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_7247195
_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 H114 Cd6.9 N25 O38.9, 2.25(C3 H6 O), 0.5(C3 H7 N O)'
_chemical_formula_sum            'C161.75 H131 Cd6.9 N25.5 O41.65'
_chemical_formula_weight         3873.87
_chemical_name_systematic        xstr1386
_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             2022-10-22
_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                 93.6969(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9412(2)
_cell_length_b                   42.7238(4)
_cell_length_c                   33.8725(4)
_cell_measurement_reflns_used    66192
_cell_measurement_temperature    156(9)
_cell_measurement_theta_max      73.4820
_cell_measurement_theta_min      3.6880
_cell_volume                     21577.3(4)
_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      156(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_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   -110.10 -18.00   0.30    0.80    --  -42.62 -38.00 -90.00  307
  2  \w    -67.00  30.20   0.30    0.80    --  -42.62  38.00  90.00  324
  3  \w    -85.00 -58.00   0.30    0.80    --  -42.62 125.00 120.00   90
  4  \w    -71.00  30.10   0.30    0.80    --  -42.62  57.00-150.00  337
  5  \w      9.00  34.80   0.30    0.80    --   42.62 -99.00-180.00   86
  6  \w     53.00  96.20   0.30    0.80    --   42.62-125.00   0.00  144
  7  \w     32.00 123.20   0.30    3.17    --  106.06 -30.00-180.00  304
  8  \w     47.00 111.20   0.30    3.17    --  106.06-125.00-180.00  214
  9  \w     47.00 109.10   0.30    3.17    --  106.06 -45.00   0.00  207
 10  \w     28.00 152.20   0.30    3.17    --  106.06 -15.00   0.00  414
 11  \w     24.80 107.00   0.30    3.17    --  106.06 -94.00-150.00  274
 12  \w     27.00 102.00   0.30    3.17    --  106.06 -94.00  30.00  250
 13  \w    128.00 158.00   0.30    3.17    --  106.06  77.00-180.00  100
 14  \w     80.00 107.00   0.30    3.17    --  106.06 -94.00  60.00   90
 15  \w     55.00  80.20   0.30    3.17    --  106.06-125.00 -60.00   84
 16  \w     34.00  80.20   0.30    3.17    --  106.06-125.00-150.00  154
 17  \w     29.00 107.00   0.30    3.17    --  106.06 -94.00 -30.00  260
 18  \w     76.00 107.20   0.30    3.17    --  106.06-107.00-150.74  104
 19  \w     83.00 170.00   0.30    3.17    --  106.06  45.00   0.00  290
 20  \w     56.00 107.00   0.30    3.17    --  106.06-105.00 -52.54  170
;
_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      -0.0109497000
_diffrn_orient_matrix_UB_12      -0.0181455000
_diffrn_orient_matrix_UB_13      -0.0393241000
_diffrn_orient_matrix_UB_21      0.1014681000
_diffrn_orient_matrix_UB_22      -0.0068544000
_diffrn_orient_matrix_UB_23      0.0024641000
_diffrn_orient_matrix_UB_31      -0.0163779000
_diffrn_orient_matrix_UB_32      -0.0303722000
_diffrn_orient_matrix_UB_33      0.0229421000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            170414
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.517
_diffrn_reflns_theta_min         3.474
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.896
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59328
_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    1.192
_exptl_crystal_description       block
_exptl_crystal_F_000             7778
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.939
_refine_diff_density_min         -2.327
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       0.000084(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2063
_refine_ls_number_reflns         42834
_refine_ls_number_restraints     358
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.1101
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1189P)^2^+241.4091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2867
_refine_ls_wR_factor_ref         0.2931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                37419
_reflns_number_total             42834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00592e2.cif
_cod_data_source_block           xstr1386_auto
_cod_depositor_comments
'Adding full bibliography for 7247186--7247196.cif.'
