Cooperatively enhanced ion pair binding with a hybrid receptor.
Mäkelä, Toni; Kalenius, Elina; Rissanen, Kari; Inorganic chemistry 54 (2015) 9154–9165; doi:10.1021/acs.inorgchem.5b01577

data_4346482
_publ_section_title
;
 Cooperatively enhanced ion pair binding with a hybrid receptor.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9154
_journal_page_last               9165
_journal_paper_doi               10.1021/acs.inorgchem.5b01577
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '0.25(C120 H136 K4 N24 O48), C H4 O, F'
_chemical_formula_sum            'C31 H38 F K N6 O13'
_chemical_formula_weight         760.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.936(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.1600(5)
_cell_length_b                   25.3181(5)
_cell_length_c                   14.3227(4)
_cell_measurement_reflns_used    7186
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.9770
_cell_measurement_theta_min      3.7160
_cell_volume                     6872.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega -112.00  -18.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.6959  -57.0000  120.0000 188

  2 omega  -71.00   31.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.6959   77.0000  -60.0000 204

  3 omega   35.00  122.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406 -125.0000  -30.0000 174

  4 omega  102.00  178.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  112.0000 -124.0000 152

  5 omega   83.00  178.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406   30.0000   30.0000 190

  6 omega   37.00  130.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -61.0000  -60.0000 186
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0036183000
_diffrn_orient_matrix_UB_12      0.0589890000
_diffrn_orient_matrix_UB_13      -0.0243687000
_diffrn_orient_matrix_UB_21      -0.0529802000
_diffrn_orient_matrix_UB_22      -0.0094638000
_diffrn_orient_matrix_UB_23      -0.1052008000
_diffrn_orient_matrix_UB_31      -0.0614822000
_diffrn_orient_matrix_UB_32      0.0116363000
_diffrn_orient_matrix_UB_33      0.0378029000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22631
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.747
_diffrn_reflns_theta_min         3.718
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.060
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description
;
;
_exptl_crystal_F_000             3184
_exptl_crystal_recrystallization_method 'Evaporation of acetone'
_exptl_crystal_size_max          0.3322
_exptl_crystal_size_mid          0.1974
_exptl_crystal_size_min          0.0777
_refine_diff_density_max         2.816
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     953
_refine_ls_number_reflns         12045
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.1372
_refine_ls_R_factor_gt           0.1226
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_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          0.2875
_refine_ls_wR_factor_ref         0.3131
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9344
_reflns_number_total             12045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01577_si_012.cif
_cod_data_source_block           R1-KF
_cod_database_code               4346482
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H34 N6 O12 K1 F1'
_reflns_odcompleteness_completeness 98.57
_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, All O(H) groups
2. Restrained distances
 H4A-H14
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(K1A) = Uanis(K1B)
4. Others
 Fixed Sof: K1A(0.95) K1B(0.05) K2A(0.8) K2B(0.2)
5.a Secondary CH2 refined with riding coordinates:
 C21A(H21A,H21B), C21B(H21C,H21D), C22A(H22A,H22B), C22B(H22C,H22D), C23A(H23A,
 H23B), C23B(H23C,H23D), C24A(H24A,H24B), C24B(H24C,H24D), C25A(H25A,H25B),
 C25B(H25C,H25D), C26A(H26A,H26B), C26B(H26C,H26D), C27A(H27A,H27B), C27B(H27C,
 H27D), C28A(H28A,H28B), C28B(H28C,H28D), C29A(H29A,H29B), C29B(H29C,H29D),
 C30A(H30A,H30B), C30B(H30C,H30D)
5.b Aromatic/amide H refined with riding coordinates:
 N1A(H1A), N1B(H1B), N2A(H2A), N2B(H2B), N3A(H3A), N3B(H3B), N4A(H4A),
 N4B(H4B), C3A(H3AA), C3B(H3BA), C4A(H4AA), C4B(H4BA), C6A(H6A), C6B(H6B),
 C7A(H7A), C7B(H7B), C10A(H10A), C10B(H10B), C11A(H11A), C11B(H11B), C13A(H13A),
  C13B(H13B), C14A(H14A), C14B(H14B), C17A(H17A), C17B(H17B), C20A(H20A),
 C20B(H20B)
5.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C31(H31A,H31B,H31C)
5.d Idealised tetrahedral OH refined as rotating group:
 O14(H14), O13(H13)
;
_shelx_res_checksum              33388
_shelx_hkl_checksum              75918
_olex2_submission_special_instructions 'No special instructions were received'