Controlling the Recognition and Reactivity of Alkyl Ammonium Guests Using an Anion Coordination-Based Tetrahedral Cage.
Zhang, Wenyao; Yang, Dong; Zhao, Jie; Hou, Lekai; Sessler, Jonathan L.; Yang, Xiao-Juan; Wu, Biao; Journal of the American Chemical Society 140 (2018) 5248–5256; doi:10.1021/jacs.8b01488

data_4132090
_publ_section_title
;
 Controlling the Recognition and Reactivity of Alkyl Ammonium Guests Using
 an Anion Coordination-Based Tetrahedral Cage.
;
_journal_issue                   15
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5248
_journal_page_last               5256
_journal_paper_doi               10.1021/jacs.8b01488
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety
'2(O4 P), 2(C63 H48 N18 O12), 4.49(C8 H20 N), 2(C2 H3 N), C8 N, 8(O)'
_chemical_formula_sum            'C177.96 H221.9 N43.99 O40 P2'
_chemical_formula_weight         3679.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-12-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   24.0880(6)
_cell_length_b                   60.3283(14)
_cell_length_c                   67.581(3)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.91
_cell_measurement_theta_min      2.78
_cell_volume                     98208(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       70
_diffrn_reflns_limit_k_min       -68
_diffrn_reflns_limit_l_max       80
_diffrn_reflns_limit_l_min       -79
_diffrn_reflns_number            93517
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        66.798
_diffrn_reflns_theta_max         66.798
_diffrn_reflns_theta_min         1.963
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.995
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             31162
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.7528
_exptl_transmission_factor_min   0.6893
_refine_diff_density_max         1.310
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1191
_refine_ls_number_reflns         21067
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.1212
_refine_ls_R_factor_gt           0.1017
_refine_ls_shift/su_max          0.182
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1300P)^2^+500.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2761
_refine_ls_wR_factor_ref         0.2891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15273
_reflns_number_total             21067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01488_si_002.cif
_cod_data_source_block           Cage3-TEA
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'none' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'F d d d'
_cod_original_formula_sum        'C177.96 H221.90 N43.99 O40 P2'
_cod_database_code               4132090
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.789
_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
 C77-C76 = C88-C89 = C85-C87 = C88A-C89
 1.53 with sigma of 0.01
 C83-C84
 1.53 with sigma of 0.01
 N20-C74 = N29-C88 = N29-C85
 1.45 with sigma of 0.01
3. Others
 Sof(N28)=0.25*FVAR(2)
 Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=FVAR(1)
 Fixed Sof: C88(0.5) C88A(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B), C66(H66A,H66B), C68(H68A,H68B), C70(H70A,H70B), C74(H74A,
 H74B), C76(H76A,H76B), C72(H72A,H72B), C83(H83A,H83B), C81(H81A,H81B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C9(H9), C8(H8), C6(H6), C63(H63), C32(H32), C45(H45), C26(H26),
 C62(H62), C33(H33), C46(H46), C49(H49), C48(H48), C25(H25), C12(H12), C35(H35),
  C29(H29), C28(H28), C60(H60), C15(H15), C34(H34), C55(H55), C20(H20),
 C54(H54), C53(H53), C59(H59), C13(H13), C19(H19), C52(H52), C14(H14), C22(H22),
  C23(H23), C40(H40), C43(H43), C42(H42), C39(H39), N16(H16), N14(H14A), N4(H4),
  N5(H5A), N9(H9A), N12(H12A), N11(H11), N15(H15A), N10(H10), N6(H6A), N17(H17),
  N7(H7)
4.c Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C71(H71A,H71B,H71C), C69(H69A,H69B,
 H69C), C73(H73A,H73B,H73C), C75(H75A,H75B,H75C), C79(H79A,H79B,H79C), C84(H84A,
 H84B,H84C), C82(H82A,H82B,H82C), C77(H77A,H77B,H77C)
;
_shelx_res_checksum              57059
_shelx_hkl_checksum              11067
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20