_cod_original_cell_volume        21577.4(5)
_cod_original_formula_sum        'C161.75 H131 Cd6.90 N25.50 O41.65'
_cod_database_code               7247195
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         Cd7C130H110N20O30
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.320
_diffrn_oxdiff_digest_frames
;
0136228bbbbfbfe5db2f6998b9e27c2697000295d5b
;
_diffrn_oxdiff_digest_hkl
;
017959c8f45ee36fedefc7fba22ae9d76e914c
;
_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 H(H,H) groups, All C(H) groups, All N(H) groups, All N(H,H) groups, All
  N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cd7-O17
 2.5 with sigma of 0.02
 C174-C175 = C175-C176
 1.54 with sigma of 0.02
 O43-C175
 1.2 with sigma of 0.02
 C171-C172 = C172-C173
 1.54 with sigma of 0.02
 O42-C172
 1.2 with sigma of 0.02
 C169-C168 = C170-C168
 1.54 with sigma of 0.02
 O41-C168
 1.2 with sigma of 0.02
 N29-C163 = N29-C162
 1.45 with sigma of 0.002
 N29-C164
 1.34 with sigma of 0.002
 O44-C164
 1.23 with sigma of 0.002
 C25-N2
 2.3 with sigma of 0.002
 C176-C175 = C175-C174 = C172-C171 = C173-C172 = C169-C168 = C170-C168 = C167-
 C165 = C166-C165
 1.54 with sigma of 0.002
 O43-C175 = O42-C172 = O41-C168 = O40-C165
 1.23 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
O41 \\sim C168 \\sim C169 \\sim C170 \\sim C165 \\sim O40 \\sim C167 \\sim
C166: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
N22 \\sim C99: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
N21 \\sim C101 \\sim C100 \\sim C99 \\sim C98 \\sim C97 \\sim N22: 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(C174) \\sim Ueq, Uanis(O43)
\\sim Ueq, Uanis(C173) \\sim Ueq, Uanis(C172) \\sim Ueq, Uanis(C171) \\sim Ueq,
Uanis(O42) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C170) \\sim Ueq, Uanis(C168) \\sim Ueq, Uanis(C169) \\sim Ueq, Uanis(O41)
\\sim Ueq, Uanis(C165) \\sim Ueq, Uanis(C166) \\sim Ueq, Uanis(O40) \\sim Ueq,
Uanis(C167) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C163) \\sim Ueq, Uanis(N29) \\sim Ueq, Uanis(C164) \\sim Ueq, Uanis(C162)
\\sim Ueq, Uanis(O44) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(N14B) \\sim Ueq, Uanis(N15B) \\sim Ueq, Uanis(N15A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C28) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(N2) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N14A) \\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(N12) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(N13) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N10) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1B) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uiso(C98) = Uiso(C97) = Uiso(C100) = Uiso(C101) = Uiso(C99)
Uanis(C61A) = Uanis(C60A) = Uanis(C59A) = Uanis(C58A) = Uanis(C57A)
Uanis(C61B) = Uanis(C60B) = Uanis(C59A) = Uanis(C58B) = Uanis(C57B)
Uanis(C22) = Uanis(C21)
Uanis(C21) = Uanis(C22)
Uanis(C67B) = Uanis(C67A) = Uanis(O13A) = Uanis(O13B)
Uanis(C65) = Uanis(C66) = Uanis(N16) = Uanis(C62) = Uanis(C63) = Uanis(C64) =
Uanis(N17)
Uanis(O11A) = Uanis(O11B)
Uanis(O2) = Uanis(O1)
Uanis(C1) = Uanis(O8) = Uanis(O7)
Uanis(N8) = Uanis(C51) = Uanis(C50) = Uanis(C49) = Uanis(C48) = Uanis(C47) =
Uanis(N9)
Uanis(N12) = Uanis(C52) = Uanis(C53) = Uanis(C54) = Uanis(C55) = Uanis(C56) =
Uanis(N13)
Uanis(N1) = Uanis(C24) = Uanis(C25) = Uanis(C26) = Uanis(C27) = Uanis(C28) =
Uanis(N2)
Uanis(N10) = Uanis(C46) = Uanis(C45) = Uanis(C44) = Uanis(C43) = Uanis(C42) =
Uanis(N11)
Uiso(N22) = Uiso(C99) = Uiso(C98) = Uiso(C97) = Uiso(N21) = Uiso(C101) =
