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_7038562
_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 O11, 2(C3 H7 N O)'
_chemical_formula_sum            'C34 H44 N8 O13'
_chemical_formula_weight         772.77
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-06-25
_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                101.4580(10)
_cell_angle_beta                 95.3000(10)
_cell_angle_gamma                100.4910(10)
_cell_formula_units_Z            2
_cell_length_a                   10.71590(10)
_cell_length_b                   11.3107(2)
_cell_length_c                   15.4992(3)
_cell_measurement_temperature    120(2)
_cell_volume                     1794.18(5)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23053
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.950
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0721 before and 0.0621 after correction. The Ratio of minimum to maximum transmission is 0.8754. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         6315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0443P)^2^+1.3666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5475
_reflns_number_total             6315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00414h2.cif
_cod_data_source_block           R1_DMF
_cod_depositor_comments
'Adding full bibliography for 7038560--7038573.cif.'
_cod_database_code               7038562
_shelxl_version_number           2014-3
_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:
 C21(H21a,H21b), C22(H22a,H22b), C23(H23a,H23b), C24(H24a,H24b), C25(H25a,
 H25b), C26(H26a,H26b), C27(H27a,H27b), C28(H28a,H28b)
2.b 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), C29(H29), C32(H32)
2.c Idealised Me refined as rotating group:
 C30(H30a,H30b,H30c), C31(H31a,H31b,H31c), C33(H33a,H33b,H33c), C34(H34a,H34b,
 H34c)
;
_olex2_date_sample_data_collection 17.9.2014
_olex2_submission_original_sample_id 'R1 + DMF'
_olex2_submission_special_instructions 'No special instructions were received'