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_7247193
_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
'C131.25 H100.25 Cd7 N15.25 O46.25, 5(C3 H7 N O)'
_chemical_formula_sum            'C147.75 H0.25 Cd7 N20.75 O51.75'
_chemical_formula_weight         3680.24
_chemical_name_systematic
'catena- [tetrakis(\m6-4,4?4??-[1,3,5-benzenetriyltris(carbonylimino)]-trisbenzoateo)-bis(\m3-oxo)-tetra(dimethlyformamide)-tetraaqua-hepta cadmium dimethylformamide'
_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     dual
_audit_creation_date             2022-08-02
_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                 91.6490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6954(2)
_cell_length_b                   42.2913(4)
_cell_length_c                   33.8929(4)
_cell_measurement_reflns_used    54078
_cell_measurement_temperature    149.4(8)
_cell_measurement_theta_max      72.4590
_cell_measurement_theta_min      3.5890
_cell_volume                     21055.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.4(8)
_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 0.980
_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    -46.00 -21.00   1.00    5.71    --  -43.17 -38.00 150.00   25
  2  \w   -116.00 -84.00   1.00    5.71    --  -43.17 -38.00 150.00   32
  3  \w   -122.00 -16.00   1.00    5.71    --  -43.17 -19.00-120.00  106
  4  \w    -54.00  29.00   1.00    5.71    --  -43.17  38.00  60.00   83
  5  \w    -84.00  -9.00   1.00    5.71    --  -43.17 125.00 150.00   75
  6  \w     40.00  81.00   1.00    5.71    --   43.17 -99.00  60.00   41
  7  \w     75.00 107.00   1.00   22.85    --  103.94 -94.00 -90.00   32
  8  \w     44.00 110.00   1.00   22.85    --  103.94-125.00 -60.00   66
  9  \w     37.00  90.00   1.00   22.85    --  103.94 -45.00  90.00   53
 10  \w    110.00 161.00   1.00   22.85    --  103.94 125.00  90.00   51
 11  \w     82.00 176.00   1.00   22.85    --  103.94  30.00  60.00   94
 12  \w     40.00 110.00   1.00   22.85    --  103.94 -45.00   0.00   70
 13  \w     80.00 178.00   1.00   22.85    --  103.94  30.00 150.00   98
 14  \w     58.00 102.00   1.00   22.85    --  103.94 -94.00 120.00   44
 15  \w     33.00  89.00   1.00   22.85    --  103.94-125.00-120.00   56
 16  \w     77.00 111.00   1.00   22.85    --  103.94-125.00 120.00   34
 17  \w     81.00 107.00   1.00   22.85    --  103.94 -94.00 150.00   26
 18  \w    117.00 178.00   1.00   22.85    --  103.94  77.00   0.00   61
 19  \w     24.00  49.00   1.00   22.85    --  103.94 -94.00 120.00   25
 20  \w     98.00 153.00   1.00   22.85    --  103.94 125.00  60.00   55
 21  \w     33.00 107.00   1.00   22.85    --  103.94-102.00  28.64   74
;
_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      -0.0250140000
_diffrn_orient_matrix_UB_12      0.0303783000
_diffrn_orient_matrix_UB_13      -0.0228974000
_diffrn_orient_matrix_UB_21      0.0703295000
_diffrn_orient_matrix_UB_22      -0.0083295000
_diffrn_orient_matrix_UB_23      -0.0312034000
_diffrn_orient_matrix_UB_31      -0.0736662000
_diffrn_orient_matrix_UB_32      -0.0182877000
_diffrn_orient_matrix_UB_33      -0.0238822000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            160787
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.912
_diffrn_reflns_theta_min         3.409
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.161
_exptl_crystal_description       block
_exptl_crystal_F_000             7128
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.064
_refine_diff_density_max         5.449
_refine_diff_density_min         -2.701
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2066
_refine_ls_number_reflns         41170
_refine_ls_number_restraints     381
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1211P)^2^+111.6593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2019
_refine_ls_wR_factor_ref         0.2235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31558
_reflns_number_total             41170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00592e2.cif
_cod_data_source_block           xstr1329
_cod_depositor_comments
'Adding full bibliography for 7247186--7247196.cif.'
