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_4344674
_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         'C28 H30 Cl Li N2 O10 U, 1.44(H4.5 O2.25), O'
_chemical_formula_sum            'C28 H36.5 Cl Li N2 O14.25 U'
_chemical_formula_weight         909.51
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.620(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.9290(3)
_cell_length_b                   18.4658(3)
_cell_length_c                   23.7388(5)
_cell_measurement_reflns_used    6561
_cell_measurement_temperature    170
_cell_measurement_theta_max      28.9500
_cell_measurement_theta_min      2.2140
_cell_volume                     7268.8(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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      170
_diffrn_detector_area_resol_mean 16.0107
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   -1.00   85.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2431   57.0000  120.0000 86

  2 omega  -48.00   42.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2431  -77.0000    0.0000 90
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0071925000
_diffrn_orient_matrix_UB_12      -0.0328337000
_diffrn_orient_matrix_UB_13      0.0157279000
_diffrn_orient_matrix_UB_21      -0.0107032000
_diffrn_orient_matrix_UB_22      -0.0199357000
_diffrn_orient_matrix_UB_23      -0.0259848000
_diffrn_orient_matrix_UB_31      0.0407361000
_diffrn_orient_matrix_UB_32      0.0005762000
_diffrn_orient_matrix_UB_33      -0.0031420000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_laue_measured_fraction_full 0.967
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14277
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.220
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.603
_exptl_absorpt_correction_T_max  0.874
_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    1.662
_exptl_crystal_description       block
_exptl_crystal_F_000             3556
_exptl_crystal_recrystallization_method 'Evaporation of acetonitrile'
_exptl_crystal_size_max          0.1258
_exptl_crystal_size_mid          0.0623
_exptl_crystal_size_min          0.0295
_refine_diff_density_max         1.604
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         6365
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0316P)^2^+6.5565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5461
_reflns_number_total             6365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02780_si_004.cif
_cod_data_source_block           R1_LiCl
_cod_original_formula_sum        'C28 H36.50 Cl Li N2 O14.25 U'
_cod_database_code               4344674
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H31 N2 O11 Li1 Cl1 U1'
_reflns_odcompleteness_completeness 98.86
_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 O(H,H) groups
2. Restrained distances
 H13B-H12A
 2.1 with sigma of 0.01
 H10A-H10_$1
 2.1 with sigma of 0.005
3. Others
 Fixed Sof: O14(0.25) H14A(0.25) H14B(0.25)
4.a Free rotating group:
 O12(H12A,H12B), O15(H15A,H15B), O14(H14A,H14B)
4.b Rotating group:
 O10(H10A,H10B), O13(H13A,H13B)
4.c 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)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C17(H17), C20(H20)
;
_olex2_submission_special_instructions 'No special instructions were received'