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_7038569
_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, C3 H7 N O, Br'
_chemical_formula_sum            'C59 H67 Br K N13 O23'
_chemical_formula_weight         1445.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 97.748(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9756(3)
_cell_length_b                   26.2676(5)
_cell_length_c                   16.2138(3)
_cell_measurement_reflns_used    7784
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.1130
_cell_measurement_theta_min      4.0980
_cell_volume                     6319.8(2)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -49.00   27.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013   37.0000  120.0000 76

  2 omega -117.00   -9.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013  -77.0000  -30.0000 108

  3 omega   41.00   99.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -45.0000 -180.0000 58

  4 omega   44.00   91.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000   60.0000 47

  5 omega   79.00  178.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   45.0000 -150.0000 99

  6 omega   78.00  178.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   30.0000  120.0000 100

  7 omega   32.00   94.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -45.0000 -120.0000 62
;
_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      0.1004664000
_diffrn_orient_matrix_UB_12      -0.0019714000
_diffrn_orient_matrix_UB_13      0.0363107000
_diffrn_orient_matrix_UB_21      -0.0201190000
_diffrn_orient_matrix_UB_22      0.0316371000
_diffrn_orient_matrix_UB_23      0.0753544000
_diffrn_orient_matrix_UB_31      -0.0169654000
_diffrn_orient_matrix_UB_32      -0.0493486000
_diffrn_orient_matrix_UB_33      0.0467953000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20073
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.741
_diffrn_reflns_theta_min         3.225
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.265
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.785
_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    1.519
_exptl_crystal_description       plate
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.1436
_exptl_crystal_size_mid          0.0656
_exptl_crystal_size_min          0.0131
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         11056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.3647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8742
_reflns_number_total             11056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00414h2.cif
_cod_data_source_block           R1_KBr
_cod_depositor_comments
'Adding full bibliography for 7038560--7038573.cif.'
_cod_database_code               7038569
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C56 H60 N12 O22 K1 Br1'
_reflns_odcompleteness_completeness 98.49
_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.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), C26A(H26a,H26b), C26B(H26c,H26d), C27A(H27a,H27b), C27B(H27c,
 H27d), C28A(H28a,H28b), C28B(H28c,H28d)
2.b Aromatic/amide H refined with riding coordinates:
 N1A(H1A), N1B(H1B), N2A(H2A), N2B(H2B), N3A(H3A), N3B(H3B), N4A(H4A),
 N4B(H4B), C3A(H3Aa), 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), C29(H29)
2.c Idealised Me refined as rotating group:
 C30(H30a,H30b,H30c), C31(H31a,H31b,H31c)
;
_olex2_date_sample_data_collection 5.2.2015
_olex2_submission_special_instructions 'No special instructions were received'