_cod_database_code               7247193
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C36H32N5O12Cd2
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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,H) groups
2. Restrained distances
 N4-C33 = N4-C34
 1.45 with sigma of 0.002
 N8-C66 = N8-C67 = N9-C69 = N9-C70 = N13-C102 = N13-C103 = N18-C138 = N18-C137
 = N22-C147 = N22-C146 = N21-C150 = N21-C149 = N20-C141 = N20-C140 = N19-C144 =
 N19-C143
 1.45 with sigma of 0.002
 N8-C65 = N9-C68 = N13-C101 = N17-C136 = N18-C139 = N4-C32 = N19-C145 = N20-
 C142 = N21-C151 = N22-C148
 1.34 with sigma of 0.002
 O38-C101 = O27-C68 = O26-C65 = O51-C148 = O53-C151 = O49-C139 = O13-C32 = O52-
 C145 = O50-C142
 1.23 with sigma of 0.02
 O22-C64 = O21-C64
 1.23 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
O22 \\sim C64: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C137 \\sim N18 \\sim O49 \\sim C139 \\sim C138: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008
C148 \\sim O51 \\sim N22 \\sim C146 \\sim C147: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008
O52 \\sim C145 \\sim N19 \\sim C144 \\sim C143: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008
N20 \\sim C142 \\sim O50 \\sim C140 \\sim C141: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008
Uanis(O22) \\sim Ueq, Uanis(C64) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C144) \\sim Ueq, Uanis(N19) \\sim Ueq, Uanis(C143) \\sim Ueq, Uanis(C145)
\\sim Ueq, Uanis(O52) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C137) \\sim Ueq, Uanis(N18) \\sim Ueq, Uanis(C139) \\sim Ueq, Uanis(O49)
\\sim Ueq, Uanis(C138) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(N20) \\sim Ueq, Uanis(C142) \\sim Ueq, Uanis(O50) \\sim Ueq, Uanis(C140)
\\sim Ueq, Uanis(C141) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(O27) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(C69)
\\sim Ueq, Uanis(C70) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(O26) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C67)
\\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(O38) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C103)
\\sim Ueq, Uanis(C102) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C134) \\sim Ueq, Uanis(N17) \\sim Ueq, Uanis(C135) \\sim Ueq, Uanis(C136)
\\sim Ueq, Uanis(O48) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C31) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O21) = Uanis(O22)
Uanis(C64) = Uanis(C61)
Uanis(O22) = Uanis(C64) = Uanis(O21)
Uanis(C32) = Uanis(O13) = Uanis(N4) = Uanis(C34) = Uanis(C33)
Uanis(C65) = Uanis(O26) = Uanis(N8)
4. Others
 Fixed Sof: O24(0.5) O27(0.75) N8(0.5) N9(0.75) C66(0.5) H66A(0.5) H66B(0.5)
 H66C(0.5) C67(0.5) H67A(0.5) H67B(0.5) H67C(0.5) C68(0.75) H68(0.75) C69(0.75)
 H69A(0.75) H69B(0.75) H69C(0.75) C70(0.75) H70A(0.75) H70B(0.75) H70C(0.75)
 O50(0.5) N20(0.5) C140(0.5) H14B(0.5) H14C(0.5) H14D(0.5) C141(0.5) H14E(0.5)
 H14F(0.5) H14G(0.5) C142(0.5) H142(0.5) O52(0.5) N19(0.5) C143(0.5) H14N(0.5)
 H14O(0.5) H14P(0.5) C144(0.5) H14Q(0.5) H14R(0.5) H14S(0.5) C145(0.5) H145(0.5)
 Fixed Uiso: H13D(0.11258) H13E(0.11258) H13F(0.11258)
5.a Rotating group:
 O10(H10A,H10B), O34(H34A,H34B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N5(H5), N6(H6), N7(H7), N10(H10), N11(H11), N12(H12),
 N14(H14), N15(H15), N16(H16), C3(H3A), C4(H4), C6(H6A), C7(H7A), C10(H10C),
 C12(H12A), C14(H14A), C17(H17), C18(H18), C20(H20), C21(H21), C25(H25),
 C26(H26), C28(H28), C29(H29), C31(H31), C32(H32), C37(H37), C38(H38), C40(H40),
  C41(H41), C44(H44), C46(H46), C48(H48), C51(H51), C52(H52), C54(H54),
 C55(H55), C59(H59), C60(H60), C62(H62), C63(H63), C65(H65), C68(H68), C73(H73),
  C74(H74), C76(H76), C77(H77), C80(H80), C82(H82), C84(H84), C87(H87),
 C88(H88), C90(H90), C91(H91), C95(H95), C96(H96), C98(H98), C99(H99),
 C101(H101), C106(H106), C107(H107), C109(H109), C110(H110), C113(H113),
 C115(H115), C117(H117), C120(H120), C121(H121), C123(H123), C124(H124),
 C128(H128), C129(H129), C131(H131), C132(H132), C136(H136), C139(H139),
 C142(H142), C148(H148), C145(H145), C151(H151)
5.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34C,H34D,H34E), C66(H66A,H66B,H66C), C67(H67A,H67B,
 H67C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C102(H10D,H10E,H10F),
 C103(H10G,H10H,H10I), C134(H13A,H13B,H13C), C135(H13D,H13E,H13F), C137(H13G,
 H13H,H13I), C138(H13J,H13K,H13L), C140(H14B,H14C,H14D), C141(H14E,H14F,H14G),
 C146(H14H,H14I,H14J), C147(H14K,H14L,H14M), C143(H14N,H14O,H14P), C144(H14Q,
 H14R,H14S), C149(H14T,H14U,H14V), C150(H15A,H15B,H15C)
;
_olex2_date_sample_data_collection 2021-03-22
_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 1.774
_oxdiff_exptl_absorpt_empirical_full_min 0.720