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_7038564
_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         '2(C28 H30 Cl N6 Na O11)'
_chemical_formula_sum            'C56 H60 Cl2 N12 Na2 O22'
_chemical_formula_weight         1370.04
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-30
_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                 90.8013(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.83850(18)
_cell_length_b                   23.7838(3)
_cell_length_c                   18.5462(2)
_cell_measurement_reflns_used    11513
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      75.6500
_cell_measurement_theta_min      3.3440
_cell_volume                     6985.67(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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_temperature      123.01(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega -113.00  -14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176  -57.0000   30.0000 99

  2 omega -130.00  -33.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000  -30.0000   90.0000 97

  3 omega   41.00   99.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -180.0000 58

  4 omega   61.00  151.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000 -180.0000 90

  5 omega   39.00   96.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -120.0000 57

  6 omega   36.00   64.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  150.0000 28

  7 omega  127.00  178.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000  -30.0000 51

  8 omega   36.00   90.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 54

  9 omega   43.00   98.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  120.0000 55
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0872456000
_diffrn_orient_matrix_UB_12      0.0044469000
_diffrn_orient_matrix_UB_13      0.0352707000
_diffrn_orient_matrix_UB_21      -0.0415620000
_diffrn_orient_matrix_UB_22      -0.0250638000
_diffrn_orient_matrix_UB_23      -0.0683069000
_diffrn_orient_matrix_UB_31      0.0109579000
_diffrn_orient_matrix_UB_32      -0.0595891000
_diffrn_orient_matrix_UB_33      0.0314406000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25224
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.749
_diffrn_reflns_theta_min         3.353
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.638
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.3592
_exptl_crystal_size_mid          0.2337
_exptl_crystal_size_min          0.179
_refine_diff_density_max         2.107
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         12292
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0658
_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^)+(0.1326P)^2^+3.7698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2023
_refine_ls_wR_factor_ref         0.2092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10679
_reflns_number_total             12292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00414h2.cif
_cod_data_source_block           R1_NaCl
_cod_depositor_comments
'Adding full bibliography for 7038560--7038573.cif.'
_cod_original_cell_volume        6985.69(14)
_cod_database_code               7038564
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C28 H30 N6 O11 Na1 Cl1'
_reflns_odcompleteness_completeness 98.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
2. Rigid bond restraints
 C28B, O8C, O9C, O10C, C23C, C24C, C25C, C26C, C27C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O8B, O9B, O10B, C23B, C24B, C25B, C26B, C27B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C23C) = Uanis(C23B)
4. Others
 Fixed Sof: H22A(0.5) H22B(0.5) H22C(0.5) H22D(0.5) H28A(0.5) H28B(0.5)
 H28C(0.5) H28D(0.5) O8B(0.5) O9B(0.5) O10B(0.5) C23B(0.5) H23A(0.5) H23B(0.5)
 C24B(0.5) H24A(0.5) H24B(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) O8C(0.5) O9C(0.5) O10C(0.5)
 C23C(0.5) H23C(0.5) H23D(0.5) C24C(0.5) H24C(0.5) H24D(0.5) C25C(0.5)
 H25C(0.5) H25D(0.5) C26C(0.5) H26C(0.5) H26D(0.5) C27C(0.5) H27C(0.5) H27D(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C21A(H21C,H21D), C22A(H22E,H22F), C23A(H23E,H23F), C24A(H24E,H24F), C25A(H25E,
 H25F), C26A(H26E,H26F), C27A(H27E,H27F), C28A(H28E,H28F), C21B(H21A,H21B),
 C22B(H22A,H22B), C22B(H22C,H22D), C28B(H28A,H28B), C28B(H28C,H28D), C23B(H23A,
 H23B), C24B(H24A,H24B), C25B(H25A,H25B), C26B(H26A,H26B), C27B(H27A,H27B),
 C23C(H23C,H23D), C24C(H24C,H24D), C25C(H25C,H25D), C26C(H26C,H26D), C27C(H27C,
 H27D)
5.b Aromatic/amide H refined with riding coordinates:
 N1A(H1A), N2A(H2A), N3A(H3A), N4A(H4A), C4A(H4AA), C5A(H5A), C7A(H7A),
 C8A(H8A), C10A(H10A), C11A(H11A), C13A(H13A), C14A(H14A), C17A(H17A),
 C20A(H20A), N1B(H1B), N2B(H2B), N3B(H3B), N4B(H4B), C4B(H4BA), C5B(H5B),
 C7B(H7B), C8B(H8B), C10B(H10B), C11B(H11B), C13B(H13B), C14B(H14B), C17B(H17B),
  C20B(H20B)
;
_olex2_date_sample_data_collection 10.7.2013
_olex2_submission_special_instructions 'No special instructions were received'