Ion pair complexes and anion binding in the solution of a ditopic receptor.
Mäkelä, T; Rissanen, K.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6481–6490; doi:10.1039/c6dt00414h

data_7038572
_publ_section_title
;
 Ion pair complexes and anion binding in the solution of a ditopic
 receptor.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6481
_journal_page_last               6490
_journal_paper_doi               10.1039/c6dt00414h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C56 H60 N12 O21.65 Rb, C H4 O, Cl, 0.35(O1)'
_chemical_formula_sum            'C57 H64 Cl N12 O23 Rb'
_chemical_formula_weight         1406.12
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-17 deposited with the CCDC.
2016-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                91.9928(15)
_cell_angle_beta                 92.1858(14)
_cell_angle_gamma                91.3214(13)
_cell_formula_units_Z            2
_cell_length_a                   10.38455(15)
_cell_length_b                   12.4289(2)
_cell_length_c                   25.4568(5)
_cell_measurement_reflns_used    16473
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.2620
_cell_measurement_theta_min      4.2530
_cell_volume                     3280.32(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 5.1977
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega -114.00  -10.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176  -73.0000  134.0000 104

  2 omega  -96.00   -3.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176  125.0000    0.0000 93

  3 omega -126.00  -34.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -45.0000 -150.0000 92

  4 omega  -85.00   17.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000   61.0000    0.0000 102

  5 omega   40.00  141.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000   90.0000 101

  6 omega   36.00  116.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -90.0000 80

  7 omega   39.00   91.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -60.0000 52

  8 omega  144.00  178.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  -30.0000 34

  9 omega   36.00   67.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   90.0000 31

 10 omega   79.00  116.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   90.0000 37

 11 omega   87.00  122.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  -30.0000 35

 12 omega   47.00   99.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -150.0000 52

 13 omega   36.00  145.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  -30.0000 109

 14 omega   24.00  175.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000    0.0000  150.0000 151
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0981368000
_diffrn_orient_matrix_UB_12      0.0159257000
_diffrn_orient_matrix_UB_13      0.0467058000
_diffrn_orient_matrix_UB_21      -0.0649258000
_diffrn_orient_matrix_UB_22      0.1054923000
_diffrn_orient_matrix_UB_23      0.0164572000
_diffrn_orient_matrix_UB_31      -0.0905933000
_diffrn_orient_matrix_UB_32      -0.0633180000
_diffrn_orient_matrix_UB_33      0.0349287000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21889
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.749
_diffrn_reflns_theta_min         3.477
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.151
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_correction_T_min  0.555
_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    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.2498
_exptl_crystal_size_mid          0.2061
_exptl_crystal_size_min          0.1427
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         11512
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0488P)^2^+11.9901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10977
_reflns_number_total             11512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00414h2.cif
_cod_data_source_block           R1_RbCl
_cod_depositor_comments
'Adding full bibliography for 7038560--7038573.cif.'
_cod_original_cell_volume        3280.31(10)
_cod_database_code               7038572
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C28 H28 N6 O10 Rb1 Cl1'
_reflns_odcompleteness_completeness 98.49
_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
 O9B-C25B = O9C-C25C
 1.42 with sigma of 0.01
 O9C-C24C = O9B-C24B
 1.42 with sigma of 0.01
 C23B-C24B
 1.52 with sigma of 0.02
 O9C-C25C = O9B-C25B = O9B-C24B = O8C-C23C = O8B-C23B = O10B-C26B = O10C-C26C =
  O10C-C27B = O10B-C27B
 1.42 with sigma of 0.01
 C23B-C24B = C26C-C25C = C26B-C25B
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C24B) \\sim Ueq, Uanis(C24C) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C23B) \\sim Ueq, Uanis(C23C) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O9D) = Uanis(O9C) = Uanis(O9B)
Uanis(C25C) = Uanis(C25B)
Uanis(C22C) = Uanis(C22B)
Uanis(Cl1B) = Uanis(Cl1A)
Uanis(C24C) = Uanis(C24B)
Uanis(C23C) = Uanis(C23B)
Uanis(C26B) = Uanis(C26C)
4. Others
 Fixed Sof: H21A(0.5) H21B(0.5) H21C(0.5) H21D(0.5) H27A(0.5) H27B(0.5)
 H27C(0.5) H27D(0.5) O8B(0.5) O9B(0.35) O10B(0.5) C22B(0.5) H22C(0.5) H22D(0.5)
 C23B(0.5) H23C(0.5) H23D(0.5) C24B(0.5) H24C(0.5) H24D(0.5) C25B(0.5)
 H25C(0.5) H25D(0.5) C26B(0.5) H26C(0.5) H26D(0.5) O8C(0.5) O9C(0.3) O10C(0.5)
 C22C(0.5) H22E(0.5) H22F(0.5) C23C(0.5) H23E(0.5) H23F(0.5) C24C(0.5)
 H24E(0.5) H24F(0.5) C25C(0.5) H25E(0.5) H25F(0.5) C26C(0.5) H26E(0.5)
 H26F(0.5) Cl1B(0.05) O9D(0.35) Cl1A(0.95)
5.a Secondary CH2 refined with riding coordinates:
 C21A(H21E,H21F), C21B(H21A,H21B), C21B(H21C,H21D), C22A(H22A,H22B), C23A(H23A,
 H23B), C24A(H24A,H24B), C25A(H25A,H25B), C26A(H26A,H26B), C27A(H27E,H27F),
 C27B(H27A,H27B), C27B(H27C,H27D), C28A(H28C,H28D), C28B(H28A,H28B), C22B(H22C,
 H22D), C23B(H23C,H23D), C24B(H24C,H24D), C25B(H25C,H25D), C26B(H26C,H26D),
 C22C(H22E,H22F), C23C(H23E,H23F), C24C(H24E,H24F), C25C(H25E,H25F), C26C(H26E,
 H26F)
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), C4A(H4AA), C4B(H4BA), C5A(H5A), C5B(H5B), C7A(H7A), C7B(H7B),
 C8A(H8A), C8B(H8B), 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:
 C29(H29A,H29B,H29C)
5.d Idealised tetrahedral OH refined as rotating group:
 O12(H12)
;
_olex2_date_sample_data_collection 15.7.2013
_olex2_submission_special_instructions 'No special instructions were received'