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_7247188
_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
'C153.5 H107.5 Cd7 N19 O40, 6(C3 H6 O), 0.25(C8 H11 N)'
_chemical_formula_sum            'C173.5 H146.25 Cd7 N19.25 O46'
_chemical_formula_weight         4023.64
_chemical_name_systematic        xstr1407
_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             2022-08-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-06-12 deposited with the CCDC.	2023-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7053(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1427(3)
_cell_length_b                   43.1990(6)
_cell_length_c                   33.7991(4)
_cell_measurement_reflns_used    27817
_cell_measurement_temperature    158(11)
_cell_measurement_theta_max      73.3860
_cell_measurement_theta_min      3.9850
_cell_volume                     20580.0(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (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      158(11)
_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 0.965
_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    -83.00  -9.00   1.00   12.02    --  -43.17 125.00 -30.00   74
  2  \w    -65.00  29.00   1.00   12.02    --  -43.17  38.00 -60.00   94
  3  \w     10.00  40.00   1.00   12.02    --   43.17 -99.00 -60.00   30
  4  \w     38.00  79.00   1.00   12.02    --   43.17 -99.00 -90.00   41
  5  \w     39.00  66.00   1.00   48.06    --  105.83 -61.00-180.00   27
  6  \w    108.00 133.00   1.00   48.06    --  105.83 -61.00-180.00   25
  7  \w    118.00 151.00   1.00   48.06    --  105.83 125.00 150.00   33
  8  \w     41.00 136.00   1.00   48.06    --  105.83 -77.00  60.00   95
  9  \w     82.00 142.00   1.00   48.06    --  105.83  45.00  30.00   60
 10  \w     80.00 172.00   1.00   48.06    --  105.83  61.00 -30.00   92
 11  \w     48.00 137.00   1.00   48.06    --  105.83 -77.00-120.00   89
;
_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      0.0854327000
_diffrn_orient_matrix_UB_12      -0.0202576000
_diffrn_orient_matrix_UB_13      -0.0088079000
_diffrn_orient_matrix_UB_21      0.0668896000
_diffrn_orient_matrix_UB_22      0.0277622000
_diffrn_orient_matrix_UB_23      0.0086329000
_diffrn_orient_matrix_UB_31      0.0132801000
_diffrn_orient_matrix_UB_32      -0.0094973000
_diffrn_orient_matrix_UB_33      0.0440428000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            83443
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.736
_diffrn_reflns_theta_min         3.453
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.288
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (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    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             8104
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         5.109
_refine_diff_density_min         -2.444
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2103
_refine_ls_number_reflns         40194
_refine_ls_number_restraints     250
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0886
_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^)+(0.1390P)^2^+99.2887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2398
_refine_ls_wR_factor_ref         0.2594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29576
_reflns_number_total             40194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00592e2.cif
_cod_data_source_block           xstr1407_auto
_cod_depositor_comments
'Adding full bibliography for 7247186--7247196.cif.'
_cod_original_formula_sum        'C173.50 H146.25 Cd7 N19.25 O46'
_cod_database_code               7247188
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         Cd7C150H110N25O35
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.326
_diffrn_oxdiff_digest_frames
;
01980541ef50674718361a5f4f87bc324300027fe6b
;
_diffrn_oxdiff_digest_hkl
;
01f999a32d950966359f2accc36fcd2feeb624
;
_reflns_odcompleteness_completeness 99.80
_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 H(H,H) groups, All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N20-C184 = N20-C185
 1.45 with sigma of 0.02
 C172-C174 = C172-C173
 1.54 with sigma of 0.02
 O47-C175
 2.3 with sigma of 0.02
 C160-C162 = C160-C161 = C166-C168 = C166-C167 = C159-C157 = C157-C158 = C170-
 C169 = C169-C171 = C163-C165 = C164-C163 = C172-C174 = C172-C173 = C176-C175 =
 C176-C177
 1.54 with sigma of 0.02
 C176-C177 = C176-C175
 1.54 with sigma of 0.02
 C166-C167 = C166-C168