Uiso(C100)
4. Others
 Fixed Sof: Cd5A(0.65) Cd5B(0.35) Cd7(0.9) O11A(0.6) O11B(0.4) O13A(0.5)
 O13B(0.4) N1(0.5) C24(0.5) H24(0.5) C25(0.5) H25(0.5) C26(0.5) C27(0.5)
 H27(0.5) C28(0.5) H28(0.5) N2(0.5) H2A(0.5) H2B(0.5) N9(0.5) H9A(0.5) H9B(0.5)
 H9C(0.5) N12(0.5) C56(0.5) H56(0.5) C55(0.5) H55(0.5) C54(0.5) C53(0.5)
 H53(0.5) C52(0.5) H52(0.5) N13(0.5) H13A(0.5) H13B(0.5) N14A(0.5) N14B(0.5)
 N15A(0.5) H15A(0.5) H15B(0.5) H15C(0.5) N15B(0.5) H15D(0.5) H15E(0.5)
 C1A(0.25) H1A(0.25) C1B(0.25) H1B(0.25) C51(0.5) H51(0.5) C50(0.5) H50(0.5)
 C49(0.5) C48(0.5) H48(0.5) C47(0.5) H47(0.5) N8(0.5) C57A(0.5) H57A(0.5)
 C57B(0.5) H57B(0.5) C58A(0.5) H58A(0.5) C58B(0.5) H58B(0.5) C59A(0.5)
 C59B(0.5) C60A(0.5) H60A(0.5) C60B(0.5) H60B(0.5) C61A(0.5) H61A(0.5)
 C61B(0.5) H61B(0.5) C67A(0.6) C67B(0.4) C159(0.75) H159(0.75) C160(0.75)
 H160(0.75) O40(0.5) C165(0.5) C166(0.5) H16G(0.5) H16H(0.5) H16I(0.5)
 C167(0.5) H16J(0.5) H16K(0.5) H16L(0.5) O41(0.5) C168(0.5) C169(0.5) H16M(0.5)
 H16N(0.5) H16O(0.5) C170(0.5) H17C(0.5) H17D(0.5) H17E(0.5) O42(0.75)
 C171(0.75) H17F(0.75) H17G(0.75) H17H(0.75) C172(0.75) C173(0.75) H17I(0.75)
 H17J(0.75) H17K(0.75) O43(0.5) C174(0.5) H17L(0.5) H17M(0.5) H17N(0.5)
 C175(0.5) C176(0.5) H17O(0.5) H17P(0.5) H17Q(0.5) O44(0.5) N29(0.5) C162(0.5)
 H16A(0.5) H16B(0.5) H16C(0.5) C163(0.5) H16D(0.5) H16E(0.5) H16F(0.5)
 C164(0.5) H164(0.5)
 Fixed Uiso: H9A(0.08997) N21(0.10391) C101(0.10391) C100(0.10391)
 C99(0.10391) C98(0.10391) C97(0.10391) N22(0.10391)
5.a Rotating group:
 N2(H2A,H2B), N4(H4A,H4B), N13(H13A,H13B), N15B(H15D,H15E), N17(H17A,H17B)
5.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C27(H27), C28(H28), N5(H5), N6(H6), N7(H7), C56(H56),
 C55(H55), C53(H53), C52(H52), N18(H18), N19(H19), N20(H20), C101(H101),
 C100(H100), C98(H98), C97(H97), N23(H23), N24(H24A), N25(H25A), N26(H26),
 N27(H27A), N28(H28A), C1(H1), C1A(H1A), C1B(H1B), C4(H4), C5(H5A), C7(H7A),
 C8(H8), C11(H11), C13(H13), C15(H15), C18(H18A), C19(H19A), C21(H21), C22(H22),
  C29(H29), C30(H30), C32(H32), C33(H33), C36(H36), C37(H37), C39(H39),
 C40(H40), C45(H45), C43(H43), C42(H42), C46(H46), C51(H51), C50(H50), C48(H48),
  C47(H47), C57A(H57A), C57B(H57B), C58A(H58A), C58B(H58B), C60A(H60A),
 C60B(H60B), C61A(H61A), C61B(H61B), C62(H62), C63(H63), C65(H65), C66(H66),
 C69(H69), C70(H70), C72(H72), C73(H73), C76(H76), C78(H78), C80(H80), C83(H83),
  C84(H84), C86(H86), C87(H87), C91(H91), C92(H92), C94(H94), C95(H95),
 C104(H104), C105(H105), C107(H107), C108(H108), C111(H111), C113(H113),
 C115(H115), C118(H118), C119(H119), C121(H121), C122(H122), C126(H126),
 C127(H127), C129(H129), C130(H130), C134(H134), C135(H135), C137(H137),
 C138(H138), C141(H141), C143(H143), C145(H145), C148(H148), C149(H149),
 C151(H151), C152(H152), C156(H156), C157(H157), C159(H159), C160(H160),
 C164(H164)
5.c Fitted hexagon refined as free rotating group:
 N1(C24,C25,C26,C27,C28), N12(C56,C55,C54,C53,C52), N21(C101,C100,C99,C98,C97),
  C45(C44,C43,C42,N10,C46), C51(C50,C49,C48,C47,N8)
5.d X=CH2 refined with riding coordinates:
 N11(H11A,H11B)
5.e Idealised Me refined as rotating group:
 N9(H9A,H9B,H9C), N15A(H15A,H15B,H15C), N22(H22A,H22B,H22C), C166(H16G,H16H,
 H16I), C167(H16J,H16K,H16L), C169(H16M,H16N,H16O), C170(H17C,H17D,H17E),
 C171(H17F,H17G,H17H), C173(H17I,H17J,H17K), C174(H17L,H17M,H17N), C176(H17O,
 H17P,H17Q), C162(H16A,H16B,H16C), C163(H16D,H16E,H16F)
;
_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 1.726
_oxdiff_exptl_absorpt_empirical_full_min 0.751