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_4346481
_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         'Cl, C30 H34 N6 O12, H4 N'
_chemical_formula_sum            'C30 H38 Cl N7 O12'
_chemical_formula_weight         724.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-10
_audit_creation_method
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Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
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_cell_angle_alpha                90
_cell_angle_beta                 95.8401(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.79743(16)
_cell_length_b                   9.21367(13)
_cell_length_c                   30.7165(4)
_cell_measurement_reflns_used    6389
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.0390
_cell_measurement_theta_min      3.8890
_cell_volume                     3321.48(8)
_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      123.00(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega -109.00  -23.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7426  -37.0000   60.0000 86

  2 omega -107.00  -12.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7426  -77.0000 -180.0000 95

  3 omega   40.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   90.0000 37

  4 omega   29.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   90.0000 80

  5 omega   46.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -120.0000 45

  6 omega   39.00   87.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  120.0000 48

  7 omega   50.00   76.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -150.0000 26

  8 omega   39.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -180.0000 56

  9 omega   48.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   30.0000 43

 10 omega   36.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -30.0000 55
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0820935000
_diffrn_orient_matrix_UB_12      0.0257452000
_diffrn_orient_matrix_UB_13      -0.0415868000
_diffrn_orient_matrix_UB_21      -0.0929557000
_diffrn_orient_matrix_UB_22      0.0501754000
_diffrn_orient_matrix_UB_23      0.0284625000
_diffrn_orient_matrix_UB_31      0.0429422000
_diffrn_orient_matrix_UB_32      0.1573415000
_diffrn_orient_matrix_UB_33      -0.0022241000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            10013
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.747
_diffrn_reflns_theta_min         3.766
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.664
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.775
_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    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_recrystallization_method
'Diffusion of diethyl ether into MeOH/DMSO solution'
_exptl_crystal_size_max          0.2219
_exptl_crystal_size_mid          0.1602
_exptl_crystal_size_min          0.0801
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         5821
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0459P)^2^+0.9631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5293
_reflns_number_total             5821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01577_si_008.cif
_cod_data_source_block           R1-NH4Cl
_cod_original_cell_volume        3321.49(8)
_cod_database_code               4346481
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H38 N7 O12 Cl1'
_reflns_odcompleteness_completeness 98.58
_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
2. Restrained distances
 N7-H7A
 0.83 with sigma of 0.01
3.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)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), C3(H3A), C4(H4A), C6(H6), C7(H7), C10(H10),
 C11(H11), C13(H13), C14(H14), C17(H17), C20(H20)
;
_shelx_res_checksum              2079
_shelx_hkl_checksum              73
_olex2_submission_special_instructions 'No special instructions were received'