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_7038571
_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 O22 Rb, 0.5(C4 H10 O), C0.5 H2.5 O, C H4 O, F'
_chemical_formula_sum            'C59.5 H71.5 F N12 O24.5 Rb'
_chemical_formula_weight         1451.25
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-01
_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                83.6625(19)
_cell_angle_beta                 71.3472(18)
_cell_angle_gamma                65.190(2)
_cell_formula_units_Z            2
_cell_length_a                   14.0458(3)
_cell_length_b                   15.7391(4)
_cell_length_c                   18.0442(4)
_cell_measurement_reflns_used    17687
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.2390
_cell_measurement_theta_min      4.0780
_cell_volume                     3429.33(15)
_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 5.1977
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega -113.00  -13.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176  -57.0000  -60.0000 100

  2 omega  -49.00   33.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176   37.0000   90.0000 82

  3 omega  -96.00   -2.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176  125.0000   90.0000 94

  4 omega  -56.00    3.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000   45.0000  -90.0000 59

  5 omega   89.00  165.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   90.0000 76

  6 omega   67.00  109.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   60.0000 42

  7 omega   39.00   99.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -30.0000 60

  8 omega  106.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000   30.0000 72

  9 omega   48.00  109.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -180.0000 61

 10 omega   59.00  176.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   15.0000   30.0000 117

 11 omega   36.00   91.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   90.0000 55

 12 omega   30.00  105.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000    0.0000 75

 13 omega   43.00   99.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  150.0000 56

 14 omega   39.00   98.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   60.0000 59

 15 omega   37.00  114.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -30.0000 77
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0794793000
_diffrn_orient_matrix_UB_12      0.0719470000
_diffrn_orient_matrix_UB_13      -0.0414275000
_diffrn_orient_matrix_UB_21      0.0056741000
_diffrn_orient_matrix_UB_22      -0.0801555000
_diffrn_orient_matrix_UB_23      -0.0454679000
_diffrn_orient_matrix_UB_31      -0.0986396000
_diffrn_orient_matrix_UB_32      -0.0059872000
_diffrn_orient_matrix_UB_33      0.0658980000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22929
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.748
_diffrn_reflns_theta_min         3.638
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.762
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.618
_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    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             1509
_exptl_crystal_size_max          0.2507
_exptl_crystal_size_mid          0.2431
_exptl_crystal_size_min          0.1219
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     934
_refine_ls_number_reflns         12028
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0496P)^2^+2.1600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11431
_reflns_number_total             12028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00414h2.cif
_cod_data_source_block           R1_RbF
_cod_depositor_comments
'Adding full bibliography for 7038560--7038573.cif.'
_cod_original_cell_volume        3429.30(14)
_cod_original_formula_sum        'C59.50 H71.50 F N12 O24.50 Rb'
_cod_database_code               7038571
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C28 H28 N6 O10 Rb1 F1'
_reflns_odcompleteness_completeness 98.92
_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
 O6C-N6B = O6B-N6B
 1.22 with sigma of 0.02
 O5C-N6A
 1.21 with sigma of 0.005
 N6A-O5A
 1.21 with sigma of 0.02
 O5D-N6A
 1.21 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O6C) = Uanis(O6B)
Uanis(O5A) = Uanis(N6A)
Uanis(O5D) = Uanis(N6A)
Uanis(O5C) = Uanis(N6A)
Uanis(N6A) = Uanis(O6A)
4. Others
 Fixed Sof: H25C(0.8) H25D(0.8) H25E(0.2) H25F(0.2) H27E(0.2) H27F(0.2)
 H27C(0.8) H27D(0.8) O5A(0.4) O6C(0.5) O10B(0.8) C26B(0.8) H26C(0.8) H26D(0.8)
 O5C(0.3) O6B(0.5) O10C(0.2) C26C(0.2) H26E(0.2) H26F(0.2) O5D(0.3) O14(0.5)
 C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C32(0.5) H32A(0.5) H32B(0.5) C33(0.5)
 H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) C29(0.5) H29A(0.5)
 H29B(0.5) H29C(0.5)
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), C25A(H25A,H25B),
 C25B(H25C,H25D), C25B(H25E,H25F), C26A(H26A,H26B), C27A(H27A,H27B), C27B(H27E,
 H27F), C27B(H27C,H27D), C28A(H28A,H28B), C28B(H28C,H28D), C26B(H26C,H26D),
 C26C(H26E,H26F), C32(H32A,H32B), C33(H33A,H33B)
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:
 C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
5.d Idealised tetrahedral OH refined as rotating group:
 O13(H13)
;
_olex2_date_sample_data_collection 15.7.2013
_olex2_submission_special_instructions 'No special instructions were received'