C109(H109), C117(H117), C100(H100),
 C3(H3A), C76(H76), C87(H87), C39(H39), C16(H16A), C40(H40), C27(H27), C84(H84),
  C94(H94), C53(H53), C18(H18), C34(H34), C107(H107), C42(H42), C134(H134),
 C23(H23), C43(H43), C78(H78), C115(H115), C13(H13), C86(H86), C20(H20),
 C92(H92), C123(H123), C131(H131), C121(H121), C10(H10G), C46(H46), C6(H6A),
 C113(H113), C72(H72), C73(H73), C24(H24), C80(H80), C31(H31), C12(H12),
 C57(H57), C9(H9A), C95(H95), C106(H106), C101(H101), C54(H54), C110(H110),
 C56(H56), C61(H61), C32(H32), C62(H62), C129(H129), C64(H64), C65(H65),
 C120(H120), C124(H124), C35(H35), C69(H69), C128(H128), C70(H70), C132(H132),
 C83(H83), C48(H48), C26(H26), C91(H91), C50(H50), C148(H148), C145(H145),
 C139(H139), C142(H142)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C136(H13A,H13B,H13C), C103(H10A,H10B,H10C), C99A(H99A,H99B,
 H99C), C1(H1A,H1B,H1C), C98A(H98A,H98B,H98C), C102(H10D,H10E,H10F), C2(H2A,H2B,
 H2C), C135(H13D,H13E,H13F), C4(H4A,H4B,H4C), C155(H15A,H15B,H15C), C156(H15D,
 H15E,H15F), C169(H16B,H16C,H16D), C168(H16E,H16F,H16G), C164(H16H,H16I,H16J),
 C166(H16K,H16L,H16M), C154(H15G,H15H,H15I), C152(H15J,H15K,H15L), C149(H14A,
 H14B,H14C), C147(H14D,H14E,H14F), C146(H14G,H14H,H14I), C151(H15M,H15N,H15O),
 C144(H14J,H14K,H14L), C143(H14M,H14N,H14O), C161(H16N,H16O,H16P), C163(H16Q,
 H16R,H16S), C138(H13G,H13H,H13I), C137(H13J,H13K,H13L), C158(H15P,H15Q,H15R),
 C159(H15S,H15T,H15U), C140(H14P,H14Q,H14R), C141(H14S,H14T,H14U)
5.d Idealised tetrahedral OH refined as rotating group:
 O49(H49), O56(H56A), O55(H55), O52(H52), O51(H51), O54(H54A)
;
_olex2_submission_original_sample_id xstr1347
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.865
_oxdiff_exptl_absorpt_empirical_full_min 0.728