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_4346485
_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         'C60 H68 K2 N12 O24, 3(C H4 O), 2(Cl)'
_chemical_formula_sum            'C63 H80 Cl2 K2 N12 O27'
_chemical_formula_weight         1586.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-06
_audit_creation_method
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Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
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_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_c                   20.8333(2)
_cell_measurement_reflns_used    13538
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.2740
_cell_measurement_theta_min      3.5880
_cell_volume                     7238.50(13)
_computing_cell_refinement
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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_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)
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_computing_data_reduction
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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_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega -112.00  -15.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7426  -57.0000  150.0000 97

  2 omega -130.00  -36.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  178.0000 -120.0000 94

  3 omega   37.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -90.0000 52

  4 omega   39.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -150.0000 31

  5 omega   38.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   60.0000 71

  6 omega   89.00  140.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   30.0000 51

  7 omega   62.00  151.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000  -90.0000 89

  8 omega  148.00  174.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   30.0000 26

  9 omega   38.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -120.0000 51

 10 omega   39.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   60.0000 57
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
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_diffrn_orient_matrix_UB_12      -0.0218846000
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_diffrn_orient_matrix_UB_22      0.0589376000
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_diffrn_orient_matrix_UB_31      -0.0686803000
_diffrn_orient_matrix_UB_32      -0.0047037000
_diffrn_orient_matrix_UB_33      0.0410219000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
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_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25335
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.743
_diffrn_reflns_theta_min         3.597
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.613
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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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)
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)
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_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       block
_exptl_crystal_F_000             3320
_exptl_crystal_recrystallization_method
'Diffusion of diethyl ether into methanol solution'
_exptl_crystal_size_max          0.2836
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_exptl_crystal_size_min          0.1057
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_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     988
_refine_ls_number_reflns         12732
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_refine_ls_R_factor_all          0.0455
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_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+4.2756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                11259
_reflns_number_total             12732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01577_si_005.cif
_cod_data_source_block           R1-KCl
_cod_database_code               4346485
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H34 N6 O12 K1 Cl1'
_reflns_odcompleteness_completeness 98.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: O9B(0.85) O9C(0.15) O11B(0.85) O11C(0.15) H24C(0.85) H24D(0.85)
 H24E(0.15) H24F(0.15) H25C(0.85) H25D(0.85) H25E(0.15) H25F(0.15) H28C(0.85)
 H28D(0.85) H28E(0.15) H28F(0.15) C29B(0.85) H29C(0.85) H29D(0.85) C29C(0.15)
 H29E(0.15) H29F(0.15) H30C(0.85) H30D(0.85) H30E(0.15) H30F(0.15)
3.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), C24B(H24E,H24F),
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 H26D), C27A(H27A,H27B), C27B(H27C,H27D), C28A(H28A,H28B), C28B(H28C,H28D),
 C28B(H28E,H28F), C29A(H29A,H29B), C29B(H29C,H29D), C29C(H29E,H29F), C30A(H30A,
 H30B), C30B(H30C,H30D), C30B(H30E,H30F)
3.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), C14B(H14B), C11A(H11A), C13B(H13B), C13A(H13A),
  C11B(H11B), C14A(H14A), C10B(H10B), C17A(H17A), C17B(H17B), C20A(H20A),
 C20B(H20B)
3.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
3.d Idealised tetrahedral OH refined as rotating group:
 O13(H13), O14(H14), O15(H15)
;
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_olex2_submission_special_instructions 'No special instructions were received'