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_4344661
_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 H36.5 K N3 O11 U, C30 H36 K N2 O12 U, 2.5(C2 H3 N), 2(H2 O), 2(I), 0.5(O)'
_chemical_formula_sum            'C67 H84 I2 K2 N7.5 O25.5 U2'
_chemical_formula_weight         2210.47
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                77.055(2)
_cell_angle_beta                 87.563(2)
_cell_angle_gamma                76.618(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7636(3)
_cell_length_b                   19.3246(5)
_cell_length_c                   20.1849(6)
_cell_measurement_reflns_used    13332
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      28.5060
_cell_measurement_theta_min      3.5020
_cell_volume                     3980.5(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      123.01(10)
_diffrn_detector_area_resol_mean 5.1977
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -61.00   33.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -        9.1326  -57.0000   90.0000 94

  2 omega  -15.00   78.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -        9.1326   57.0000 -120.0000 93

  3 omega  -20.00   50.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -        9.1326  -99.0000    0.0000 70
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0000742000
_diffrn_orient_matrix_UB_12      -0.0376214000
_diffrn_orient_matrix_UB_13      0.0094866000
_diffrn_orient_matrix_UB_21      0.0116310000
_diffrn_orient_matrix_UB_22      -0.0030158000
_diffrn_orient_matrix_UB_23      -0.0342068000
_diffrn_orient_matrix_UB_31      0.0667345000
_diffrn_orient_matrix_UB_32      -0.0084649000
_diffrn_orient_matrix_UB_33      0.0063325000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_laue_measured_fraction_full 0.965
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28271
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.855
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.022
_exptl_absorpt_correction_T_max  0.715
_exptl_absorpt_correction_T_min  0.447
_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    1.844
_exptl_crystal_description       block
_exptl_crystal_F_000             2141
_exptl_crystal_recrystallization_method
'Diffusion of diethyl ether into acetonitrile solution'
_exptl_crystal_size_max          0.1989
_exptl_crystal_size_mid          0.0905
_exptl_crystal_size_min          0.0759
_refine_diff_density_max         2.023
_refine_diff_density_min         -2.523
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     962
_refine_ls_number_reflns         13894
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0274P)^2^+17.2516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12169
_reflns_number_total             13894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02780_si_016.cif
_cod_data_source_block           R2_KI
_cod_original_cell_volume        3980.51(19)
_cod_original_formula_sum        'C67 H84 I2 K2 N7.50 O25.50 U2'
_cod_database_code               4344661
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H32 N2 O8 U1 K1 I1'
_reflns_odcompleteness_completeness 98.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H26B,H26A,H26C} of C26B, All C(H,H) groups, All C(H,H,H,
  H) groups
 At 1.5 times of:
  All O(H,H) groups, {H34A,H34B,H34C} of C34, {H32A,H32B,H32C} of C32, {H36A,
  H36B,H36C} of C36, {H38A,H38B,H38C} of C38
2. Restrained distances
 N6-C37
 1.13 with sigma of 0.005
 C37-C38
 1.42 with sigma of 0.005
 H30D_$1-H38C
 2.1 with sigma of 0.02
 H1A-H38A_$1
 2.1 with sigma of 0.01
 H38A_$1-H30D
 2.1 with sigma of 0.01
 H38A_$1-H20A
 2.1 with sigma of 0.005
 C34-N4 = C38-N6
 2.59 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(O8B) = Uanis(O9B)
Uanis(N3) = Uanis(C31)
Uanis(N6) = Uanis(C37)
Uanis(C37) = Uanis(C38)
Uanis(C32) = Uanis(C31)
Uanis(O13) = Uanis(O15)
4. Others
 Fixed Sof: O8B(0.5) O8C(0.5) H26B(0.5) H26A(0.5) H26C(0.5) H27A(0.5)
 H27B(0.5) H27C(0.5) H27D(0.5) N6(0.5) C37(0.5) C38(0.5) H38A(0.5) H38B(0.5)
 H38C(0.5) O14(0.5)
5.a Free rotating group:
 O15(H15A,H15B)
5.b Rotating group:
 O12(H12A,H12B), O11(H11A,H11C), O13(H13A,H13C)
5.c Secondary CH2 refined with riding coordinates:
 C21B(H21A,H21B), C22B(H22A,H22B), C23B(H23A,H23B), C24B(H24A,H24B), C25B(H25A,
 H25B), C26B(H26A,H26C), C27B(H27A,H27B), C27B(H27C,H27D), C28B(H28A,H28B),
 C29B(H29A,H29B), C30B(H30A,H30B), C21A(H21C,H21D), C22A(H22C,H22D), C23A(H23C,
 H23D), C24A(H24C,H24D), C25A(H25C,H25D), C26A(H26D,H26E), C27A(H27E,H27F),
 C28A(H28C,H28D), C29A(H29C,H29D), C30A(H30C,H30D)
5.d Aromatic/amide H refined with riding coordinates:
 C1B(H1B), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B), C8B(H8B), C10B(H10B),
 C11B(H11B), C12B(H12C), C13B(H13B), C17B(H17B), C20B(H20B), C26B(H26B),
 C1A(H1A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C8A(H8A), C10A(H10A),
 C11A(H11D), C12A(H12D), C13A(H13D), C17A(H17A), C20A(H20A)
5.e Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C)
;
_olex2_submission_special_instructions 'No special instructions were received'