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_4346488
_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         'C30 H34 Br0.98 K N6 O12, 0.02(Br)'
_chemical_formula_sum            'C30 H34 Br K N6 O12'
_chemical_formula_weight         789.64
_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     iterative
_audit_creation_date             2015-01-22
_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                 96.827(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7776(3)
_cell_length_b                   9.0066(2)
_cell_length_c                   31.8166(10)
_cell_measurement_reflns_used    5239
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      74.9820
_cell_measurement_theta_min      3.7720
_cell_volume                     3351.05(16)
_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    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -95.00  -67.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176 -139.0000 -145.0000 28

  2 omega  -49.00   33.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176   37.0000  150.0000 82

  3 omega  -96.00   -4.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176  125.0000 -150.0000 92

  4 omega   79.00  170.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -120.0000 91

  5 omega   42.00  137.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000   90.0000 95

  6 omega   56.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -90.0000 35

  7 omega  100.00  140.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  -90.0000 40

  8 omega   38.00   78.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -120.0000 40

  9 omega   96.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000 -180.0000 78
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0624120000
_diffrn_orient_matrix_UB_12      -0.1361674000
_diffrn_orient_matrix_UB_13      0.0209901000
_diffrn_orient_matrix_UB_21      -0.0196978000
_diffrn_orient_matrix_UB_22      0.0599169000
_diffrn_orient_matrix_UB_23      0.0439271000
_diffrn_orient_matrix_UB_31      -0.1142450000
_diffrn_orient_matrix_UB_32      -0.0846333000
_diffrn_orient_matrix_UB_33      -0.0028148000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            10074
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.746
_diffrn_reflns_theta_min         3.780
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.414
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.644
_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    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_recrystallization_method
'Diffusion of diethyl ether into acetone solution'
_exptl_crystal_size_max          0.1789
_exptl_crystal_size_mid          0.1191
_exptl_crystal_size_min          0.0468
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         5887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0447P)^2^+4.9514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5230
_reflns_number_total             5887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01577_si_007.cif
_cod_data_source_block           R1-KBr_2
_cod_original_cell_volume        3351.07(15)
_cod_database_code               4346488
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H32 Br1 K1 N6 O12'
_reflns_odcompleteness_completeness 98.78
_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 N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Br1A) = Uanis(Br1B)
3. Others
 Fixed Sof: O9A(0.6) O9B(0.4) C25A(0.6) H25A(0.6) H25B(0.6) C25B(0.4)
 H25C(0.4) H25D(0.4) C26A(0.6) H26A(0.6) H26B(0.6) C26B(0.4) H26C(0.4)
 H26D(0.4) Br1A(0.98) Br1B(0.02)
4.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25A(H25A,
 H25B), C25B(H25C,H25D), C26A(H26A,H26B), C26B(H26C,H26D), C27(H27A,H27B),
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), C3(H3A), C4(H4A), C6(H6), C7(H7), C10(H10),
 C11(H11), C13(H13), C14(H14), C17(H17), C20(H20)
;
_shelx_res_checksum              67026
_shelx_hkl_checksum              92120
_olex2_submission_special_instructions 'No special instructions were received'