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_4344665
_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         'C30 H32 Cl N2 O10 Rb U, 1.5(C2 H3 N)'
_chemical_formula_sum            'C33 H36.5 Cl N3.5 O10 Rb U'
_chemical_formula_weight         1001.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.099(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9380(3)
_cell_length_b                   15.8870(2)
_cell_length_c                   15.9668(3)
_cell_measurement_reflns_used    7772
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.5457
_cell_measurement_theta_min      2.9095
_cell_volume                     3718.78(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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      173
_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  -70.00  -25.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.5108  111.0000  171.9689 45

  2 omega   -1.00   85.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2921   77.0000   90.0000 86

  3 omega    3.00   90.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2921   57.0000 -150.0000 87
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0223157000
_diffrn_orient_matrix_UB_12      -0.0010468000
_diffrn_orient_matrix_UB_13      -0.0306348000
_diffrn_orient_matrix_UB_21      -0.0397111000
_diffrn_orient_matrix_UB_22      -0.0175629000
_diffrn_orient_matrix_UB_23      -0.0340067000
_diffrn_orient_matrix_UB_31      -0.0164202000
_diffrn_orient_matrix_UB_32      0.0410365000
_diffrn_orient_matrix_UB_33      -0.0153304000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18725
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.915
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.795
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_description       block
_exptl_crystal_F_000             1940
_exptl_crystal_recrystallization_method 'Diffusion of EtOAc into ACN/MeoH/DMSO'
_exptl_crystal_size_max          0.2579
_exptl_crystal_size_mid          0.2468
_exptl_crystal_size_min          0.1106
_refine_diff_density_max         1.290
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6507
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+5.9687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5703
_reflns_number_total             6507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02780_si_018.cif
_cod_data_source_block           R2_RbCl
_cod_original_cell_volume        3718.77(13)
_cod_original_formula_sum        'C33 H36.50 Cl N3.50 O10 Rb U'
_cod_database_code               4344665
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H32 N2 O10 Rb1 Cl1'
_reflns_odcompleteness_completeness 99.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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
2. Restrained distances
 N4-C33
 1.13 with sigma of 0.01
 C34-C33
 1.43 with sigma of 0.01
 N4-C34
 2.57 with sigma of 0.01
 H32C-H34A
 2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(N4)
Uanis(C33) = Uanis(C34)
4. Others
 Fixed Sof: N4(0.5) C33(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
5.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)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C11(H11), C12(H12), C13(H13),
 C14(H14), C17(H17), C20(H20)
5.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C32(H32A,H32B,H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'