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_7247187
_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
'C133.2 H98.2 Cd6.8 N16 O46, 2(C3 H7 N O), 1.5(C2 H3 N)'
_chemical_formula_sum            'C142.2 H117.2 Cd6.8 N19.5 O48'
_chemical_formula_weight         3631.47
_chemical_name_systematic
'catena- [tetrakis(\m6-4,4?4??-[1,3,5-benzenetriyltris(carbonylimino)]-trisbenzoateo)-bis(\m3-oxo)-tetra(dimethlyformamide)-tetraaqua-hepta cadmium acetonitrile'
_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             2022-08-03
_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                 95.3182(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6817(2)
_cell_length_b                   43.2808(4)
_cell_length_c                   33.7646(4)
_cell_measurement_reflns_used    31721
_cell_measurement_temperature    154(7)
_cell_measurement_theta_max      73.1000
_cell_measurement_theta_min      3.8940
_cell_volume                     19907.8(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      154(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.972
_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    -70.00 -26.00   1.00   14.65    --  -42.62  57.00  60.00   44
  2  \w    -41.00 -10.00   1.00   14.65    --  -42.62 125.00-120.00   31
  3  \w   -117.00 -19.00   1.00   14.65    --  -42.62 -38.00  30.00   98
  4  \w     56.00  95.00   1.00   14.65    --   42.62-125.00-120.00   39
  5  \w     29.00  56.00   1.00   14.65    --   42.62-125.00 -30.00   27
  6  \w     25.00  98.00   1.00   58.59    --  106.06 -94.00-180.00   73
  7  \w    136.00 165.00   1.00   58.59    --  106.06  45.00 -60.00   29
  8  \w     86.00 154.00   1.00   58.59    --  106.06  45.00 -30.00   68
  9  \w    119.00 171.00   1.00   58.59    --  106.06  77.00  30.00   52
 10  \w     97.00 173.00   1.00   58.59    --  106.06 125.00-120.00   76
 11  \w    104.00 156.00   1.00   58.59    --  106.06  77.00   0.00   52
 12  \w     81.00 122.00   1.00   58.59    --  106.06  45.00 -60.00   41
 13  \w     97.00 145.00   1.00   58.59    --  106.06 125.00-150.00   48
;
_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      0.0085960000
_diffrn_orient_matrix_UB_12      -0.0029377000
_diffrn_orient_matrix_UB_13      0.0456690000
_diffrn_orient_matrix_UB_21      0.0920840000
_diffrn_orient_matrix_UB_22      0.0206321000
_diffrn_orient_matrix_UB_23      0.0028332000
_diffrn_orient_matrix_UB_31      -0.0650374000
_diffrn_orient_matrix_UB_32      0.0288608000
_diffrn_orient_matrix_UB_33      0.0026386000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            81548
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.473
_diffrn_reflns_theta_min         3.537
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.289
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37880
_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    1.212
_exptl_crystal_description       block
_exptl_crystal_F_000             7269
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.499
_refine_diff_density_min         -1.918
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2052
_refine_ls_number_reflns         38920
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0757
_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^)+(0.1292P)^2^+27.5689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2108
_refine_ls_wR_factor_ref         0.2280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29727
_reflns_number_total             38920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00592e2.cif
_cod_data_source_block           xstr1343_auto
_cod_depositor_comments
'Adding full bibliography for 7247186--7247196.cif.'
