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_4344671
_publ_section_title
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 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 H42 N2 Na O13 U, C32 H40 N2 Na O12 U, 2.8(C H4 O), 0.2(H2 O), 2(Br)'
_chemical_formula_sum            'C66.8 H93.6 Br2 N4 Na2 O28 U2'
_chemical_formula_weight         2082.51
_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
_audit_creation_date             2015-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                94.4530(10)
_cell_angle_beta                 97.5330(10)
_cell_angle_gamma                112.1390(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5154(2)
_cell_length_b                   12.9926(2)
_cell_length_c                   31.2989(5)
_cell_measurement_temperature    123(2)
_cell_volume                     3888.91(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_laue_measured_fraction_full 0.975
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            40936
_diffrn_reflns_point_group_measured_fraction_full 0.975
_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         1.916
_exptl_absorpt_coefficient_mu    5.279
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0808 before and 0.0618 after correction.
The Ratio of minimum to maximum transmission is 0.7443.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description       block
_exptl_crystal_F_000             2045
_exptl_crystal_recrystallization_method
'Diffusion of diethyl ether into MeOH solution'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.458
_refine_diff_density_min         -1.459
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1026
_refine_ls_number_reflns         13716
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0386
_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^)+25.9937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11867
_reflns_number_total             13716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02780_si_010.cif
_cod_data_source_block           R2_NaBr_1
_cod_original_formula_sum        'C66.80 H93.60 Br2 N4 Na2 O28 U2'
_cod_database_code               4344671
_shelxl_version_number           2014-3
_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
 O13-H4S
 0.87 with sigma of 0.01
 O9C-C28C
 1.42 with sigma of 0.01
 O10B-C30C = O10B-C30B
 1.42 with sigma of 0.01
 H16B-Br1B
 2.5 with sigma of 0.02
 O9B-C28B = O8B-C26B
 1.42 with sigma of 0.01
 O8B-C27B
 1.42 with sigma of 0.01
 O8B-C27B = O9B-C29B = O9C-C29C = O9B-C28B
 1.42 with sigma of 0.01
 C27B-C28B = C29C-C30C = C30B-C29B
 1.52 with sigma of 0.01
 C27C-C28C
 1.52 with sigma of 0.01
 C27C-C26B
 2.37 with sigma of 0.02
 H16B_$1-H6S
 2.1 with sigma of 0.02
 C32-H4S
 1.867108 with sigma of 0.02
 Na1A-H4S
 2.961072 with sigma of 0.02
3. Rigid bond restraints
 O10B, C29B, C30B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O8B, O10B, O9B, C27B, C28B, C29B, C30B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O9B, C27B, C28B, C29B, C30B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O9C, C27C, C28C, C29C, C30C
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C28B \\sim C28C: within 1.7A with sigma of 0.005 and sigma for terminal atoms
of 0.005
O9B \\sim O9C: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.001
C30B \\sim C30C: within 1.7A with sigma of 0.001 and sigma for terminal atoms
of 0.001
C27B \\sim C27C: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
Uanis(C30B) \\sim Ueq, Uanis(C30C) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C30B) \\sim Ueq, Uanis(C30C) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.1
Uanis(Br2A) = Uanis(Br2B)
Uanis(C27B) = Uanis(C28B)
Uanis(C28C) = Uanis(C27C)
5. Others
 Fixed Sof: O9B(0.7) C27B(0.7) H76A(0.7) H76B(0.7) C28B(0.7) H75A(0.7)
 H75B(0.7) C29B(0.7) H73A(0.7) H73B(0.7) C30B(0.7) H72A(0.7) H72B(0.7) O9C(0.3)
 C27C(0.3) H76C(0.3) H76D(0.3) C28C(0.3) H75C(0.3) H75D(0.3) C29C(0.3)
 H73C(0.3) H73D(0.3) C30C(0.3) H72C(0.3) H72D(0.3) O18(0.8) H8S(0.8) C37(0.8)
 H9SA(0.8) H9SB(0.8) H9SC(0.8) O19(0.2) H16A(0.2) H16B(0.2) Br2B(0.3) Br1A(0.8)
 Br2A(0.7) Br1B(0.2)
6.a Free rotating group:
 O19(H16A,H16B)
6.b Rotating group:
 O12(H3SA,H3SB)
6.c Secondary CH2 refined with riding coordinates:
 C21B(H85A,H85B), C22B(H84A,H84B), C23B(H82A,H82B), C24B(H81A,H81B), C25B(H79A,
 H79B), C26B(H78A,H78B), C27B(H76A,H76B), C28B(H75A,H75B), C29B(H73A,H73B),
 C30B(H72A,H72B), C27C(H76C,H76D), C28C(H75C,H75D), C29C(H73C,H73D), C30C(H72C,
 H72D), C21A(H29A,H29B), C22A(H30A,H30B), C23A(H32A,H32B), C24A(H33A,H33B),
 C25A(H35A,H35B), C26A(H36A,H36B), C27A(H38A,H38B), C28A(H39A,H39B), C29A(H41A,
 H41B), C30A(H42A,H42B)
6.d Aromatic/amide H refined with riding coordinates:
 C1B(H57), C3B(H59), C4B(H60), C5B(H61), C6B(H62), C8B(H48), C10B(H50),
 C11B(H51), C12B(H52), C13B(H53), C17B(H70), C20B(H67), C1A(H5), C3A(H7),
 C4A(H8), C5A(H9), C6A(H10), C8A(H14), C10A(H16), C11A(H17), C12A(H18),
 C13A(H19), C17A(H24), C20A(H27)
6.e Idealised Me refined as rotating group:
 C33(H11A,H11B,H11C), C34(H15A,H15B,H15C), C31(H2SA,H2SB,H2SC), C32(H5SA,H5SB,
 H5SC), C36(H7SA,H7SB,H7SC), C35(H13A,H13B,H13C), C37(H9SA,H9SB,H9SC)
6.f Idealised tetrahedral OH refined as rotating group:
 O17(H6S), O16(H12S), O18(H8S)
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_olex2_date_sample_data_collection 10.7.2013
_olex2_submission_special_instructions 'No special instructions were received'