Ion Pair Binding in the Solid-State with Ditopic Crown Ether Uranyl Salophen Receptors.
Mäkelä, Toni; Minkkinen, Miia-Elina; Rissanen, Kari; Inorganic chemistry 55 (2016) 1339–1346; doi:10.1021/acs.inorgchem.5b02780

data_4344660
_publ_section_title
;
 Ion Pair Binding in the Solid-State with Ditopic Crown Ether Uranyl
 Salophen Receptors.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1339
_journal_page_last               1346
_journal_paper_doi               10.1021/acs.inorgchem.5b02780
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C32 H32 Br N3 Na O10 U, 2(C34 H40 N4 Na O11 U), 2(C30 H36 N2 Na O12 U), 3(C2 H3 N), H2 O, H O, 4(Br)'
_chemical_formula_sum            'C166 H196 Br5 N18 Na5 O58 U5'
_chemical_formula_weight         5076.05
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-10-13
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.3064(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.55643(15)
_cell_length_b                   55.9218(9)
_cell_length_c                   25.9826(5)
_cell_measurement_reflns_used    21586
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7580
_cell_measurement_theta_min      1.9820
_cell_volume                     19692.3(5)
_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      293(2)
_diffrn_detector_area_resol_mean 16.0107
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega    5.00   81.00   0.5000   95.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2431   57.0000   30.0000 152

  2 omega  -47.00   43.00   0.5000   95.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2431  -77.0000  -90.0000 180
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0484236000
_diffrn_orient_matrix_UB_12      -0.0048071000
_diffrn_orient_matrix_UB_13      0.0006037000
_diffrn_orient_matrix_UB_21      0.0196169000
_diffrn_orient_matrix_UB_22      0.0115872000
_diffrn_orient_matrix_UB_23      -0.0041177000
_diffrn_orient_matrix_UB_31      0.0031220000
_diffrn_orient_matrix_UB_32      0.0018801000
_diffrn_orient_matrix_UB_33      0.0269827000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0951
_diffrn_reflns_laue_measured_fraction_full 0.968
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       67
_diffrn_reflns_limit_k_min       -74
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            73377
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.858
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.207
_exptl_absorpt_correction_T_max  0.713
_exptl_absorpt_correction_T_min  0.648
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       block
_exptl_crystal_F_000             9888
_exptl_crystal_recrystallization_method
'Diffusion of diethyl ether into acetonitrile solution'
_exptl_crystal_size_max          0.1268
_exptl_crystal_size_mid          0.1105
_exptl_crystal_size_min          0.0965
_refine_diff_density_max         1.711
_refine_diff_density_min         -2.203
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2401
_refine_ls_number_reflns         34888
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0196P)^2^+135.3149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28554
_reflns_number_total             34888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02780_si_011.cif
_cod_data_source_block           R2_NaBr_2
_cod_database_code               4344660
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C40 H32 N2 O20 U1 Na1 Br1'
_reflns_odcompleteness_completeness 98.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C42B-C41
 1.45 with sigma of 0.01
 H14F-H11G_$1
 2.1 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C15F \\sim C15H: within 1.7A with sigma of 0.005 and sigma for terminal atoms
of 0.005
4. Others
 Fixed Sof: C15E(0.5) H15A(0.5) H15B(0.5) C15F(0.5) H15C(0.5) H15D(0.5)
 C15G(0.5) H15E(0.5) H15F(0.5) C15H(0.5) H15G(0.5) H15H(0.5) C42A(0.25)
 C42B(0.25) N11A(0.5) N11B(0.5) H46A(0.5) H46B(0.5) H46C(0.5) H50A(0.5)
 H50B(0.5) H50C(0.5)
5.a Free rotating group:
 O18(H18A,H18B)
5.b Rotating group:
 O13(H13E,H13F), O11(H11F,H11G), O14(H14E,H14F), O16(H16A,H16B), O12(H12H,
 H12I), O15(H15I,H15J)
5.c Secondary CH2 refined with riding coordinates:
 C11E(H11A,H11B), C11F(H11C,H11D), C12E(H12A,H12B), C12F(H12C,H12D), C13E(H13A,
 H13B), C13F(H13C,H13D), C14E(H14A,H14B), C14F(H14C,H14D), C15E(H15A,H15B),
 C15F(H15C,H15D), C15G(H15E,H15F), C15H(H15G,H15H), C21C(H21A,H21B), C22C(H22A,
 H22B), C23C(H23A,H23B), C24C(H24A,H24B), C25C(H25A,H25B), C26C(H26A,H26B),
 C27C(H27A,H27B), C28C(H28A,H28B), C29C(H29A,H29B), C30C(H30A,H30B), C21A(H21C,
 H21D), C22A(H22C,H22D), C23A(H23C,H23D), C24A(H24C,H24D), C25A(H25C,H25D),
 C26A(H26C,H26D), C27A(H27C,H27D), C28A(H28C,H28D), C29A(H29C,H29D), C30A(H30C,
 H30D), C21D(H21E,H21F), C22D(H22E,H22F), C23D(H23E,H23F), C24D(H24E,H24F),
 C25D(H25E,H25F), C26D(H26E,H26F), C27D(H27E,H27F), C28D(H28E,H28F), C29D(H29E,
 H29F), C30D(H30E,H30F), C21B(H21G,H21H), C22B(H22G,H22H), C23B(H23G,H23H),
 C24B(H24G,H24H), C25B(H25G,H25H), C26B(H26G,H26H), C27B(H27G,H27H), C28B(H28G,
 H28H), C29B(H29G,H29H), C30B(H30G,H30H)
5.d Aromatic/amide H refined with riding coordinates:
 C1E(H1E), C1F(H1F), C3E(H3E), C3F(H3F), C4E(H4E), C4F(H4F), C5E(H5E),
 C5F(H5F), C6E(H6E), C6F(H6F), C9E(H9E), C9F(H9F), C1C(H1C), C3C(H3C), C4C(H4C),
  C5C(H5C), C6C(H6C), C8C(H8C), C10C(H10C), C11C(H11E), C12C(H12E), C13C(H13G),
 C17C(H17C), C20C(H20C), C1A(H1A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A),
 C8A(H8A), C10A(H10A), C11A(H11H), C12A(H12F), C13A(H13H), C17A(H17A),
 C20A(H20A), C1D(H1D), C3D(H3D), C4D(H4D), C5D(H5D), C6D(H6D), C8D(H8D),
 C10D(H10D), C11D(H11I), C12D(H12G), C13D(H13I), C17D(H17D), C20D(H20D),
 C1B(H1B), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B), C8B(H8B), C10B(H10B),
 C11B(H11J), C12B(H12J), C13B(H13J), C17B(H17B), C20B(H20B)
5.e Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C48(H48A,H48B,H48C), C46(H46A,H46B,H46C), C44(H44A,H44B,H44C), C50(H50A,
 H50B,H50C)
;
_olex2_submission_special_instructions 'No special instructions were received'