_cod_original_cell_volume        19907.9(5)
_cod_original_formula_sum        'C142.20 H117.20 Cd6.80 N19.50 O48'
_cod_database_code               7247187
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C38H35N6O12Cd2
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.254
_diffrn_oxdiff_digest_frames
;
015c8a28e81d165413b925068c25b79d6300027ff4b
;
_diffrn_oxdiff_digest_hkl
;
019b3313a2917488e1151333bffdc3b924ff56
;
_reflns_odcompleteness_completeness 99.82
_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 C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-C26 = N3-C27 = N5-C36 = N5-C37 = N6A-C39A = N6A-C40A = N6B-C39B = N6B-C40B
 1.45 with sigma of 0.002
 N16A-C130 = N16B-C130
 1.34 with sigma of 0.002
 N6A-C38 = N6B-C38
 1.34 with sigma of 0.002
 C142-C141 = C140-C139
 1.54 with sigma of 0.002
 N19-C140 = N20-C142
 1.12 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C40B) \\sim Ueq, Uanis(N6B) \\sim Ueq, Uanis(N6A) \\sim Ueq, Uanis(C39A)
\\sim Ueq, Uanis(C39B) \\sim Ueq, Uanis(C40A) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(O17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C130) \\sim Ueq, Uanis(O46) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C131)
\\sim Ueq, Uanis(N16B) \\sim Ueq, Uanis(N16A) \\sim Ueq, Uanis(C0AA) \\sim Ueq,
Uanis(C132) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C141) \\sim Ueq, Uanis(C142) \\sim Ueq, Uanis(N20) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C140) \\sim Ueq, Uanis(C139) \\sim Ueq, Uanis(N19) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O13B) = Uanis(O13A) = Uanis(C28) = Uanis(O12)
Uanis(O19A) = Uanis(O19B)
Uanis(O4) = Uanis(C2) = Uanis(O5)
Uanis(O37) = Uanis(C100) = Uanis(O36)
4. Others
 Fixed Sof: Cd5(0.8) O3A(0.5) O3B(0.5) O13A(0.5) O13B(0.5) O19A(0.6) O19B(0.4)
 N6A(0.5) N6B(0.5) N16A(0.5) N16B(0.5) C0AA(0.5) C1A(0.5) H1A(0.5) C1B(0.5)
 H1BA(0.5) H1BB(0.5) C30A(0.7) H30A(0.7) C30B(0.5) H30B(0.5) C31A(0.5)
 H31A(0.5) C31B(0.5) H31B(0.5) H38(0.5) H38A(0.5) C39A(0.5) H39A(0.5) H39B(0.5)
 H39C(0.5) C39B(0.5) H39D(0.5) H39E(0.5) H39F(0.5) C40A(0.5) H40A(0.5)
 H40B(0.5) H40C(0.5) C40B(0.5) H40D(0.5) H40E(0.5) H40F(0.5) C95A(0.7)
 H95A(0.7) C95B(0.3) H95B(0.3) C96A(0.7) H96A(0.7) C96B(0.3) H96B(0.3)
 H130(0.5) C131(0.5) H13B(0.5) H13C(0.5) H13D(0.5) C132(0.5) H13E(0.5)
 H13F(0.5) H13G(0.5) C133(0.5) N19(0.5) C139(0.5) H13Q(0.5) H13R(0.5) H13S(0.5)
 C140(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N4(H4), N7(H7), N8(H8), N9(H9), N10(H10), N11(H11), N12(H12),
 N13(H13), N14(H14), N15(H15), C1A(H1A), C4(H4A), C5(H5), C7(H7A), C8(H8A),
 C11(H11A), C13(H13A), C15(H15A), C19(H19), C20(H20), C22(H22), C23(H23),
 C25(H25), C30A(H30A), C30B(H30B), C31A(H31A), C31B(H31B), C33(H33), C34(H34),
 C35(H35), C38(H38), C38(H38A), C43(H43), C44(H44), C46(H46), C47(H47),
 C50(H50), C52(H52), C54(H54), C57(H57), C58(H58), C60(H60), C61(H61), C65(H65),
  C66(H66), C68(H68), C69(H69), C73(H73), C74(H74), C76(H76), C77(H77),
 C80(H80), C82(H82), C84(H84), C87(H87), C88(H88), C90(H90), C91(H91),
 C95A(H95A), C95B(H95B), C96A(H96A), C96B(H96B), 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), C130(H130), C138(H138), C135(H135)
5.b X=CH2 refined with riding coordinates:
 C1B(H1BA,H1BB)
5.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C39A(H39A,H39B,H39C), C39B(H39D,H39E,H39F), C40A(H40A,H40B,H40C),
 C40B(H40D,H40E,H40F), C131(H13B,H13C,H13D), C132(H13E,H13F,H13G), C136(H13H,
 H13I,H13J), C137(H13K,H13L,H13M), C2AA(H2AA,H2AB,H2AC), C134(H13N,H13O,H13P),
 C139(H13Q,H13R,H13S), C141(H14A,H14B,H14C)
;
_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 1.970
_oxdiff_exptl_absorpt_empirical_full_min 0.663