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_4132089
_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
'8(O4 P), 8(C63 H48 N18 O12), 9(C16 N), 6(C2 N), 8.18(C11 N), 4(C8 N), 2(C5 N), 2(C2 H3 N), 12(O), C2 N2'
_chemical_formula_sum            'C700 H862 N173 O140 P8'
_chemical_formula_weight         14187.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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                 93.821(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   64.9220(17)
_cell_length_b                   38.8988(9)
_cell_length_c                   43.3302(12)
_cell_measurement_reflns_used    9809
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.74
_cell_measurement_theta_min      2.61
_cell_volume                     109182(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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0597
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       77
_diffrn_reflns_limit_h_min       -77
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            235270
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        66.731
_diffrn_reflns_theta_max         66.731
_diffrn_reflns_theta_min         1.325
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5662
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.863
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             30052
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.3
_platon_squeeze_details
;
;
_refine_diff_density_max         1.141
_refine_diff_density_min         -1.326
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     5056
_refine_ls_number_reflns         95076
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.1827
_refine_ls_R_factor_gt           0.1355
_refine_ls_shift/su_max          0.093
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3429
_refine_ls_wR_factor_ref         0.3901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                45335
_reflns_number_total             95076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01488_si_002.cif
_cod_data_source_block           Cage3-CH3CN
_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_database_code               4132089
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.814
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C254-C253
 1.47 with sigma of 0.02
 N84-C410
 1.47 with sigma of 0.02
 N84-C406
 1.47 with sigma of 0.02
 N84-C418
 1.5 with sigma of 0.02
 N84-C414
 1.47 with sigma of 0.02
 N85-C423
 1.47 with sigma of 0.02
 N85-C427
 1.47 with sigma of 0.02
 N82-C382
 1.47 with sigma of 0.02
 C351-C352
 1.53 with sigma of 0.02
 C331-C332
 1.53 with sigma of 0.02
 C395-C396
 1.53 with sigma of 0.02
 C308-C309
 1.53 with sigma of 0.02
 C323-C324
 1.53 with sigma of 0.02
 C410-C411
 1.53 with sigma of 0.02
 C423-C424
 1.53 with sigma of 0.02
 C420-C421
 1.53 with sigma of 0.02
 C3AA-C2AA
 1.53 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C424) \\sim Ueq, Uanis(C352) \\sim Ueq, Uanis(C179) \\sim Ueq,
Uanis(C395) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Aromatic/amide H refined with riding coordinates:
 N14(H14), N68(H68A), N32(H32), N4(H4), N33(H33), N40(H40A), N9(H9), N58(H58),
 N63(H63A), N15(H15), N17(H17), N34(H34), N11(H11), N22(H22), N45(H45A),
 N16(H16), N41(H41), N27(H27), N12(H12), N50(H50), N10(H10), N35(H35), N5(H5),
 N30(H30), N28(H28), N42(H42A), N60(H60A), N43(H43A), N64(H64), N29(H29),
 N69(H69A), N6(H6), N61(H61), N59(H59A), N23(H23), N66(H66), N7(H7), N65(H65),
 C214(H214), N46(H46A), C215(H215), N70(H70), N25(H25), C218(H218), C217(H217),
 C88(H88), N24(H24), C109(H109), C108(H108), C238(H238), C237(H237), N47(H47),
 C6(H6A), C46(H46), C89(H89), C194(H194), C71(H71), C197(H197), C5(H5A),
 C198(H198), C195(H195), C45(H45), C26(H26), C72(H72), C111(H111), N48(H48A),
 C234(H234), C138(H138), C106(H106), C91(H91), C135(H135), C48(H48), C29(H29A),
 C28(H28A), C134(H134), C25(H25A), C63(H63), C235(H235), N53(H53A), C49(H49),
 C59(H59), C35(H35A), C52(H52), C175(H175), C139(H139), C132(H132), C152(H152),
 N52(H52A), C131(H131), C43(H43), C92(H92), C112(H112), C55(H55), C151(H151),
 C174(H174), C232(H232), C39(H39), C141(H141), C105(H105), C69(H69), C32(H32A),
 C140(H140), C23(H23A), C60(H60), C68(H68), C12(H12A), C9(H9A), C54(H54),
 C40(H40), C172(H172), C53(H53), C8(H8), C42(H42), C171(H171), C102(H102),
 C34(H34A), C33(H33A), C118(H118), C98(H98), C149(H149), C115(H115), C122(H122),
  C212(H212), C15(H15A), C154(H154), C117(H117), C145(H145), C103(H103),
 C155(H155), C209(H209), C62(H62), C208(H208), C78(H78), C116(H116), C201(H201),
  C126(H126), C204(H204), C211(H211), C123(H123), N71(H71A), N51(H51),
 C224(H224), C22(H22A), C13(H13), C75(H75), C169(H169), C228(H228), C14(H14A),
 C146(H146), C158(H158), C244(H244), C97(H97), C229(H229), C148(H148),
 C231(H231), C77(H77), C125(H125), C203(H203), C161(H161), C241(H241), C76(H76),
  C243(H243), C82(H82), C83(H83), C19(H19), C202(H202), C95(H95), C160(H160),
 C189(H189), C223(H223), C221(H221), C185(H185), C159(H159), C242(H242),
 C188(H188), C86(H86), C20(H20), C96(H96), C186(H186), C168(H168), C222(H222),
 C165(H165), C85(H85), C166(H166), C181(H181), C252(H252), C251(H251),
 C178(H178), C180(H180), C248(H248), C179(H179), C249(H249)
4.b Idealised Me refined as rotating group:
 C254(H25B,H25C,H25D)
;
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'