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_4346486
_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, H4 N, Br'
_chemical_formula_sum            'C30 H38 Br N7 O12'
_chemical_formula_weight         768.58
_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_length_c                   31.0693(4)
_cell_measurement_reflns_used    7402
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.2040
_cell_measurement_theta_min      4.4810
_cell_volume                     3346.68(8)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 5.1977
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
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  1 omega -114.00  -13.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176  -57.0000    0.0000 101

  2 omega  -48.00   33.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176   37.0000  150.0000 81

  3 omega  100.00  171.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000   60.0000 71

  4 omega   53.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  120.0000 38

  5 omega   53.00  145.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  -30.0000 92

  6 omega   36.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   30.0000 55

  7 omega   51.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -30.0000 40

  8 omega   79.00  168.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  150.0000 89
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_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0241265000
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_diffrn_orient_matrix_UB_22      0.0794694000
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_diffrn_orient_matrix_UB_32      -0.0455855000
_diffrn_orient_matrix_UB_33      0.0002252000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            10069
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.747
_diffrn_reflns_theta_min         3.764
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.316
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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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)
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_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_recrystallization_method
'Diffusion of diethyl ether into MeOH/DMF solution'
_exptl_crystal_size_max          0.3488
_exptl_crystal_size_mid          0.1463
_exptl_crystal_size_min          0.0657
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_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         5845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0310
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_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^)+(0.0360P)^2^+1.8115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0736
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_reflns_number_gt                5467
_reflns_number_total             5845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01577_si_015.cif
_cod_data_source_block           R1-NH4Br
_cod_database_code               4346486
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H36 N7 O11 Br1'
_reflns_odcompleteness_completeness 98.59
_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.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)
2.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              54491
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_olex2_submission_special_instructions 'No special instructions were received'