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_7247191
_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
'0.29(C279.5 H205 Cd14 N32 O89.5), 1.43(C3 H7 N O), 1.19(C9 H10 O)'
_chemical_formula_sum            'C94.83 H81.86 Cd4 N10.57 O28.17'
_chemical_formula_weight         2269.85
_chemical_name_systematic        xstr1363
_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             2022-10-11
_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                 93.6760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            7
_cell_length_a                   14.61500(10)
_cell_length_b                   43.0674(3)
_cell_length_c                   33.6023(2)
_cell_measurement_reflns_used    78657
_cell_measurement_temperature    137.4(6)
_cell_measurement_theta_max      73.3720
_cell_measurement_theta_min      3.7970
_cell_volume                     21106.8(2)
_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      137.4(6)
_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 0.983
_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   -108.00 -72.00   0.50    2.75    --  -42.62 -57.00  30.00   72
  2  \w    -80.00  -7.00   0.50    2.75    --  -42.62 125.00   0.00  146
  3  \w    -67.00  32.00   0.50    2.75    --  -42.62  38.00 -60.00  198
  4  \w   -116.00 -19.00   0.50    2.75    --  -42.62 -38.00 120.00  194
  5  \w     19.00  84.00   0.50    2.75    --   42.62 -99.00 -30.00  130
  6  \w    111.00 175.00   0.50   10.97    --  106.06  77.00  60.00  128
  7  \w     34.00  61.00   0.50   10.97    --  106.06-125.00-150.00   54
  8  \w     18.00 177.00   0.50   10.97    --  106.06   0.00  60.00  318
  9  \w     75.00 109.00   0.50   10.97    --  106.06-125.00 -90.00   68
 10  \w    116.00 166.00   0.50   10.97    --  106.06 125.00 150.00  100
 11  \w     46.00 123.00   0.50   10.97    --  106.06 -45.00   0.00  154
 12  \w     39.00  69.00   0.50   10.97    --  106.06-125.00   0.00   60
 13  \w     87.00 112.00   0.50   10.97    --  106.06-125.00   0.00   50
 14  \w     65.00 132.00   0.50   10.97    --  106.06 -77.00-120.00  134
 15  \w     31.00 108.00   0.50   10.97    --  106.06-102.00 161.24  154
 16  \w     28.00  54.00   0.50   10.97    --  106.06-103.00  21.00   52
 17  \w     80.00 106.00   0.50   10.97    --  106.06-103.00  21.00   52
 18  \w     35.00 113.00   0.50   10.97    --  106.06 -45.00 150.00  156
 19  \w     69.00 109.00   0.50   10.97    --  106.06-110.00 107.00   80
;
_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      -0.0108506000
_diffrn_orient_matrix_UB_12      0.0100168000
_diffrn_orient_matrix_UB_13      -0.0440660000
_diffrn_orient_matrix_UB_21      0.0342599000
_diffrn_orient_matrix_UB_22      0.0327899000
_diffrn_orient_matrix_UB_23      0.0116605000
_diffrn_orient_matrix_UB_31      0.0993120000
_diffrn_orient_matrix_UB_32      -0.0101987000
_diffrn_orient_matrix_UB_33      -0.0057575000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            152041
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.646
_diffrn_reflns_theta_min         3.534
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.135
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60493
_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    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             7995
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.436
_refine_diff_density_min         -1.664
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2021
_refine_ls_number_reflns         41905
_refine_ls_number_restraints     1797
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1033P)^2^+110.1722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2080
_refine_ls_wR_factor_ref         0.2136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                37505
_reflns_number_total             41905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00592e2.cif
_cod_data_source_block           xstr1363_auto
_cod_depositor_comments
'Adding full bibliography for 7247186--7247196.cif.'
