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_7247189
_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
'0.4(C260 H186 Cd14 N30 O87.98), 2.26(C3 H6 O), 2.2(C3 H7 N O)'
_chemical_formula_sum            'C117.39 H103.38 Cd5.6 N14.2 O39.66'
_chemical_formula_weight         2976.96
_chemical_name_systematic
'catena- [tetrakis(\m6-4,4?4??-[1,3,5-benzenetriyltris(carbonylimino)]-trisbenzoateo)-bis(\m3-oxo)-tri(dimethlyformamide)-pentaaqua-hepta cadmium acetone'
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-10-04
_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                 94.4569(11)
_cell_angle_gamma                90
_cell_formula_units_Z            5
_cell_length_a                   13.9475(2)
_cell_length_b                   43.3134(4)
_cell_length_c                   33.5321(4)
_cell_measurement_reflns_used    49814
_cell_measurement_temperature    151(1)
_cell_measurement_theta_max      73.2150
_cell_measurement_theta_min      3.8490
_cell_volume                     20195.9(4)
_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      151(1)
_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 0.984
_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    -71.00  27.00   1.00    6.88    --  -42.37  57.00   0.00   98
  2  \w   -116.00 -22.00   1.00    6.88    --  -42.37 -57.00-150.00   94
  3  \w     54.00  92.00   1.00    6.88    --   42.37-125.00 150.00   38
  4  \w    -24.00  67.00   1.00    6.88    --   42.37 -38.00  60.00   91
  5  \w     36.00  63.00   1.00    6.88    --   42.37 -99.00  60.00   27
  6  \w      7.00  34.00   1.00    6.88    --   42.37 -99.00  60.00   27
  7  \w     25.00 107.00   1.00   27.52    --  106.06 -94.00 150.00   82
  8  \w     44.00  97.00   1.00   27.52    --  106.06-125.00  60.00   53
  9  \w     81.00 164.00   1.00   27.52    --  106.06  45.00-120.00   83
 10  \w     59.00 118.00   1.00   27.52    --  106.06 -45.00   0.00   59
 11  \w     82.00 107.00   1.00   27.52    --  106.06 -94.00-120.00   25
 12  \w     58.00 135.00   1.00   27.52    --  106.06 -61.00-120.00   77
 13  \w     44.00 127.00   1.00   27.52    --  106.06 -45.00 150.00   83
 14  \w    122.00 178.00   1.00   27.52    --  106.06  15.00   0.00   56
 15  \w    109.00 135.00   1.00   27.52    --  106.06 125.00-120.00   26
 16  \w    128.00 177.00   1.00   27.52    --  106.06  77.00-180.00   49
 17  \w    153.00 178.00   1.00   27.52    --  106.06 125.00-120.00   25
 18  \w     82.00 107.00   1.00   27.52    --  106.06 -94.00 -60.00   25
 19  \w     70.00 106.00   1.00   27.52    --  106.06 -94.00-150.00   36
 20  \w     54.00 121.00   1.00   27.52    --  106.06  15.00   0.00   67
 21  \w    122.00 177.00   1.00   27.52    --  106.06  77.00 -60.00   55
 22  \w     70.00 108.00   1.00   27.52    --  106.06-105.00  67.45   38
;
_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      -0.0665256000
_diffrn_orient_matrix_UB_12      -0.0144978000
_diffrn_orient_matrix_UB_13      0.0294921000
_diffrn_orient_matrix_UB_21      -0.0558201000
_diffrn_orient_matrix_UB_22      0.0306119000
_diffrn_orient_matrix_UB_23      0.0014017000
_diffrn_orient_matrix_UB_31      -0.0687598000
_diffrn_orient_matrix_UB_32      -0.0108505000
_diffrn_orient_matrix_UB_33      -0.0353919000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            148527
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.535
_diffrn_reflns_theta_min         3.498
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.376
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32398
_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    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             7466
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.926
_refine_diff_density_min         -2.165
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2088
_refine_ls_number_reflns         40073
_refine_ls_number_restraints     466
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1158P)^2^+135.9879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2200
_refine_ls_wR_factor_ref         0.2454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29670
_reflns_number_total             40073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00592e2.cif
_cod_data_source_block           xstr1356_auto
_cod_depositor_comments
'Adding full bibliography for 7247186--7247196.cif.'
