Self-assembled orthoester cryptands: orthoester scope, post-functionalization, kinetic locking and tunable degradation kinetics.
Löw, Henrik; Mena-Osteritz, Elena; von Delius, Max; Chemical science 9 (2018) 4785–4793; doi:10.1039/c8sc01750f

data_1549314
_publ_section_title
;
 Self-assembled orthoester cryptands: orthoester scope,
 post-functionalization, kinetic locking and tunable degradation kinetics.
;
_journal_issue                   21
_journal_name_full               'Chemical science'
_journal_page_first              4785
_journal_page_last               4793
_journal_paper_doi               10.1039/c8sc01750f
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C26 H34 Na O9, C32 H12 B F24'
_chemical_formula_sum            'C58 H46 B F24 Na O9'
_chemical_formula_weight         1376.75
_chemical_name_systematic
'(1,9-diphenyl-2,5,8,10,13,16,17,20,23-nonaoxabicyclo[7.7.7]tricosane)-sodium tetrakis(3,5-bis(trifluoromethyl)phenyl)borate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-06 deposited with the CCDC.
2018-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.142(4)
_cell_length_b                   24.665(5)
_cell_length_c                   26.029(6)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.65
_cell_volume                     12289(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      149.96
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            80330
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.019
_diffrn_reflns_theta_min         2.065
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6847
_exptl_absorpt_correction_type   none
_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    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             5584
_exptl_crystal_preparation       'Chloroform solution'
_exptl_crystal_recrystallization_method
'Solvent layering of hexane over chloroform solution'
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.00041(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         13422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0360P)^2^+9.3322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1113
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9548
_reflns_number_total             13422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01750f2.cif
_cod_data_source_block           hl17072_0m
_cod_depositor_comments
'Adding full bibliography for 1549313--1549320.cif.'
_cod_database_code               1549314
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.955
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: F00J(0.5) F00K(0.5) F00R(0.5) F00T(0.5) F00U(0.5) F023(0.5)
 F02I(0.5) F02A(0.5) F02L(0.5) F1(0.5) F2(0.5) F3(0.5) F0AA(0.5) F6(0.5)
 F35(0.5) F2AA(0.5) F1AA(0.5) F5(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,
 H16B), C23(H23A,H23B), C28(H28A,H28B), C32(H32A,H32B), C35(H35A,H35B),
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C18(H18), C20(H20), C21(H21),
 C27(H27), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C42(H42),
  C43(H43), C45(H45), C47(H47), C48(H48), C54(H54), C55(H55)
;
_olex2_exptl_crystal_mounting_method Glowing
_olex2_submission_special_instructions 'No special instructions were received'