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_4346491
_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
'C36 H48 K N8 O14, C30 H35.2 K N6 O12.6, C3 H7 N O, C O3'
_chemical_formula_sum            'C70 H90.2 K2 N15 O30.6'
_chemical_formula_weight         1709.57
_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   mixed
_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)
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_cell_angle_alpha                90
_cell_angle_beta                 103.0744(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.28885(14)
_cell_length_b                   37.9226(7)
_cell_length_c                   21.1223(3)
_cell_measurement_reflns_used    10718
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.9130
_cell_measurement_theta_min      4.0920
_cell_volume                     8027.9(2)
_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
;
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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -45.00   -3.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.8209   37.0000 -180.0000 42

  2 omega -113.00  -24.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.8209  -37.0000   30.0000 89

  3 omega   23.00   87.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8209 -125.0000  -90.0000 64

  4 omega   32.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -30.0000 -150.0000 59

  5 omega   32.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -30.0000  -30.0000 59

  6 omega   32.00   87.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -30.0000   30.0000 55

  7 omega   83.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -94.0000 -150.0000 26

  8 omega   37.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -94.0000 -150.0000 26

  9 omega   39.00  107.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -94.0000  150.0000 68

 10 omega   94.00  169.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  125.0000  120.0000 75
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0540233000
_diffrn_orient_matrix_UB_12      0.0373615000
_diffrn_orient_matrix_UB_13      -0.0068469000
_diffrn_orient_matrix_UB_21      -0.1387646000
_diffrn_orient_matrix_UB_22      0.0155341000
_diffrn_orient_matrix_UB_23      -0.0009919000
_diffrn_orient_matrix_UB_31      0.0380839000
_diffrn_orient_matrix_UB_32      0.0036371000
_diffrn_orient_matrix_UB_33      0.0745655000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27060
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.750
_diffrn_reflns_theta_min         3.169
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94262
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             3592
_exptl_crystal_recrystallization_method
'Crystallized from DMF/MeOH/H2O mixture with added KF'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         14054
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0641P)^2^+4.8818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11653
_reflns_number_total             14054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01577_si_010.cif
_cod_data_source_block           R1-K2CO3
_cod_original_formula_sum        'C70 H90.20 K2 N15 O30.60'
_cod_database_code               4346491
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C38 H51 N9 O17 K2'
_reflns_odcompleteness_completeness 98.64
_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 C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C23A-C24A = C23C-C24C
 1.51 with sigma of 0.01
 O8C-C22C = O8A-C22A = O8A-C23A = O8C-C23C
 1.42 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C23A) = Uanis(C24A)
4. Others
 Fixed Sof: K1A(0.6) K1B(0.4) O8A(0.5) O8C(0.5) O18(0.6) H18A(0.6) H18B(0.6)
 H21C(0.6) H21D(0.6) H21E(0.4) H21F(0.4) C22A(0.4) H22E(0.4) H22F(0.4)
 C22C(0.6) H22C(0.6) H22D(0.6) C23A(0.6) H23E(0.6) H23F(0.6) C23C(0.4)
 H23C(0.4) H23D(0.4) C24A(0.4) H24E(0.4) H24F(0.4) C24C(0.6) H24C(0.6) H24D(0.6)
5.a Rotating group:
 O18(H18A,H18B)
5.b Secondary CH2 refined with riding coordinates:
 C21B(H21A,H21B), C22B(H22A,H22B), C23B(H23A,H23B), C24B(H24A,H24B), C25B(H25A,
 H25B), C26B(H26A,H26B), C27B(H27A,H27B), C28B(H28A,H28B), C29B(H29A,H29B),
 C30B(H30A,H30B), C21A(H21C,H21D), C21A(H21E,H21F), C22A(H22E,H22F), C22C(H22C,
 H22D), C23A(H23E,H23F), C23C(H23C,H23D), C24A(H24E,H24F), C24C(H24C,H24D),
 C25A(H25C,H25D), C26A(H26C,H26D), C27A(H27C,H27D), C28A(H28C,H28D), C29A(H29C,
 H29D), C30A(H30C,H30D)
5.c Aromatic/amide H refined with riding coordinates:
 N1B(H1B), N2B(H2B), N3B(H3B), N4B(H4B), C3B(H3BA), C4B(H4BA), C6B(H6B),
 C7B(H7B), C10B(H10B), C11B(H11B), C13B(H13B), C14B(H14B), C17B(H17B),
 C20B(H20B), C32(H32), C35(H35), N2A(H2A), N4A(H4A), C3A(H3AA), C4A(H4AA),
 C6A(H6A), C7A(H7A), C10A(H10A), C11A(H11A), C13A(H13A), C14A(H14A), C17A(H17A),
  C20A(H20A), C38(H38)
5.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              75996
_shelx_hkl_checksum              35727
_olex2_submission_special_instructions 'No special instructions were received'