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_4344666
_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 H32.8 Cs F N2 O10 S0.6 U, C2 H6 O S'
_chemical_formula_sum            'C32 H38.8 Cs F N2 O11 S1.6 U'
_chemical_formula_weight         1068.68
_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             2015-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.5212(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4915(2)
_cell_length_b                   16.7088(2)
_cell_length_c                   15.9434(2)
_cell_measurement_reflns_used    8340
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.4633
_cell_measurement_theta_min      2.9690
_cell_volume                     3782.68(9)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -50.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2921  -37.0000  120.0000 98

  2 omega  -14.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2921   19.0000   90.0000 101
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0282475000
_diffrn_orient_matrix_UB_12      -0.0297234000
_diffrn_orient_matrix_UB_13      0.0142681000
_diffrn_orient_matrix_UB_21      -0.0408940000
_diffrn_orient_matrix_UB_22      0.0175108000
_diffrn_orient_matrix_UB_23      -0.0251475000
_diffrn_orient_matrix_UB_31      0.0049166000
_diffrn_orient_matrix_UB_32      -0.0247310000
_diffrn_orient_matrix_UB_33      -0.0350229000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_laue_measured_fraction_full 0.968
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12626
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.975
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.390
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94474
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_description       block
_exptl_crystal_F_000             2058
_exptl_crystal_recrystallization_method 'Evaporation of acetone/DMSO solution'
_exptl_crystal_size_max          0.2432
_exptl_crystal_size_mid          0.2106
_exptl_crystal_size_min          0.0996
_refine_diff_density_max         1.091
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         6634
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0200P)^2^+9.2934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5992
_reflns_number_total             6634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02780_si_007.cif
_cod_data_source_block           R1_CsF
_cod_original_cell_volume        3782.68(10)
_cod_original_formula_sum        'C32 H38.80 Cs F N2 O11 S1.60 U'
_cod_database_code               4344666
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C32 H28 N2 O11 U1 Cs1 F1 S2'
_reflns_odcompleteness_completeness 98.68
_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
 S2B-O11B = S2A-O11A = S2C-O11C
 1.45 with sigma of 0.01
 S2A-C32A = S2C-C32C = S2B-C32B = S2A-C31A = S2B-C31B = S2C-C31C
 1.7 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C31A) = Uanis(S2A)
Uanis(C32A) = Uanis(S2A)
Uanis(S2A) = Uanis(O11A)
Uanis(C31B) = Uanis(S2B)
Uanis(C32B) = Uanis(S2B)
Uanis(S2B) = Uanis(O11B)
Uanis(C32C) = Uanis(S2C)
Uanis(C31C) = Uanis(S2C)
Uanis(S2C) = Uanis(O11C)
4. Others
 Fixed Sof: S2A(0.2) S2B(0.2) S2C(0.2) O6A(0.6) O6B(0.4) O11A(0.35) O11B(0.35)
 O11C(0.3) H21A(0.6) H21B(0.6) H21C(0.4) H21D(0.4) C22A(0.6) H22A(0.6)
 H22B(0.6) C22B(0.4) H22C(0.4) H22D(0.4) H23A(0.6) H23B(0.6) H23C(0.4)
 H23D(0.4) C31A(0.3) H31A(0.3) H31B(0.3) H31C(0.3) C31B(0.3) H31D(0.3)
 H31E(0.3) H31F(0.3) C31C(0.4) C32A(0.3) H32A(0.3) H32B(0.3) H32C(0.3)
 C32B(0.3) H32D(0.3) H32E(0.3) H32F(0.3) C32C(0.4) H32G(0.4) H32H(0.4) H32I(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C21(H21C,H21D), C22A(H22A,H22B), C22B(H22C,H22D), C23(H23A,
 H23B), C23(H23C,H23D), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B)
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:
 C31A(H31A,H31B,H31C), C31B(H31D,H31E,H31F), C32A(H32A,H32B,H32C), C32B(H32D,
 H32E,H32F), C32C(H32G,H32H,H32I), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_olex2_submission_special_instructions 'No special instructions were received'