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_7038561
_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
'2(C28 H30 N6 O11), 2(C3 H6 O), 1.8(H2 O), 0.2(O)'
_chemical_formula_sum            'C62 H75.6 N12 O26'
_chemical_formula_weight         1404.94
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-25
_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                90
_cell_angle_beta                 95.2966(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.41305(15)
_cell_length_b                   23.7285(2)
_cell_length_c                   18.50903(16)
_cell_measurement_reflns_used    10473
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.2966
_cell_measurement_theta_min      3.0336
_cell_volume                     6740.38(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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      123.00(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  -62.00   18.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.9459   57.0000   30.0000 160

  2 omega  -60.00   16.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000   15.0000  -60.0000 152

  3 omega   25.00   96.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -94.0000  -60.0000 142

  4 omega   29.00  104.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -94.0000    0.0000 150

  5 omega   38.00   94.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -45.0000  120.0000 112

  6 omega   33.00   91.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -30.0000  150.0000 116

  7 omega   32.00   86.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -30.0000   60.0000 108

  8 omega   94.00  172.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  125.0000 -150.0000 156
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0364006000
_diffrn_orient_matrix_UB_12      0.0601343000
_diffrn_orient_matrix_UB_13      0.0113264000
_diffrn_orient_matrix_UB_21      0.0629776000
_diffrn_orient_matrix_UB_22      -0.0209873000
_diffrn_orient_matrix_UB_23      0.0638711000
_diffrn_orient_matrix_UB_31      0.0692259000
_diffrn_orient_matrix_UB_32      -0.0124839000
_diffrn_orient_matrix_UB_33      -0.0527306000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22369
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.748
_diffrn_reflns_theta_min         3.430
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             2958
_exptl_crystal_size_max          0.1771
_exptl_crystal_size_mid          0.1524
_exptl_crystal_size_min          0.0951
_refine_diff_density_max         0.760
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1125
_refine_ls_number_reflns         11832
_refine_ls_number_restraints     488
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0598
_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^)+(0.1038P)^2^+4.7689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1655
_refine_ls_wR_factor_ref         0.1758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10022
_reflns_number_total             11832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00414h2.cif
_cod_data_source_block           R1
_cod_depositor_comments
'Adding full bibliography for 7038560--7038573.cif.'
_cod_original_cell_volume        6740.38(11)
_cod_original_formula_sum        'C62 H75.60 N12 O26'
_cod_database_code               7038561
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C28 H30 N6 O11 Na1 F1'
_reflns_odcompleteness_completeness 98.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C25D-C26D
 1.52 with sigma of 0.02
 O9D-C25D
 1.42 with sigma of 0.02
 O8D-C23D
 1.42 with sigma of 0.02
 O8D-C22D
 1.42 with sigma of 0.02
 C28A-C27A
 1.52 with sigma of 0.01
 O7A-C21A = O7A-C21C = O8A-C22A = O8C-C22C = O8A-C23A = O8C-C23C = O9C-C24C =
 O9A-C24A = O9C-C25C = C25C-C26C = O9A-C25A = O10C-C26C = O10A-C26A = O10C-C27C
 = O10A-C27A = O11A-C28A = O11A-C28C
 1.42 with sigma of 0.01
 C21C-C22C = C22A-C21A = C24C-C23C = C24A-C23A = C25C-C26C = C25A-C26A = C27A-
 C28A = C28C-C27C
 1.52 with sigma of 0.01
 H7SC-H29A_$1
 2.1 with sigma of 0.01
 H27D-H29C_$2
 2.05 with sigma of 0.02
 O7B-O14
 2.8 with sigma of 0.01
 O11B-C28D = O11B-C28B
 1.42 with sigma of 0.02
 O11B-O14
