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_4346494
_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 Cl N6 O12 Rb'
_chemical_formula_sum            'C30 H34 Cl N6 O12 Rb'
_chemical_formula_weight         791.55
_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             2015-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.2885(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.80087(19)
_cell_length_b                   9.11972(16)
_cell_length_c                   31.1833(6)
_cell_measurement_reflns_used    5633
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      75.3810
_cell_measurement_theta_min      3.7640
_cell_volume                     3335.77(10)
_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    'XS (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   32.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176   37.0000  120.0000 81

  2 omega  -70.00   29.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176   77.0000 -150.0000 99

  3 omega   36.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   30.0000 53

  4 omega   62.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -30.0000 47

  5 omega   57.00   95.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -30.0000 38

  6 omega  102.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000   60.0000 76

  7 omega   93.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  150.0000 85

  8 omega   30.00   57.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -30.0000 27

  9 omega   39.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -60.0000 51

 10 omega   55.00   85.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -150.0000 30
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0546245000
_diffrn_orient_matrix_UB_12      -0.0092865000
_diffrn_orient_matrix_UB_13      -0.0470895000
_diffrn_orient_matrix_UB_21      0.0934147000
_diffrn_orient_matrix_UB_22      0.1018275000
_diffrn_orient_matrix_UB_23      -0.0140132000
_diffrn_orient_matrix_UB_31      0.0743996000
_diffrn_orient_matrix_UB_32      -0.1345965000
_diffrn_orient_matrix_UB_33      -0.0073588000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            10385
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.749
_diffrn_reflns_theta_min         3.768
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.411
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.727
_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    1.576
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_recrystallization_method
'Diffusion of diethyl ether into acetone solution'
_exptl_crystal_size_max          0.1191
_exptl_crystal_size_mid          0.1055
_exptl_crystal_size_min          0.0666
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         5844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0546P)^2^+4.3250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5298
_reflns_number_total             5844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01577_si_014.cif
_cod_data_source_block           R1-RbCl
_cod_original_cell_volume        3335.78(10)
_cod_database_code               4346494
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H34 Cl1 N6 O12 Rb1 '
_reflns_odcompleteness_completeness 98.74
_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
2. Uiso/Uaniso restraints and constraints
Uanis(Rb1B) = Uanis(Rb1A)
3. Others
 Fixed Sof: Rb1A(0.98) Rb1B(0.02) O9A(0.8) O9B(0.2) H24A(0.8) H24B(0.8)
 H24C(0.2) H24D(0.2) H25A(0.8) H25B(0.8) H25C(0.2) H25D(0.2)
4.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C24(H24C,
 H24D), C25(H25A,H25B), C25(H25C,H25D), C26(H26A,H26B), 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              88733
_shelx_hkl_checksum              40086
_olex2_submission_special_instructions 'No special instructions were received'