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_7038565
_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         'C30 H33 N7 Na O11, O, Br'
_chemical_formula_sum            'C30 H33 Br N7 Na O12'
_chemical_formula_weight         786.53
_chemical_name_systematic
;
 ?
;
_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     direct
_audit_creation_date             2015-08-26
_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                72.838(3)
_cell_angle_beta                 87.307(2)
_cell_angle_gamma                87.437(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4682(3)
_cell_length_b                   12.1247(3)
_cell_length_c                   16.1742(5)
_cell_measurement_reflns_used    8343
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.1310
_cell_measurement_theta_min      4.6650
_cell_volume                     1771.22(9)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 5.1977
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega -113.00  -21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176  -57.0000  -90.0000 92

  2 omega   57.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6176 -125.0000 -120.0000 33

  3 omega  -82.00   18.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000   77.0000   60.0000 100

  4 omega  -24.00   16.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000   45.0000 -120.0000 40

  5 omega  -48.00   21.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000   30.0000 -150.0000 69

  6 omega   36.00  116.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -120.0000 80

  7 omega   45.00   88.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   30.0000 43

  8 omega   47.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -180.0000 51

  9 omega  117.00  145.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  -90.0000 28

 10 omega   36.00  104.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  -90.0000 68

 11 omega   40.00   99.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   90.0000 59

 12 omega   82.00  178.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   15.0000   60.0000 96

 13 omega   32.00  108.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000    0.0000 76

 14 omega   29.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   90.0000 80

 15 omega   59.00  178.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   15.0000    0.0000 119
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0724280000
_diffrn_orient_matrix_UB_12      -0.0062516000
_diffrn_orient_matrix_UB_13      0.0846600000
_diffrn_orient_matrix_UB_21      -0.1327709000
_diffrn_orient_matrix_UB_22      -0.0537226000
_diffrn_orient_matrix_UB_23      0.0525605000
_diffrn_orient_matrix_UB_31      0.0607192000
_diffrn_orient_matrix_UB_32      -0.1215617000
_diffrn_orient_matrix_UB_33      0.0044702000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11524
_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         66.747
_diffrn_reflns_theta_min         5.573
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.317
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.642
_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    1.475
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.2158
_exptl_crystal_size_min          0.0476
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         6209
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0454P)^2^+1.2094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5905
_reflns_number_total             6209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00414h2.cif
_cod_data_source_block           tcy-053_nabr_190713_abs2
_cod_depositor_comments
'Adding full bibliography for 7038560--7038573.cif.'
_cod_original_cell_volume        1771.21(9)
_cod_database_code               7038565
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C28 H28 N6 O11 Na1 Br1'
_reflns_odcompleteness_completeness 98.38
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-O10A
 1.43 with sigma of 0.01
 O10B-C27
 1.43 with sigma of 0.01
 O10A-C26A
 1.43 with sigma of 0.01
 O10B-C26B
 1.43 with sigma of 0.01
 C25-C26A
 1.5 with sigma of 0.01
 C26B-C25
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O10B) = Uanis(O10A)
Uanis(C26B) = Uanis(C26A)
4. Others
 Fixed Sof: O10A(0.9) O10B(0.1) H25A(0.8) H25B(0.8) H25C(0.2) H25D(0.2)
 C26A(0.8) H26A(0.8) H26B(0.8) C26B(0.2) H26C(0.2) H26D(0.2) H27A(0.9)
 H27B(0.9) H27C(0.1) H27D(0.1) O12(0.6) O13(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C25(H25C,H25D), C26A(H26A,H26B), C26B(H26C,H26D), C27(H27A,H27B),
 C27(H27C,H27D), C28(H28A,H28B)
5.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)
5.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C)
;
_olex2_date_sample_data_collection 19.7.2013
_olex2_submission_special_instructions 'No special instructions were received'