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_4344676
_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
'2(C28 H30 N2 O10 U), 0.5(C H4 O), 4.5(H2 O), 0.5(O)'
_chemical_formula_sum            'C56.5 H71 N4 O25.5 U2'
_chemical_formula_weight         1690.23
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-01-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.995(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6788(3)
_cell_length_b                   26.8778(4)
_cell_length_c                   16.5218(4)
_cell_measurement_reflns_used    7244
_cell_measurement_temperature    170
_cell_measurement_theta_max      28.3680
_cell_measurement_theta_min      2.2600
_cell_volume                     6324.9(2)
_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      170
_diffrn_detector_area_resol_mean 16.0107
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -5.00   79.00   1.0000  250.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2431   77.0000 -180.0000 84

  2 omega   -1.00   84.00   1.0000  250.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2431   57.0000   90.0000 85
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0431843000
_diffrn_orient_matrix_UB_12      0.0010701000
_diffrn_orient_matrix_UB_13      0.0119612000
_diffrn_orient_matrix_UB_21      0.0235420000
_diffrn_orient_matrix_UB_22      -0.0065707000
_diffrn_orient_matrix_UB_23      0.0413606000
_diffrn_orient_matrix_UB_31      0.0079051000
_diffrn_orient_matrix_UB_32      0.0255492000
_diffrn_orient_matrix_UB_33      0.0101343000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_laue_measured_fraction_full 0.970
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23777
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.831
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.199
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.776
_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    1.775
_exptl_crystal_description
;
;
_exptl_crystal_F_000             3304
_exptl_crystal_recrystallization_method
'Evaporation of acetonitrile with added NH4Cl'
_exptl_crystal_size_max          0.3591
_exptl_crystal_size_mid          0.0707
_exptl_crystal_size_min          0.0281
_refine_diff_density_max         1.374
_refine_diff_density_min         -1.344
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         11108
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0471P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8664
_reflns_number_total             11108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02780_si_002.cif
_cod_data_source_block           R1_H2O
_cod_original_formula_sum        'C56.50 H71 N4 O25.50 U2'
_cod_database_code               4344676
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C28 H32 N3 O9 U1 Cl1'
_reflns_odcompleteness_completeness 98.91
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups, All O(H,H,H,H) groups
2. Restrained distances
 O7B-C24C = O7B-C24B
 1.42 with sigma of 0.01
 C11C-C9B
 2.42 with sigma of 0.01
 C11C-C13C
 2.42 with sigma of 0.01
 H14A-O13
 1.9 with sigma of 0.02
 C9B-C14C = C13C-C14C = C13C-C12C = C11C-C12C = C11C-C10C = C9B-C10C
 1.4 with sigma of 0.01
 H25D-H18A
 2.1 with sigma of 0.01
 H17B-H8B
 2 with sigma of 0.01
 H10D-O7A_$1
 2 with sigma of 0.01
3. Rigid bond restraints
 U1B, O2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 U1C, O2C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C22B, O6C, C23C, C24C, O7B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C22B, O6B, C23B, C24B, O7B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C9B, C10B, C11B, C12B, C13B, C14B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C9B, C10C, C11C, C12C, C13C, C14C
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C24C \\sim C24B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
O2C \\sim O2B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C11B \\sim C11C: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
C14B \\sim C14C: within 1.7A with sigma of 0.005 and sigma for terminal atoms
of 0.005
C13B \\sim C13C: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.01
C23C \\sim C23B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
O6C \\sim O6B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.01
C10C \\sim C10B: within 1.7A with sigma of 0.005 and sigma for terminal atoms
of 0.005
O4B \\sim O4C: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.005
C12B \\sim C12C: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
Uanis(O6B) = Uanis(C23B)
Uanis(O6C) = Uanis(C23C)
Uanis(C12C) = Uanis(C12B)
Uanis(C11C) = Uanis(C12C)
Uanis(O19) = Uanis(C29)
5. Others
 Fixed Sof: U1B(0.7) U1C(0.3) O2B(0.7) O2C(0.3) O4B(0.7) O4C(0.3) O6B(0.5)
 O6C(0.5) H11A(0.7) H11B(0.7) H11C(0.3) H11D(0.3) C10B(0.7) H10B(0.7) C10C(0.3)
 H10C(0.3) C11B(0.7) H11E(0.7) C11C(0.3) H11F(0.3) C12B(0.7) H12B(0.7)
 C12C(0.3) H12C(0.3) C13B(0.7) H13B(0.7) C13C(0.3) H13C(0.3) C14B(0.7)
 C14C(0.3) H22A(0.5) H22B(0.5) H22C(0.5) H22D(0.5) C23B(0.5) H23A(0.5)
 H23B(0.5) C23C(0.5) H23C(0.5) H23D(0.5) C24B(0.5) H24A(0.5) H24B(0.5)
 C24C(0.5) H24C(0.5) H24D(0.5) O19(0.5) H19(0.5) C29(0.5) H29A(0.5) H29B(0.5)
 H29C(0.5) O17(0.5) H17C(0.5) H17D(0.5) O15(0.5) H15A(0.5) H15B(0.5) O18(0.5)
 H18A(0.5) H18B(0.5) O16(0.5)
6.a Riding coordinates:
 O11(H11A,H11B), O11(H11C,H11D)
6.b Free rotating group:
 O17(H17C,H17D), O15(H15A,H15B), O12(H12D,H12E), O18(H18A,H18B), O13(H13D,
 H13E), O14(H14A,H14B)
6.c Rotating group:
 O10(H10A,H10D)
6.d Secondary CH2 refined with riding coordinates:
 C21B(H21A,H21B), C22B(H22A,H22B), C22B(H22C,H22D), C23B(H23A,H23B), C23C(H23C,
 H23D), C24B(H24A,H24B), C24C(H24C,H24D), C25B(H25A,H25B), C26B(H26A,H26B),
 C27B(H27A,H27B), C28B(H28A,H28B), C21A(H21C,H21D), C22A(H22E,H22F), C23A(H23E,
 H23F), C24A(H24E,H24F), C25A(H25C,H25D), C26A(H26C,H26D), C27A(H27C,H27D),
 C28A(H28C,H28D)
6.e Aromatic/amide H refined with riding coordinates:
 C1B(H1B), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B), C8B(H8B), C10B(H10B),
 C10C(H10C), C11B(H11E), C11C(H11F), C12B(H12B), C12C(H12C), C13B(H13B),
 C13C(H13C), C17B(H17B), C20B(H20B), C1A(H1A), C3A(H3A), C4A(H4A), C5A(H5A),
 C6A(H6A), C8A(H8A), C10A(H10E), C11A(H11G), C12A(H12A), C13A(H13A), C17A(H17A),
  C20A(H20A)
6.f Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C)
6.g Idealised tetrahedral OH refined as rotating group:
 O19(H19)
;
_olex2_submission_special_instructions 'No special instructions were received'