_cod_original_formula_sum        'C117.39 H103.38 Cd5.60 N14.20 O39.66'
_cod_database_code               7247189
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C150H130N30O50Cd7
_shelx_estimated_absorpt_t_max   0.701
_shelx_estimated_absorpt_t_min   0.278
_diffrn_oxdiff_digest_frames
;
01910c31f676668ab6a0200084137a351900027504d
;
_diffrn_oxdiff_digest_hkl
;
0119044b2dc567debec50603193edf817b8d65
;
_reflns_odcompleteness_completeness 99.93
_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
2. Restrained distances
 C138-C137
 2.2 with sigma of 0.02
 C130-C132
 2.6 with sigma of 0.02
 C132-C130
 2.1 with sigma of 0.02
 N1-C1 = N1-C2
 1.45 with sigma of 0.002
 N1-C3
 1.34 with sigma of 0.002
 O1-C3 = O9-C4 = O10-C4
 1.23 with sigma of 0.002
 O50-C143 = O49-C140 = O44_$1-C149_$1 = O45_$1-C146_$1
 1.23 with sigma of 0.002
 C150-C149 = C149-C148 = C147-C146 = C146-C145 = C141_$2-C140_$2 = C140_$2-
 C139_$2 = C144_$2-C143_$2 = C143_$2-C142_$2
 1.54 with sigma of 0.002
 O44-C150
 2.54 with sigma of 0.002
 N2-C70 = N2-C69
 1.45 with sigma of 0.002
 N2-C68
 1.34 with sigma of 0.002
 N6-C67 = N6-C66
 1.45 with sigma of 0.002
 N16-C136 = N16-C137 = N18_$3-C131_$3 = N18_$3-C130_$3 = N17_$3-C134_$3 =
 N17_$3-C133_$3
 1.45 with sigma of 0.002
 N18-C132 = N17-C135 = N16_$4-C138_$4
 1.34 with sigma of 0.002
 O48-C135 = O47-C132 = O46_$4-C138_$4 = O23-C65
 1.23 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
N6 \\sim C65 \\sim C66 \\sim C67: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
N18 \\sim C130 \\sim C131: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
O46 \\sim N16 \\sim C136 \\sim C137 \\sim C138: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008
O50 \\sim C142 \\sim C143 \\sim C144: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
O44 \\sim C149: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C134) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O50B) \\sim Ueq, Uanis(O50A) \\sim Ueq, Uanis(O14A) \\sim Ueq,
Uanis(O14B) \\sim Ueq, Uanis(Cd5A) \\sim Ueq, Uanis(Cd5B) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C151) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(N2) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C68)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C67) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(O23)
\\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C131) \\sim Ueq, Uanis(N18) \\sim Ueq, Uanis(C130) \\sim Ueq, Uanis(C132)
\\sim Ueq, Uanis(O47) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C135) \\sim Ueq, Uanis(N17) \\sim Ueq, Uanis(C134) \\sim Ueq, Uanis(C133)
\\sim Ueq, Uanis(O48) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C137) \\sim Ueq, Uanis(N16) \\sim Ueq, Uanis(C136) \\sim Ueq, Uanis(C138)
\\sim Ueq, Uanis(O46) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C55A) \\sim Ueq, Uanis(C55B) \\sim Ueq, Uanis(C54B) \\sim Ueq,
Uanis(C54A) \\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C141) \\sim Ueq, Uanis(C140) \\sim Ueq, Uanis(O49) \\sim Ueq, Uanis(C139)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O50) \\sim Ueq, Uanis(C143) \\sim Ueq, Uanis(C142) \\sim Ueq, Uanis(C144)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C147) \\sim Ueq, Uanis(C146) \\sim Ueq, Uanis(O45) \\sim Ueq, Uanis(C145)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O44) \\sim Ueq, Uanis(C149) \\sim Ueq, Uanis(C150) \\sim Ueq, Uanis(C148)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O10) = Uanis(C4) = Uanis(O9)
Uanis(C116) = Uanis(C121) = Uanis(C120) = Uanis(C119)
4. Others
 Fixed Sof: Cd5A(0.5) Cd5B(0.5) O14A(0.62) O14B(0.37) O50A(0.5) O50B(0.5)
 C1A(0.5) C54A(0.5) H54A(0.5) C54B(0.5) H54B(0.5) C55A(0.5) H55A(0.5) C55B(0.5)
 H55B(0.5) C151(0.5) O44(0.33) C148(0.33) H14B(0.33) H14C(0.33) H14D(0.33)
 C149(0.33) C150(0.33) H15A(0.33) H15B(0.33) H15C(0.33) O45(0.5) C145(0.5)
 H14E(0.5) H14F(0.5) H14G(0.5) C146(0.5) C147(0.5) H14H(0.5) H14I(0.5)
 H14J(0.5) O47(0.75) N18(0.75) C130(0.75) H13G(0.75) H13H(0.75) H13I(0.75)
 C131(0.75) H13J(0.75) H13K(0.75) H13L(0.75) C132(0.75) H132(0.75)
5.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), N5(H5), N7(H7), N8(H8), N9(H9), N10(H10), N11(H11), N12(H12),
 N13(H13), N14(H14), N15(H15), C3(H3A), C7(H7A), C8(H8A), C10(H10A), C11(H11A),
 C14(H14A), C16(H16), C18(H18), C22(H22), C23(H23), C25(H25), C26(H26),
 C29(H29), C30(H30), C32(H32), C33(H33), C37(H37), C38(H38), C40(H40), C41(H41),
  C44(H44), C46(H46), C48(H48), C51(H51), C52(H52), C54A(H54A), C54B(H54B),
 C55A(H55A), C55B(H55B), C58(H58), C59(H59), C61(H61), C62(H62), C64(H64),
 C65(H65), 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), C103(H103), C104(H104), C106(H106), C107(H107), C110(H110),
 C112(H112), C114(H114), C117(H117), C118(H118), C120(H120), C121(H121),
 C124(H124), C125(H125), C127(H127), C128(H128), C138(H138), C132(H132),
 C135(H135)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C148(H14B,H14C,H14D), C150(H15A,H15B,
 H15C), C145(H14E,H14F,H14G), C147(H14H,H14I,H14J), C136(H13A,H13B,H13C),
 C137(H13D,H13E,H13F), C130(H13G,H13H,H13I), C131(H13J,H13K,H13L), C133(H13M,
 H13N,H13O), C134(H13P,H13Q,H13R), C139(H13S,H13T,H13U), C141(H14K,H14L,H14M),
 C142(H14N,H14O,H14P), C144(H14Q,H14R,H14S)
;
_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 1.973
_oxdiff_exptl_absorpt_empirical_full_min 0.576