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_4344673
_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 H34 F N2 O10 Rb S0.5 U, 0.15(C2 H3 O S), 0.85(C2 H6 O S)'
_chemical_formula_sum            'C32 H39.55 F N2 O11 Rb S1.5 U'
_chemical_formula_weight         1018.79
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.4206(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3212(2)
_cell_length_b                   16.7621(2)
_cell_length_c                   15.8630(2)
_cell_measurement_reflns_used    7840
_cell_measurement_temperature    170
_cell_measurement_theta_max      30.5528
_cell_measurement_theta_min      2.8911
_cell_volume                     3718.84(8)
_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      170
_diffrn_detector_area_resol_mean 16.0107
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega   -8.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2921   77.0000  -30.0000 99

  2 omega  -50.00   48.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2921  -37.0000   60.0000 98
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0451464000
_diffrn_orient_matrix_UB_12      -0.0054447000
_diffrn_orient_matrix_UB_13      -0.0107852000
_diffrn_orient_matrix_UB_21      -0.0197154000
_diffrn_orient_matrix_UB_22      -0.0301388000
_diffrn_orient_matrix_UB_23      -0.0299124000
_diffrn_orient_matrix_UB_31      -0.0120320000
_diffrn_orient_matrix_UB_32      0.0292026000
_diffrn_orient_matrix_UB_33      -0.0329434000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_laue_measured_fraction_full 0.966
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12315
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.897
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.812
_exptl_absorpt_correction_T_max  0.538
_exptl_absorpt_correction_T_min  0.309
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       block
_exptl_crystal_F_000             1982
_exptl_crystal_recrystallization_method 'Evaporation of acetone/DMSO'
_exptl_crystal_size_max          0.3398
_exptl_crystal_size_mid          0.2722
_exptl_crystal_size_min          0.1235
_refine_diff_density_max         1.855
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         6497
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0324P)^2^+17.9014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5854
_reflns_number_total             6497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02780_si_006.cif
_cod_data_source_block           R1_RbF
_cod_original_cell_volume        3718.84(9)
_cod_original_formula_sum        'C32 H39.55 F N2 O11 Rb S1.50 U'
_cod_database_code               4344673
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C32 H40 N2 O11 U1 Rb1 F1 S2'
_reflns_odcompleteness_completeness 98.64
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1A-C29A = S1B-C29B = S1A-C30A = S1B-C30B
 1.86 with sigma of 0.01
 S1B-O10B = S1A-O10A = O10C-S1C = S1D-O10D
 1.68 with sigma of 0.01
 C32C-S1C = C31C-S1C = S1D-C32D = C31D-S1D
 1.86 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(S1B) = Uanis(S1A)
Uanis(O10B) = Uanis(S1B)
Uanis(O10A) = Uanis(S1A)
Uanis(C29B) = Uanis(S1B)
Uanis(C29A) = Uanis(S1A)
Uanis(S1B) = Uanis(C30B)
Uanis(C30A) = Uanis(S1A)
Uanis(C31D) = Uanis(S1D)
Uanis(O10D) = Uanis(S1D)
Uanis(C32D) = Uanis(S1D)
Uanis(C27B) = Uanis(C27A)
Uanis(S1C) = Uanis(O10C)
Uanis(C31C) = Uanis(S1C)
Uanis(S1C) = Uanis(C32C)
Uanis(C32D) = Uanis(C32C)
4. Others
 Fixed Sof: S1A(0.25) S1B(0.25) O8A(0.7) O8B(0.3) O10A(0.5) O10B(0.5)
 H26A(0.7) H26B(0.7) H26C(0.3) H26D(0.3) C27A(0.7) H27A(0.7) H27B(0.7)
 C27B(0.3) H27C(0.3) H27D(0.3) H28A(0.7) H28B(0.7) H28C(0.3) H28D(0.3)
 C29A(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C29B(0.5) H29D(0.5) H29E(0.5)
 H29F(0.5) C30A(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C30B(0.5) H30D(0.5)
 H30E(0.5) H30F(0.5) S1D(0.15) O10D(0.15) C31D(0.15) H31D(0.15) H31E(0.15)
 H31F(0.15) C32D(0.15) S1C(0.85) O10C(0.85) C31C(0.85) H31A(0.85) H31B(0.85)
 H31C(0.85) C32C(0.85) H32A(0.85) H32B(0.85) H32C(0.85)
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), C26(H26C,H26D), C27A(H27A,H27B), C27B(H27C,H27D),
 C28(H28A,H28B), C28(H28C,H28D)
5.b 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)
5.c Idealised Me refined as rotating group:
 C29A(H29A,H29B,H29C), C29B(H29D,H29E,H29F), C30A(H30A,H30B,H30C), C30B(H30D,
 H30E,H30F), C31D(H31D,H31E,H31F), C31C(H31A,H31B,H31C), C32C(H32A,H32B,H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'