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_4344663
_publ_section_title
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 Ion Pair Binding in the Solid-State with Ditopic Crown Ether Uranyl
 Salophen Receptors.
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_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 H40 F N2 Na O12 U, 3(C H4 O), 0.5(H2 O)'
_chemical_formula_sum            'C35 H52 F N2 Na O15.5 U'
_chemical_formula_weight         1028.80
_chemical_name_systematic
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 ?
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_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-10-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   21.3355(2)
_cell_length_b                   24.9757(3)
_cell_length_c                   31.4697(4)
_cell_measurement_temperature    123.15
_cell_volume                     16769.2(3)
_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      123.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker-Nonius Kappa CCD with APEXII detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.0810
_diffrn_reflns_laue_measured_fraction_full 0.971
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            110281
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.412
_exptl_absorpt_coefficient_mu    3.954
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1044 before and 0.0727 after correction.
The Ratio of minimum to maximum transmission is 0.7292.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       needle
_exptl_crystal_F_000             8192
_exptl_crystal_recrystallization_method
'Diffusion of diethyl ether into MeOH solution'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.097
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1023
_refine_ls_number_reflns         14746
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0175P)^2^+121.3199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10211
_reflns_number_total             14746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02780_si_009.cif
_cod_data_source_block           R2_NaF
_cod_database_code               4344663
_shelxl_version_number           2013-4
_olex2_refinement_description
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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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O11-H11
 0.87 with sigma of 0.01
 O12-H12
 0.87 with sigma of 0.01
 O13-H13
 0.87 with sigma of 0.01
 H20-F1A_$1
 1.8 with sigma of 0.02
 H16-O21
 1.9 with sigma of 0.02
 H21E-O19
 2.6 with sigma of 0.02
 H21E-H16
 2.1 with sigma of 0.01
 O14-H14
 0.87 with sigma of 0.01
 C31-H11
 1.921857 with sigma of 0.02
 Na1A-H11
 2.984395 with sigma of 0.02
 C32-H12
 1.899189 with sigma of 0.02
 Na1A-H12
 2.900838 with sigma of 0.02
 C33-H13
 1.885778 with sigma of 0.02
 Na1B-H13
 2.980558 with sigma of 0.02
 C34-H14
 1.891694 with sigma of 0.02
 Na1B-H14
 2.974784 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O18) = Uanis(C38)
4.a Free rotating group:
 O21(H21E,H21F)
4.b Secondary CH2 refined with riding coordinates:
 C21A(H21A,H21B), C22A(H22A,H22B), C23A(H23A,H23B), C24A(H24A,H24B), C25A(H25A,
 H25B), C26A(H26A,H26B), C27A(H27A,H27B), C28A(H28A,H28B), C29A(H29A,H29B),
 C30A(H30A,H30B), C21B(H21C,H21D), C22B(H22C,H22D), C23B(H23C,H23D), C24B(H24C,
 H24D), C25B(H25C,H25D), C26B(H26C,H26D), C27B(H27C,H27D), C28B(H28C,H28D),
 C29B(H29C,H29D), C30B(H30C,H30D)
4.c Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C8A(H8A), C10A(H10A),
 C11A(H11A), C12A(H12A), C13A(H13A), C17A(H17A), C20A(H20A), C1B(H1B), C3B(H3B),
  C4B(H4B), C5B(H5B), C6B(H6B), C8B(H8B), C10B(H10B), C11B(H11B), C12B(H12B),
 C13B(H13B), C17B(H17B), C20B(H20B)
4.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C36(H36A,H36B,H36C), C40(H40A,H40B,H40C)
4.e Idealised tetrahedral OH refined as rotating group:
 O17(H17), O19(H19), O16(H16), O20(H20)
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_olex2_submission_special_instructions 'No special instructions were received'