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_7038563
_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         'C28 H30 N6 O11, C2 H6 O S'
_chemical_formula_sum            'C30 H36 N6 O12 S'
_chemical_formula_weight         704.71
_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             2015-06-25
_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                86.562(3)
_cell_angle_beta                 89.252(3)
_cell_angle_gamma                80.827(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8481(3)
_cell_length_b                   10.1334(4)
_cell_length_c                   18.5466(6)
_cell_measurement_reflns_used    5701
_cell_measurement_temperature    134.41(10)
_cell_measurement_theta_max      74.2980
_cell_measurement_theta_min      4.4140
_cell_volume                     1638.68(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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_environment      N~2~
_diffrn_ambient_temperature      134.41(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega  -49.00   32.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   37.0000    0.0000 81

  2 omega    1.00   81.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.6513  -99.0000   90.0000 80

  3 omega   38.00  121.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.2851 -125.0000   30.0000 83

  4 omega   59.00   99.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.2851  -45.0000  150.0000 40

  5 omega   31.00  126.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.2851  -77.0000   30.0000 95

  6 omega   81.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.2851   45.0000 -150.0000 97

  7 omega   94.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.2851  125.0000   30.0000 84

  8 omega   81.00  174.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.2851   61.0000  150.0000 93

  9 omega   76.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.2851   77.0000   90.0000 102

 10 omega   31.00  107.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.2851  -94.0000 -180.0000 76

 11 omega -114.00  -14.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  -57.0000 -150.0000 100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1693412000
_diffrn_orient_matrix_UB_12      -0.0653700000
_diffrn_orient_matrix_UB_13      -0.0032045000
_diffrn_orient_matrix_UB_21      0.0424868000
_diffrn_orient_matrix_UB_22      0.1037017000
_diffrn_orient_matrix_UB_23      0.0504268000
_diffrn_orient_matrix_UB_31      -0.0249853000
_diffrn_orient_matrix_UB_32      -0.0936466000
_diffrn_orient_matrix_UB_33      0.0661177000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9087
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.741
_diffrn_reflns_theta_min         4.427
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.3294
_exptl_crystal_size_mid          0.1606
_exptl_crystal_size_min          0.0817
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         5740
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0849P)^2^+1.4743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5067
_reflns_number_total             5740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00414h2.cif
_cod_data_source_block           R1_DMSO
_cod_depositor_comments
'Adding full bibliography for 7038560--7038573.cif.'
_cod_original_cell_volume        1638.69(10)
_cod_database_code               7038563
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C28 H28 N6 O12 Na1 F1'
_reflns_odcompleteness_completeness 98.58
_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
2. Restrained distances
 O10A-C27A = O10A-C26A
 1.42 with sigma of 0.02
 C28A-C27A
 1.51 with sigma of 0.02
 O11A-C28A
 1.42 with sigma of 0.02
 C25B-O9B
 1.42 with sigma of 0.02
 C25A-O9B
 1.42 with sigma of 0.02
 O10B-C27B = O10B-C26B
 1.42 with sigma of 0.02
 C25B-C26B
 1.51 with sigma of 0.02
 C26A-C25A = C25B-C26B
 1.51 with sigma of 0.02
 C27B-C28B
 1.51 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O10A) = Uanis(O10B)
Uanis(C27B) = Uanis(C27A)
Uanis(O10B) = Uanis(O10A)
Uanis(C25B) = Uanis(C25A)
Uanis(C26A) = Uanis(C26B)
Uanis(C26B) = Uanis(C26A)
Uanis(C28B) = Uanis(C28A)
4. Others
 Fixed Sof: O10B(0.5) O11B(0.5) C25B(0.5) H25A(0.5) H25B(0.5) C26B(0.5)
 H26A(0.5) H26B(0.5) C27B(0.5) H27A(0.5) H27B(0.5) C28B(0.5) H28A(0.5)
 H28B(0.5) O10A(0.5) O11A(0.5) C25A(0.5) H40A(0.5) H40B(0.5) C26A(0.5)
 H41A(0.5) H41B(0.5) C27A(0.5) H43A(0.5) H43B(0.5) C28A(0.5) H44A(0.5) H44B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25B(H25A,
 H25B), C26B(H26A,H26B), C27B(H27A,H27B), C28B(H28A,H28B), C25A(H40A,H40B),
 C26A(H41A,H41B), C27A(H43A,H43B), C28A(H44A,H44B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), C4(H4A), C5(H5), C7(H7), C8(H8), C10(H10),
 C11(H11), C13(H13), C14(H14), C17(H17), C20(H20)
5.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_olex2_date_sample_data_collection 26.9.2014
_olex2_submission_special_instructions 'No special instructions were received'