 2.8 with sigma of 0.02
 O14-O11B
 2.8 with sigma of 0.01
3. Rigid bond restraints
 C36, O16, C32, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C36, O17, C35, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O8A \\sim O9A \\sim O10A \\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim C25A
\\sim C26A \\sim C27A \\sim C28A: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O8C \\sim O9C \\sim O10C \\sim C21C \\sim C22C \\sim C23C \\sim C24C \\sim C25C
\\sim C26C \\sim C27C \\sim C28C: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C35 \\sim C32: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C37 \\sim C34: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
O17 \\sim O16: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
O8B \\sim O9B \\sim O10B \\sim C21B \\sim C22B \\sim H80A \\sim H80B \\sim C23B
\\sim H82A \\sim H82B \\sim C24B \\sim H83A \\sim H83B \\sim C25B \\sim H85A
\\sim H85B \\sim C26B \\sim H86A \\sim H86B \\sim C27B \\sim H88A \\sim H88B
\\sim C28B \\sim H89A \\sim H89B: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O8D \\sim O9D \\sim O10D \\sim C21D \\sim H21D \\sim C22D \\sim H22C \\sim H22D
\\sim C23D \\sim H23C \\sim H23D \\sim C24D \\sim H24C \\sim H24D \\sim C25D
\\sim H25C \\sim H25D \\sim C26D \\sim H26C \\sim H26D \\sim C27D \\sim H27C
\\sim H27D \\sim C28D \\sim H28C: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C28D) = Uanis(C28B)
Uanis(C21B) = Uanis(C21D)
Uanis(C28C) = Uanis(C28A)
Uanis(C27D) = Uanis(C27B)
Uanis(O14) = Uanis(O13)
5. Others
 Fixed Sof: O8C(0.4) O9C(0.4) O10C(0.4) C21C(0.4) H21A(0.4) H21B(0.4)
 C22C(0.4) H22A(0.4) H22B(0.4) C23C(0.4) H23A(0.4) H23B(0.4) C24C(0.4)
 H24A(0.4) H24B(0.4) C25C(0.4) H25A(0.4) H25B(0.4) C26C(0.4) H26A(0.4)
 H26B(0.4) C27C(0.4) H27A(0.4) H27B(0.4) C28C(0.4) H28A(0.4) H28B(0.4) O8D(0.2)
 O9D(0.2) O10D(0.2) C21D(0.2) H21C(0.2) H21D(0.2) C22D(0.2) H22C(0.2) H22D(0.2)
 C23D(0.2) H23C(0.2) H23D(0.2) C24D(0.2) H24C(0.2) H24D(0.2) C25D(0.2)
 H25C(0.2) H25D(0.2) C26D(0.2) H26C(0.2) H26D(0.2) C27D(0.2) H27C(0.2)
 H27D(0.2) C28D(0.2) H28C(0.2) H28D(0.2) O17(0.5) C35(0.5) H35C(0.5) H35D(0.5)
 H35E(0.5) C37(0.5) H37C(0.5) H37D(0.5) H37E(0.5) O8A(0.6) O8B(0.8) O9A(0.6)
 O9B(0.8) O10A(0.6) O10B(0.8) O13(0.8) H10A(0.8) H10B(0.8) O16(0.5) C21A(0.6)
 H34A(0.6) H34B(0.6) C21B(0.8) H79A(0.8) H79B(0.8) C22A(0.6) H35A(0.6)
 H35B(0.6) C22B(0.8) H80A(0.8) H80B(0.8) C23A(0.6) H37A(0.6) H37B(0.6)
 C23B(0.8) H82A(0.8) H82B(0.8) C24A(0.6) H38A(0.6) H38B(0.6) C24B(0.8)
 H83A(0.8) H83B(0.8) C25A(0.6) H40A(0.6) H40B(0.6) C25B(0.8) H85A(0.8)
 H85B(0.8) C26A(0.6) H41A(0.6) H41B(0.6) C26B(0.8) H86A(0.8) H86B(0.8)
 C27A(0.6) H43A(0.6) H43B(0.6) C27B(0.8) H88A(0.8) H88B(0.8) C28A(0.6)
 H44A(0.6) H44B(0.6) C28B(0.8) H89A(0.8) H89B(0.8) C32(0.5) H7SA(0.5) H7SB(0.5)
 H7SC(0.5) C34(0.5) H8SA(0.5) H8SB(0.5) H8SC(0.5) O14(0.2)
6.a Free rotating group:
 O12(H12A,H12B), O13(H10A,H10B)
6.b Secondary CH2 refined with riding coordinates:
 C21C(H21A,H21B), C22C(H22A,H22B), C23C(H23A,H23B), C24C(H24A,H24B), C25C(H25A,
 H25B), C26C(H26A,H26B), C27C(H27A,H27B), C28C(H28A,H28B), C21D(H21C,H21D),
 C22D(H22C,H22D), C23D(H23C,H23D), C24D(H24C,H24D), C25D(H25C,H25D), C26D(H26C,
 H26D), C27D(H27C,H27D), C28D(H28C,H28D), C21A(H34A,H34B), C21B(H79A,H79B),
 C22A(H35A,H35B), C22B(H80A,H80B), C23A(H37A,H37B), C23B(H82A,H82B), C24A(H38A,
 H38B), C24B(H83A,H83B), C25A(H40A,H40B), C25B(H85A,H85B), C26A(H41A,H41B),
 C26B(H86A,H86B), C27A(H43A,H43B), C27B(H88A,H88B), C28A(H44A,H44B), C28B(H89A,
 H89B)
6.c Aromatic/amide H refined with riding coordinates:
 N1A(H1A), N2A(H2A), N4A(H4A), C4A(H4AA), C5A(H5A), C7A(H7A), C8A(H8A),
 C10A(H10C), C11A(H11A), C13A(H13A), C14A(H14A), C17A(H17A), C20A(H20A),
 N2B(H2B), N3B(H3B), N4B(H4B), C4B(H4BA), C5B(H5B), C7B(H7B), C8B(H8B),
 C10B(H10D), C11B(H11B), C13B(H13B), C14B(H14B), C17B(H17B), C20B(H20B)
6.d Idealised Me refined as rotating group:
 C35(H35C,H35D,H35E), C37(H37C,H37D,H37E), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C32(H7SA,H7SB,H7SC), C34(H8SA,H8SB,H8SC)
;
_olex2_date_sample_data_collection 26.11.2012
_olex2_submission_original_sample_id R1
_olex2_submission_special_instructions 'No special instructions were received'