_cod_database_code               7247191
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C130H110N20O20Cd7
_diffrn_oxdiff_digest_frames
;
019d3a3bb2e51c14baab3f9c8743ae7b1a00028a87b
;
_diffrn_oxdiff_digest_hkl
;
01d77f0a2a0ad2df0edb8039e1a37f9a5bf295
;
_reflns_odcompleteness_completeness 99.95
_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
 C159-C158 = C158-C157 = C157-C156 = C156-C155 = C160-C155 = C160-C159
 1.34 with sigma of 0.02
 N4-C31 = N4-C32 = N8-C66 = N8-C65 = N12-C100 = N12-C99 = N13-C103 = N13-C102 =
  N17-C139 = N17-C138 = N19-C141 = N19-C142
 1.45 with sigma of 0.002
 N4-C30 = N19-C140 = N8-C64 = N17-C137 = N12-C98 = N13-C101
 1.34 with sigma of 0.002
 O8-C30 = O47-C140 = O46-C137 = O31-C98 = O36-C101
 1.23 with sigma of 0.002
 C64-O21
 1.23 with sigma of 0.02
 O21-C64
 1.23 with sigma of 0.002
 N18-C135 = N18-C136
 1.45 with sigma of 0.002
 N18-C134
 1.34 with sigma of 0.002
 O48-C134
 1.23 with sigma of 0.002
 O33-C145 = O49-C154 = O50-C163 = O51-C172
 1.23 with sigma of 0.002
 C144-C143 = C145-C144 = C146-C145 = C155-C154 = C154-C153 = C153-C152 = C162-
 C161 = C163-C162 = C164-C163 = C173-C172 = C172-C171 = C171-C170
 1.54 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C139) \\sim Ueq, Uanis(N17) \\sim Ueq, Uanis(C137) \\sim Ueq, Uanis(O46)
\\sim Ueq, Uanis(C138) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C135) \\sim Ueq, Uanis(N18) \\sim Ueq, Uanis(C136) \\sim Ueq, Uanis(C134)
\\sim Ueq, Uanis(O48) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(N13) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(O36) \\sim Ueq, Uanis(C103)
\\sim Ueq, Uanis(C102) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C158) \\sim Ueq, Uanis(C159) \\sim Ueq, Uanis(C160) \\sim Ueq,
Uanis(C155) \\sim Ueq, Uanis(C156) \\sim Ueq, Uanis(C157) \\sim Ueq,
Uanis(C154) \\sim Ueq, Uanis(O49) \\sim Ueq, Uanis(C153) \\sim Ueq, Uanis(C152)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C32) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(O8)
\\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(O51) = Uanis(C174) = Uanis(C173) = Uanis(C175) = Uanis(C172) =
Uanis(C178) = Uanis(C176) = Uanis(C171) = Uanis(C177)
Uanis(C158) = Uanis(O49) = Uanis(C154) = Uanis(C153) = Uanis(C155) =
Uanis(C152) = Uanis(C160) = Uanis(C156) = Uanis(C159) = Uanis(C157)
Uanis(C161) = Uanis(O50) = Uanis(C163) = Uanis(C162) = Uanis(C164) =
Uanis(C169) = Uanis(C165) = Uanis(C168) = Uanis(C166) = Uanis(C167)
Uanis(C143) = Uanis(C144) = Uanis(C145) = Uanis(O33) = Uanis(C147) =
Uanis(C146) = Uanis(C148) = Uanis(C149) = Uanis(C150) = Uanis(C151)
Uanis(N13) = Uanis(C101) = Uanis(O36) = Uanis(C102) = Uanis(C103)
Uanis(C65) = Uanis(N8) = Uanis(C64) = Uanis(O21) = Uanis(C66)
Uanis(N19) = Uanis(C140) = Uanis(O47) = Uanis(C142) = Uanis(C141)
Uanis(C170) = Uanis(C171) = Uanis(C172) = Uanis(O51) = Uanis(C173) =
