Encapsulation of closo-dodecaiodododecaborate in 2-hydroxypropyl-γ-cyclodextrin prevents hemolysis
Hollow, Sophia E.; Johnstone, Timothy C.; Chemical Communications  (2022) –; doi:10.1039/D1CC06348K

data_7129621
_publ_section_title
;
 Encapsulation of closo-dodecaiodododecaborate in
 2-hydroxypropyl-\g-cyclodextrin prevents hemolysis
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06348K
_journal_year                    2022
_chemical_formula_moiety         'B12 I12, 6(C3 H7 N O), Na2, O H2'
_chemical_formula_sum            'C18 H44 B12 I12 N6 Na2 O7'
_chemical_formula_weight         2155.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-11-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-11-10 deposited with the CCDC.	2022-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.8693(6)
_cell_length_b                   22.9629(4)
_cell_length_c                   19.7457(3)
_cell_measurement_reflns_used    52718
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      31.0400
_cell_measurement_theta_min      2.1960
_cell_volume                     13089.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -59.00  10.00   0.50   20.00    --   -5.10 -57.00 120.00  138
  2  \w     -6.00  23.00   0.50   20.00    --   -5.10  77.00 -30.00   58
  3  \w    -52.00  66.00   0.50   20.00    --   -5.10   0.00 -90.00  236
  4  \w    -17.00  24.00   0.50   20.00    --    5.18  77.00-120.00   82
  5  \w    -17.00  23.00   0.50   20.00    --    5.18  77.00 120.00   80
  6  \w      2.00  28.00   0.50   20.00    --    5.18 -77.00 -60.00   52
  7  \w    -61.00  -1.00   0.50   20.00    --    5.18 -19.00  30.00  120
  8  \w    -19.00  28.00   0.50   20.00    --    5.18 -77.00  30.00   94
  9  \w    -25.00   6.00   0.50   20.00    --    5.18 -77.00-180.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0230702000
_diffrn_orient_matrix_UB_12      -0.0097501000
_diffrn_orient_matrix_UB_13      -0.0049598000
_diffrn_orient_matrix_UB_21      -0.0059168000
_diffrn_orient_matrix_UB_22      -0.0097058000
_diffrn_orient_matrix_UB_23      -0.0330104000
_diffrn_orient_matrix_UB_31      0.0060320000
_diffrn_orient_matrix_UB_32      0.0276469000
_diffrn_orient_matrix_UB_33      -0.0133044000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            174695
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.170
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.724
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.074
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.187
_exptl_crystal_description       plate
_exptl_crystal_F_000             7744
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.035
_refine_diff_density_min         -1.716
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         12413
_refine_ls_number_restraints     612
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+342.3536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9776
_reflns_number_total             12413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06348k2.cif
_cod_data_source_block           tcj00095_man
_cod_database_code               7129621
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.366
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained planarity
 O81, C81, C82, C83
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Na1 \\sim Na2 \\sim Na3 \\sim Na4 \\sim N31 \\sim O31 \\sim C31 \\sim C32 \\sim
C33 \\sim N41 \\sim O41 \\sim C41 \\sim C42 \\sim C43 \\sim N51 \\sim O51 \\sim
C51 \\sim C52 \\sim C53 \\sim N61 \\sim O61 \\sim C61 \\sim C62 \\sim C63 \\sim
N21 \\sim O21 \\sim C21 \\sim C22 \\sim C23 \\sim N11 \\sim O11 \\sim C11 \\sim
C12 \\sim C13 \\sim O1 \\sim O2 \\sim N71 \\sim O71 \\sim C71 \\sim C72 \\sim
C73 \\sim N81 \\sim O81 \\sim C81 \\sim C82 \\sim C83: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 Na1, Na2, Na3, Na4, N31, O31, C31, C32, C33, N41, O41, C41, C42, C43, N51,
 O51, C51, C52, C53, N61, O61, C61, C62, C63, N21, O21, C21, C22, C23, N11, O11,
  C11, C12, C13, O1, O2, N71, O71, C71, C72, C73, N81, O81, C81, C82, C83
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Same fragment restrains
{N31, O31, C31, C32, C33} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21, O21, C21, C22, C23}
{N31, O31, C31, C32, C33} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11, O11, C11, C12, C13}
{N31, O31, C31, C32, C33} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N71, O71, C71, C72, C73}
{N31, O31, C31, C32, C33} sigma for 1-2: 0.002, 1-3: 0.004
as in
{N81, O81, C81, C82, C83}
6. Others
 Fixed Sof: Na2(0.5) Na3(0.5) Na4(0.5) N41(0.5) O41(0.5) C41(0.5) H41(0.5)
 C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5)
 N11(0.5) O11(0.5) C11(0.5) H11(0.5) C12(0.5) H12A(0.5) H12B(0.5) H12C(0.5)
 C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) O1(0.5) H1A(0.5) H1B(0.5) O2(0.5)
 H2A(0.5) H2B(0.5) N71(0.5) O71(0.5) C71(0.5) H71(0.5) C72(0.5) H72A(0.5)
 H72B(0.5) H72C(0.5) C73(0.5) H73A(0.5) H73B(0.5) H73C(0.5) N81(0.5) O81(0.5)
 C81(0.5) H81(0.5) C82(0.5) H82A(0.5) H82B(0.5) H82C(0.5) C83(0.5) H83A(0.5)
 H83B(0.5) H83C(0.5)
7.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B)
7.b Me refined with riding coordinates:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C62(H62A,H62B,H62C), C63(H63A,
 H63B,H63C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C82(H82A,H82B,
 H82C), C83(H83A,H83B,H83C)
7.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C41(H41), C51(H51), C61(H61), C21(H21), C11(H11), C71(H71), C81(H81)
;
_shelx_res_checksum              38678
_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 1.806
_oxdiff_exptl_absorpt_empirical_full_min 0.464