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_4346487
_publ_section_title
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 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(Br)'
_chemical_formula_sum            'C63 H80 Br2 K2 N12 O27'
_chemical_formula_weight         1675.41
_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             2015-03-04
_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
_cell_angle_beta                 107.6352(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.93502(16)
_cell_length_b                   24.5596(2)
_cell_length_c                   20.95712(19)
_cell_measurement_reflns_used    12354
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      74.6210
_cell_measurement_theta_min      4.2110
_cell_volume                     7325.78(13)
_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
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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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -49.00   33.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176   37.0000  -90.0000 82

  2 omega -132.00  -88.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000 -111.0000  -90.0000 44

  3 omega  -83.00   17.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000   77.0000 -180.0000 100

  4 omega   39.00   99.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000    0.0000 60

  5 omega   36.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -150.0000 55

  6 omega   44.00   99.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   60.0000 55

  7 omega   39.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -60.0000 52

  8 omega   91.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000 -120.0000 87

  9 omega  106.00  172.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  120.0000 66
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0411493000
_diffrn_orient_matrix_UB_12      -0.0099388000
_diffrn_orient_matrix_UB_13      0.0758520000
_diffrn_orient_matrix_UB_21      0.0562167000
_diffrn_orient_matrix_UB_22      -0.0488283000
_diffrn_orient_matrix_UB_23      -0.0137340000
_diffrn_orient_matrix_UB_31      0.0828371000
_diffrn_orient_matrix_UB_32      0.0381232000
_diffrn_orient_matrix_UB_33      0.0021542000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24794
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.740
_diffrn_reflns_theta_min         3.690
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.189
_exptl_absorpt_correction_T_max  0.774
_exptl_absorpt_correction_T_min  0.561
_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    1.519
_exptl_crystal_description       block
_exptl_crystal_F_000             3464
_exptl_crystal_recrystallization_method
'Diffusion of diethyl ether into methanol solution'
_exptl_crystal_size_max          0.3163
_exptl_crystal_size_mid          0.1857
_exptl_crystal_size_min          0.1002
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1015
_refine_ls_number_reflns         12867
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+7.8300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11249
_reflns_number_total             12867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01577_si_006.cif
_cod_data_source_block           R1-KBr_1
_cod_original_cell_volume        7325.76(13)
_cod_database_code               4346487
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H34 N6 O12 K1 Br1'
_reflns_odcompleteness_completeness 98.66
_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. Restrained distances
 H14-Br2
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Br1C) = Uanis(Br1A)
Uanis(N6A) = Uanis(N6C)
Uanis(N6A) = Uanis(C12A)
4. Others
 Fixed Sof: O5A(0.5) O5C(0.5) O6A(0.5) O6C(0.5) O9B(0.75) O9C(0.25) O11B(0.6)
 O11C(0.4) N6A(0.5) N6C(0.5) H24C(0.75) H24D(0.75) H24E(0.25) H24F(0.25)
 C25B(0.75) H25C(0.75) H25D(0.75) C25C(0.25) H25E(0.25) H25F(0.25) H26C(0.75)
 H26D(0.75) H26E(0.25) H26F(0.25) H28C(0.6) H28D(0.6) H28E(0.4) H28F(0.4)
 C29B(0.6) H29C(0.6) H29D(0.6) C29C(0.4) H29E(0.4) H29F(0.4) H30C(0.6)
 H30D(0.6) H30E(0.4) H30F(0.4) Br1C(0.05) Br1A(0.95)
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), C24B(H24E,H24F),
 C25A(H25A,H25B), C25B(H25C,H25D), C25C(H25E,H25F), C26A(H26A,H26B), C26B(H26C,
 H26D), C26B(H26E,H26F), 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)
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), C33(H33A,H33B,H33C)
5.d Idealised tetrahedral OH refined as rotating group:
 O14(H14), O13(H13), O15(H15)
;
_shelx_res_checksum              8863
_shelx_hkl_checksum              6587
_olex2_submission_special_instructions 'No special instructions were received'