Uanis(C178) = Uanis(C176) = Uanis(C177) = Uanis(C175) = Uanis(C174)
4. Others
 Fixed Sof: Cd5A(0.5) Cd5B(0.5) O30A(0.5) O30B(0.5) O33(0.75) O34A(0.5)
 O34B(0.5) C1A(0.75) H1A(0.75) C1B(0.75) H1B(0.75) C120(0.25) H120(0.25)
 C121(0.25) H121(0.25) C143(0.75) H14B(0.75) H14C(0.75) H14D(0.75) C144(0.75)
 H14E(0.75) H14F(0.75) C145(0.75) C149(0.75) H149(0.75) C148(0.75) H148(0.75)
 C147(0.75) H147(0.75) C146(0.75) C151(0.75) H151(0.75) C150(0.75) H150(0.75)
 O48(0.5) N18(0.5) C134(0.5) H134(0.5) C135(0.5) H13G(0.5) H13H(0.5) H13I(0.5)
 C136(0.5) H13J(0.5) H13K(0.5) H13L(0.5) O49(0.8) C152(0.8) H15A(0.8) H15B(0.8)
 H15C(0.8) C153(0.8) H15D(0.8) H15E(0.8) C154(0.8) C155(0.8) C160(0.8)
 H160(0.8) C159(0.8) H159(0.8) C158(0.8) H158(0.8) C157(0.8) H157(0.8)
 C156(0.8) H156(0.8) O50(0.75) C161(0.75) H16A(0.75) H16B(0.75) H16C(0.75)
 C162(0.75) H16D(0.75) H16E(0.75) C163(0.75) C166(0.75) H166(0.75) C164(0.75)
 C169(0.75) H169(0.75) C168(0.75) H168(0.75) C167(0.75) H167(0.75) O51(0.5)
 C171(0.5) H17A(0.5) H17B(0.5) C172(0.5) C177(0.5) H177(0.5) C178(0.5)
 H178(0.5) C173(0.5) C174(0.5) H174(0.5) C175(0.5) H175(0.5) C176(0.5)
 H176(0.5) C170(0.5) H17C(0.5) H17D(0.5) H17E(0.5)
 Fixed Uiso: H13G(0.16649) H13H(0.16649) H13I(0.16649)
5.a Secondary CH2 refined with riding coordinates:
 C144(H14E,H14F), C153(H15D,H15E), C162(H16D,H16E), C171(H17A,H17B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N5(H5), N6(H6), N7(H7), N9(H9), N10(H10), N11(H11),
 N14(H14), N15(H15), N16(H16), C1A(H1A), C1B(H1B), C3(H3A), C4(H4), C6(H6A),
 C7(H7A), C10(H10A), C12(H12), C14(H14A), C17(H17), C18(H18), C20(H20),
 C21(H21), C24(H24), C25(H25), C27(H27), C28(H28), C30(H30), C35(H35), C36(H36),
  C38(H38), C39(H39), C42(H42), C44(H44), C46(H46), C49(H49), C50(H50),
 C52(H52), C53(H53), C55(H55), C58(H58), C59(H59), C61(H61), C62(H62), C64(H64),
  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),
  C98(H98), 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), C149(H149),
 C148(H148), C147(H147), C151(H151), C150(H150), C137(H137), C140(H140),
 C134(H134), C160(H160), C159(H159), C158(H158), C157(H157), C156(H156),
 C166(H166), C165(H165), C169(H169), C168(H168), C167(H167), C177(H177),
 C178(H178), C174(H174), C175(H175), C176(H176)
5.c Fitted hexagon refined as free rotating group:
 C149(C148,C147,C146,C151,C150), C155(C160,C159,C158,C157,C156), C166(C165,
 C164,C169,C168,C167), C177(C178,C173,C174,C175,C176)
5.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C66(H66A,H66B,H66C), C99(H99A,H99B,
 H99C), C100(H10B,H10C,H10D), C102(H10E,H10F,H10G), C143(H14B,H14C,H14D),
 C138(H13A,H13B,H13C), C139(H13D,H13E,H13F), C141(H14G,H14H,H14I), C142(H14J,
 H14K,H14L), C135(H13G,H13H,H13I), C136(H13J,H13K,H13L), C152(H15A,H15B,H15C),
 C161(H16A,H16B,H16C), C170(H17C,H17D,H17E)
;
_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 1.650
_oxdiff_exptl_absorpt_empirical_full_min 0.610