Cooperatively enhanced ion pair binding with a hybrid receptor.
Mäkelä, Toni; Kalenius, Elina; Rissanen, Kari; Inorganic chemistry 54 (2015) 9154–9165; doi:10.1021/acs.inorgchem.5b01577

data_4346492
_publ_section_title
;
 Cooperatively enhanced ion pair binding with a hybrid receptor.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9154
_journal_page_last               9165
_journal_paper_doi               10.1021/acs.inorgchem.5b01577
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C30 H34 N6 O12, C0.5 H2 O0.5'
_chemical_formula_sum            'C30.5 H36 N6 O12.5'
_chemical_formula_weight         686.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-11
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.7387(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8305(2)
_cell_length_b                   13.83565(19)
_cell_length_c                   17.9254(3)
_cell_measurement_reflns_used    5715
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      75.6910
_cell_measurement_theta_min      3.2040
_cell_volume                     3406.40(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega -113.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2426  -77.0000 -150.0000 101

  2 omega -119.00  -18.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2426  -19.0000   60.0000 101

  3 omega   36.00   87.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -60.0000 51

  4 omega   30.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -30.0000 77

  5 omega   60.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -150.0000 31

  6 omega   66.00  141.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000    0.0000 75

  7 omega   37.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   90.0000 54

  8 omega   43.00  145.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000   30.0000 102
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0288643000
_diffrn_orient_matrix_UB_12      -0.0121358000
_diffrn_orient_matrix_UB_13      0.0851269000
_diffrn_orient_matrix_UB_21      0.0839246000
_diffrn_orient_matrix_UB_22      -0.0675309000
_diffrn_orient_matrix_UB_23      -0.0155555000
_diffrn_orient_matrix_UB_31      0.0686186000
_diffrn_orient_matrix_UB_32      0.0876747000
_diffrn_orient_matrix_UB_33      -0.0002062000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10604
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.744
_diffrn_reflns_theta_min         4.047
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.767
_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    1.339
_exptl_crystal_description       plate
_exptl_crystal_F_000             1444
_exptl_crystal_recrystallization_method
'Diffusion of methanol into DMF solution'
_exptl_crystal_size_max          0.5102
_exptl_crystal_size_mid          0.3416
_exptl_crystal_size_min          0.0736
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         5984
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.1195
_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^)+(0.1157P)^2^+15.6693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3215
_refine_ls_wR_factor_ref         0.3246
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5533
_reflns_number_total             5984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01577_si_004.cif
_cod_data_source_block           R1
_cod_original_cell_volume        3406.41(9)
_cod_original_formula_sum        'C30.50 H36 N6 O12.50'
_cod_database_code               4346492
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H34 N6 O12'
_reflns_odcompleteness_completeness 98.62
_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 N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C9A-C10A = C9A-C14A = C13A-C14A = C12A-C13A = C10A-C11A = C11A-C12A
 1.39 with sigma of 0.02
 O6A-N6A = O5A-N6A
 1.22 with sigma of 0.02
 C14B-C9B = C14B-C13B = C13B-C12B = C11B-C12B = C10B-C9B = C11B-C10B
 1.39 with sigma of 0.02
 O5B-N6B = O6B-N6B
 1.22 with sigma of 0.02
 H31C-H29A
 2 with sigma of 0.02
3. Rigid bond restraints
 C9A, C10A, C11A, C12A, C13A, C14A, N6A, O6A, O5A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9B, C10B, C11B, C12B, C13B, C14B, N6B, O5B, O6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N6B \\sim N6A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
O6B \\sim O6A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
O5B \\sim O5A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C11A \\sim C11B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C31A \\sim C31B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
Uanis(O6A) \\sim Ueq, Uanis(O5A) \\sim Ueq: with sigma of 0.025 and sigma for
terminal atoms of 0.025
5. Others
 Fixed Sof: O5A(0.5) O5B(0.5) O6A(0.5) O6B(0.5) O13(0.5) H13(0.25) H13C(0.25)
 H4A(0.5) H4B(0.5) N6A(0.5) N6B(0.5) C9A(0.5) C9B(0.5) C10A(0.5) H10A(0.5)
 C10B(0.5) H10B(0.5) C11A(0.5) H11A(0.5) C11B(0.5) H11B(0.5) C12A(0.5)
 C12B(0.5) C13A(0.5) H13A(0.5) C13B(0.5) H13B(0.5) C14A(0.5) H14A(0.5)
 C14B(0.5) H14B(0.5) C31A(0.25) H31A(0.25) H31B(0.25) H31C(0.25) C31B(0.25)
 H31D(0.25) H31E(0.25) H31F(0.25)
6.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), C29(H29A,H29B),
 C30(H30A,H30B)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4A), N4(H4B), C3(H3A), C4(H4), C6(H6), C7(H7),
 C10A(H10A), C10B(H10B), C11A(H11A), C11B(H11B), C13A(H13A), C13B(H13B),
 C14A(H14A), C14B(H14B), C17(H17), C20(H20)
6.c Tetrahedral OH refined with riding coordinates:
 O13(H13), O13(H13C)
6.d Idealised Me refined as rotating group:
 C31A(H31A,H31B,H31C), C31B(H31D,H31E,H31F)
;
_shelx_res_checksum              4557
_shelx_hkl_checksum              32412
_olex2_submission_special_instructions 'No special instructions were received'