 1.54 with sigma of 0.02
 C159-C157 = C158-C157 = C167-C166 = C168-C166 = C161-C160 = C162-C160 = C165-
 C163 = C164-C163 = C170-C169 = C171-C169 = C176-C175 = C177-C176 = C173-C172 =
 C174-C172
 1.54 with sigma of 0.002
 O43-C166 = O44-C160 = O41-C157 = O42-C169 = O46-C172 = O45-C163 = O47-C176
 1.23 with sigma of 0.002
 Cd5-N10
 2.3 with sigma of 0.002
 O46-C173
 2.4 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C81 \\sim N10 \\sim C77 \\sim C78 \\sim C79 \\sim C80: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
Uanis(C176) \\sim Ueq, Uanis(C175) \\sim Ueq, Uanis(O47) \\sim Ueq, Uanis(C177)
\\sim Ueq, Uanis(C173) \\sim Ueq, Uanis(C172) \\sim Ueq, Uanis(C174) \\sim Ueq,
Uanis(O46) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C165) \\sim Ueq, Uanis(C163) \\sim Ueq, Uanis(C164) \\sim Ueq, Uanis(O45)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N11) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C84)
\\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C82) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(O41) \\sim Ueq, Uanis(C157) \\sim Ueq, Uanis(C159) \\sim Ueq, Uanis(C158)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N10) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C79)
\\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(N1) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(C2) = Uanis(C1)
Uanis(C169) = Uanis(C171) = Uanis(C170) = Uanis(O42)
Uanis(N20) = Uanis(C185) = Uanis(C184) = Uanis(C183) = Uanis(C178) =
Uanis(C182) = Uanis(C179) = Uanis(C181) = Uanis(C180)
Uanis(N2) = Uanis(C41A) = Uanis(C40A) = Uanis(C40B) = Uanis(C41B) = Uanis(C39)
= Uanis(C38) = Uanis(C37)
Uanis(O32) = Uanis(C122) = Uanis(O33)
Uanis(C81) = Uanis(N10) = Uanis(C77) = Uanis(C78) = Uanis(C79) = Uanis(C80)
4. Others
 Fixed Sof: C1(0.5) H1(0.5) C2(0.5) H2(0.5) C3(0.5) H3A(0.5) C4(0.5) H4A(0.5)
 C5(0.5) H5A(0.5) H39(0.65) H39A(0.35) C41B(0.65) H41B(0.65) C40B(0.65)
 H40B(0.65) C172(0.5) C174(0.5) H0AA(0.5) H1AA(0.5) H2AA(0.5) C173(0.5)
 H3AA(0.5) H4AA(0.5) H5AA(0.5) C185(0.25) H6AA(0.25) H7AA(0.25) H8AA(0.25)
 N20(0.25) C184(0.25) H9AA(0.25) H0BA(0.25) H1BA(0.25) O47(0.5) C176(0.5)
 C175(0.5) H5BA(0.5) H6BA(0.5) H7BA(0.5) C177(0.5) H8BA(0.5) H9BA(0.5)
 H0CA(0.5) C183(0.25) C178(0.25) H1CA(0.25) C179(0.25) H2CA(0.25) C180(0.25)
 H3CA(0.25) C181(0.25) H4CA(0.25) C182(0.25) H5CA(0.25) O46(0.5) C40A(0.35)
 H40A(0.35) C41A(0.35) H41A(0.35)
 Fixed Uiso: H9AA(0.14573)
5.a Rotating group:
 O22(H22A,H22B)
5.b Aromatic/amide H refined with riding coordinates:
 N8(H8), N16(H16), N6(H6), N3(H3), N15(H15), N14(H14), N18(H18), C87(H87),
 C88(H88), C89(H89), C90(H90), C91(H91), N7(H7), N5(H5), N17(H17), N13(H13),
 N4(H4), C51(H51), C150(H150), C15(H15A), C133(H133), C103(H103), C131(H131),
 C101(H101), C105(H105), C19(H19), C55(H55), C17(H17A), C108(H108), C53(H53),
 C135(H135), C23(H23), C149(H149), C142(H142), C47(H47), C98(H98), C48(H48),
 C22(H22), C45(H45), C44(H44), C139(H139), C9(H9), C138(H138), C33(H33),
 C36(H36), C34(H34), C12(H12), C141(H141), C59(H59), C66(H66), C97(H97),
 C112(H112), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C58(H58),
 C61(H61), C30(H30), C1(H1), C2(H2), C3(H3A), C4(H4A), C5(H5A), C120(H120),
 C125(H125), C11(H11), C69(H69), C8(H8A), C127(H127), C119(H119), C31(H31),
 C146(H146), C147(H147), C26(H26), C67(H67), C62(H62), C25(H25), C111(H111),
 C128(H128), C109(H109), C94(H94), C70(H70), C116(H116), C95(H95), C117(H117),
 C124(H124), C39(H39), C39(H39A), C86(H86), C82(H82), C83(H83), C84(H84),
 C85(H85), C38(H38), C152(H152), C156(H156), C155(H155), C154(H154), C153(H153),
  C41B(H41B), C40B(H40B), C37(H37), C81(H81), C77(H77), C78(H78), C79(H79),
 C80(H80), C178(H1CA), C179(H2CA), C180(H3CA), C181(H4CA), C182(H5CA),
 C40A(H40A), C41A(H41A)
5.c Fitted hexagon refined as free rotating group:
 N12(C87,C88,C89,C90,C91), N9(C72,C73,C74,C75,C76), N1(C1,C2,C3,C4,C5),
 C86(N11,C82,C83,C84,C85), C152(N19,C156,C155,C154,C153), C81(N10,C77,C78,C79,
 C80), C183(C178,C179,C180,C181,C182)
5.d Idealised Me refined as rotating group:
 C168(H,HA,HB), C161(HC,HD,HE), C164(HF,HG,HH), C159(HI,HJ,HK), C158(HL,HM,HN),
  C165(HO,HP,HQ), C170(HR,HS,HT), C167(HU,HV,HW), C171(HX,HY,HZ), C174(H0AA,
 H1AA,H2AA), C173(H3AA,H4AA,H5AA), C185(H6AA,H7AA,H8AA), C184(H9AA,H0BA,H1BA),
 C162(H2BA,H3BA,H4BA), C175(H5BA,H6BA,H7BA), C177(H8BA,H9BA,H0CA)
;
_olex2_submission_original_sample_id xstr1407
_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 1.621
_oxdiff_exptl_absorpt_empirical_full_min 0.658