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_7038566
_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 Na O11, C1.5 H3 O0.25, 0.5(H2 O), I'
_chemical_formula_sum            'C29.5 H31 I N6 Na O11.75'
_chemical_formula_weight         807.49
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                90
_cell_angle_beta                 100.291(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.1422(5)
_cell_length_b                   7.22931(19)
_cell_length_c                   42.6101(13)
_cell_measurement_reflns_used    9031
_cell_measurement_temperature    134.41(10)
_cell_measurement_theta_max      72.8130
_cell_measurement_theta_min      4.0430
_cell_volume                     6711.0(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -49.00   33.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   37.0000  -90.0000 82

  2 omega -114.00  -14.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  -57.0000  120.0000 100

  3 omega  -96.00   -2.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  125.0000  -30.0000 94

  4 omega   94.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  125.0000   30.0000 82

  5 omega   22.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -94.0000  -30.0000 87

  6 omega   29.00   64.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000   90.0000 35

  7 omega   81.00  171.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   30.0000 -150.0000 90

  8 omega   34.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818 -125.0000  -90.0000 87

  9 omega   78.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   30.0000  120.0000 98

 10 omega   29.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000  -60.0000 62

 11 omega   29.00  138.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -77.0000   60.0000 109
;
_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      0.0119188000
_diffrn_orient_matrix_UB_12      -0.1612585000
_diffrn_orient_matrix_UB_13      0.0239590000
_diffrn_orient_matrix_UB_21      0.0198764000
_diffrn_orient_matrix_UB_22      0.1386345000
_diffrn_orient_matrix_UB_23      0.0273472000
_diffrn_orient_matrix_UB_31      -0.0668095000
_diffrn_orient_matrix_UB_32      0.0125154000
_diffrn_orient_matrix_UB_33      0.0054346000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            19325
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.726
_diffrn_reflns_theta_min         4.058
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.240
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.216
_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    1.598
_exptl_crystal_description       needle
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.5371
_exptl_crystal_size_mid          0.0609
_exptl_crystal_size_min          0.0388
_refine_diff_density_max         0.983
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         5947
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0581P)^2^+3.4029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5434
_reflns_number_total             5947
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00414h2.cif
_cod_data_source_block           R1_NaI
_cod_depositor_comments
'Adding full bibliography for 7038560--7038573.cif.'
_cod_original_formula_sum        'C29.50 H31 I N6 Na O11.75'
_cod_database_code               7038566
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C28 H28 N6 O12 Na1 I1'
_reflns_odcompleteness_completeness 99.74
_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
 O12-C30
 1.21 with sigma of 0.01
 C29-C30 = C31-C30
 1.52 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C30) = Uanis(O12)
Uanis(C30) = Uanis(C31)
4. Others
 Fixed Sof: C23A(0.65) H23A(0.65) H23B(0.65) C24A(0.65) H24A(0.65) H24B(0.65)
 C23B(0.35) H23C(0.35) H23D(0.35) C24B(0.35) H24C(0.35) H24D(0.35) O12(0.25)
 C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C30(0.5) C31(0.5) H31A(0.5) H31B(0.5)
 H31C(0.5) O13(0.5) H13A(0.5) H13B(0.5)
5.a Free rotating group:
 O13(H13A,H13B)
5.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C23A(H23A,H23B), C24A(H24A,H24B), C23B(H23C,H23D),
 C24B(H24C,H24D)
5.c 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.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C31(H31A,H31B,H31C)
;
_olex2_date_sample_data_collection 29.9.2014
_olex2_submission_special_instructions 'No special instructions were received'