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_7038573
_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(C3 H7 N O), I'
_chemical_formula_sum            'C57.5 H63.5 I N12.5 O22.5 Rb'
_chemical_formula_weight         1502.07
_chemical_name_systematic
;
 ?
;
_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             2015-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
2015-09-17 deposited with the CCDC.
2016-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.788(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4923(4)
_cell_length_b                   25.4062(6)
_cell_length_c                   16.2455(4)
_cell_measurement_reflns_used    10684
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.1540
_cell_measurement_theta_min      4.0980
_cell_volume                     6349.4(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega -110.00  -23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4013  -37.0000  -90.0000 87

  2 omega -110.00  -24.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4013  -37.0000    0.0000 86

  3 omega   34.00   99.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -45.0000   60.0000 65

  4 omega   76.00  153.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   61.0000  -30.0000 77

  5 omega   29.00   83.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000    0.0000 54

  6 omega   36.00  121.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818 -125.0000   60.0000 85

  7 omega   35.00   76.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000  150.0000 41

  8 omega   36.00   88.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000 -150.0000 52
;
_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      0.0814436000
_diffrn_orient_matrix_UB_12      -0.0141107000
_diffrn_orient_matrix_UB_13      -0.0413279000
_diffrn_orient_matrix_UB_21      0.0581085000
_diffrn_orient_matrix_UB_22      0.0149288000
_diffrn_orient_matrix_UB_23      0.0801872000
_diffrn_orient_matrix_UB_31      -0.0049809000
_diffrn_orient_matrix_UB_32      -0.0570901000
_diffrn_orient_matrix_UB_33      0.0311105000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15987
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.744
_diffrn_reflns_theta_min         3.245
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.652
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58482
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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    1.571
_exptl_crystal_description       plate
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.0895
_exptl_crystal_size_min          0.0405
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         15987
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0904P)^2^+4.4056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13164
_reflns_number_total             15987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00414h2.cif
_cod_data_source_block           R1_RbI
_cod_depositor_comments
'Adding full bibliography for 7038560--7038573.cif.'
_cod_original_formula_sum        'C57.50 H63.50 I N12.50 O22.50 Rb'
_cod_database_code               7038573
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H30 N6 O11 Rb1 I1'
_reflns_odcompleteness_completeness 98.77
_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
 C31-N7
 1.45 with sigma of 0.02
 N7-C29
 1.33 with sigma of 0.02
 C29-O12
 1.23 with sigma of 0.02
 N7-C30
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C29) = Uanis(O12)
Uanis(C30) = Uanis(C31)
4. Others
 Fixed Sof: O12(0.5) C29(0.5) H29(0.5) C30(0.5) H7C(0.5) H30(0.5) H7D(0.5)
 C31(0.5) H31A(0.5) H31B(0.5) H31C(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), C26A(H26A,H26B), C26B(H26C,H26D), C27A(H27A,H27B), C27B(H27C,
 H27D), C28A(H28A,H28B), C28B(H28C,H28D)
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), 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)
5.c Idealised Me refined as rotating group:
 C30(H7C,H30,H7D), C31(H31A,H31B,H31C)
;
_olex2_date_sample_data_collection 3.2.2015
_olex2_submission_special_instructions 'No special instructions were received'