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_7038568
_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 K N12 O22, H2 O, Cl'
_chemical_formula_sum            'C56 H62 Cl K N12 O23'
_chemical_formula_weight         1345.72
_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             2015-06-26
_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                105.004(2)
_cell_angle_beta                 97.408(2)
_cell_angle_gamma                109.292(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5214(2)
_cell_length_b                   15.4120(4)
_cell_length_c                   21.1832(5)
_cell_measurement_reflns_used    11120
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.0840
_cell_measurement_theta_min      4.4260
_cell_volume                     3043.68(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      123.01(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   27.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   37.0000 -150.0000 76

  2 omega   23.00   98.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.6513 -125.0000  -30.0000 75

  3 omega   35.00  121.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      105.0818 -125.0000   60.0000 86

  4 omega   54.00   99.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -45.0000   90.0000 45

  5 omega   86.00  171.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   45.0000  150.0000 85

  6 omega   94.00  178.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  125.0000   90.0000 84

  7 omega   52.00  178.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   15.0000  -90.0000 126

  8 omega  102.00  178.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  125.0000 -180.0000 76

  9 omega   37.00  133.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -61.0000 -180.0000 96

 10 omega   22.00  109.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -94.0000  120.0000 87

 11 omega -122.00   -1.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  -19.0000   30.0000 121
;
_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      -0.1029641000
_diffrn_orient_matrix_UB_12      -0.0952647000
_diffrn_orient_matrix_UB_13      -0.0530661000
_diffrn_orient_matrix_UB_21      -0.0447264000
_diffrn_orient_matrix_UB_22      0.0585321000
_diffrn_orient_matrix_UB_23      -0.0410681000
_diffrn_orient_matrix_UB_31      0.1134628000
_diffrn_orient_matrix_UB_32      -0.0036139000
_diffrn_orient_matrix_UB_33      -0.0387098000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17614
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.748
_diffrn_reflns_theta_min         3.209
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.957
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.2021
_exptl_crystal_size_mid          0.1879
_exptl_crystal_size_min          0.1025
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         10659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0542
_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^)+(0.1027P)^2^+0.9218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9612
_reflns_number_total             10659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00414h2.cif
_cod_data_source_block           R1_KCl
_cod_depositor_comments
'Adding full bibliography for 7038560--7038573.cif.'
_cod_original_cell_volume        3043.69(14)
_cod_database_code               7038568
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C56 H56 N12 O23 K2 Cl2'
_reflns_odcompleteness_completeness 98.54
_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 O(H,H) groups
2.a Free rotating group:
 O12(H12a,H12b)
2.b Secondary CH2 refined with riding coordinates:
 C21A(H21c,H21d), C21B(H21a,H21b), C22A(H22a,H22b), C22B(H22c,H22d), C23A(H23c,
 H23d), C23B(H23a,H23b), C24A(H24a,H24b), C24B(H24c,H24d), C25A(H25a,H25b),
 C25B(H25c,H25d), C26A(H26c,H26d), C26B(H26a,H26b), C27A(H27a,H27b), C27B(H27c,
 H27d), C28A(H28c,H28d), C28B(H28a,H28b)
2.c Aromatic/amide H refined with riding coordinates:
 N1A(H1A), N1B(H1B), N2A(H2A), N2B(H2B), N3A(H3Aa), N3B(H3B), N4A(H4A),
 N4B(H4B), C3A(H3A), C3B(H3Ba), C4A(H4Aa), C4B(H4Ba), C6A(H6A), C6B(H6B),
 C7A(H7A), C7B(H7B), C10A(H10A), C10B(H10B), C11A(H11A), C11B(H11B), C13A(H13A),
  C13B(H13B), C14A(H14A), C14B(H14B), C17A(H17A), C17B(H17B), C20A(H20A),
 C20B(H20B)
;
_olex2_date_sample_data_collection 21.5.2015
_olex2_submission_special_instructions 'No special instructions were received'