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_4344664
_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         'C29 H32 Br N2 Na O10 U'
_chemical_formula_sum            'C29 H32 Br N2 Na O10 U'
_chemical_formula_weight         902.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 97.497(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.02121(18)
_cell_length_b                   32.1044(11)
_cell_length_c                   25.8906(6)
_cell_measurement_reflns_used    7618
_cell_measurement_temperature    170
_cell_measurement_theta_max      28.8150
_cell_measurement_theta_min      2.4750
_cell_volume                     6610.3(3)
_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      170
_diffrn_detector_area_resol_mean 16.0107
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -80.00   26.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7006  -19.0000  120.0000 106

  2 omega  -11.00   60.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4819  -99.0000    0.0000 71
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0559259000
_diffrn_orient_matrix_UB_12      -0.0171967000
_diffrn_orient_matrix_UB_13      -0.0018684000
_diffrn_orient_matrix_UB_21      -0.0633561000
_diffrn_orient_matrix_UB_22      0.0127775000
_diffrn_orient_matrix_UB_23      0.0083862000
_diffrn_orient_matrix_UB_31      -0.0285245000
_diffrn_orient_matrix_UB_32      0.0053220000
_diffrn_orient_matrix_UB_33      -0.0262878000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            24694
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.032
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.188
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.222
_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    1.814
_exptl_crystal_description       plate
_exptl_crystal_F_000             3472
_exptl_crystal_recrystallization_method
'Diffusion of diethyl ether into MeOH solution'
_exptl_crystal_size_max          0.5514
_exptl_crystal_size_mid          0.1227
_exptl_crystal_size_min          0.0364
_refine_diff_density_max         3.812
_refine_diff_density_min         -3.519
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         11575
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0982P)^2^+14.5670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9404
_reflns_number_total             11575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02780_si_005.cif
_cod_data_source_block           R1_NaBr
_cod_depositor_comments
;

2023-09-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        6610.2(3)
_cod_original_formula_moiety
'C28 H30 Br N2 Na O10 U, C29 H32 Br N2 Na O10 U'
_cod_original_formula_sum        'C57 H62 Br2 N4 Na2 O20 U2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1804.96
_cod_database_code               4344664
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C28 H28 N2 O9 U1 Na1 Br1'
_reflns_odcompleteness_completeness 98.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
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
 O10-H10
 0.85 with sigma of 0.01
 U1B-O4B = U1C-O4C = U1B-O3B = U1C-O3C
 2.23 with sigma of 0.01
 H11C-H25B_$1
 2.1 with sigma of 0.01
 C29-H10
 1.923221 with sigma of 0.02
 U1A-H10
 3.044178 with sigma of 0.02
3. Rigid bond restraints
 C1C, C2C, C7C, C6C, C5C, C4C, C3C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1B, C2B, C3B, C4B, C5B, C6B, C7B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O1C) = Uanis(O1B)
Uanis(O4B) = Uanis(U1B)
Uanis(U1B) = Uanis(O2B)
Uanis(C1C) = Uanis(N1B)
Uanis(C1B) = Uanis(N1B)
Uanis(C2B) = Uanis(C2C)
Uanis(C2C) = Uanis(C1C)
Uanis(C2B) = Uanis(C1B)
Uanis(C3B) = Uanis(C3C)
Uanis(C4B) = Uanis(C4C)
Uanis(C5B) = Uanis(C5C)
Uanis(U1C) = Uanis(U1B)
Uanis(O4C) = Uanis(U1C)
Uanis(U1C) = Uanis(O2C)
Uanis(U1B) = Uanis(O11B)
Uanis(U1C) = Uanis(O11C)
Uanis(C6B) = Uanis(C5B)
Uanis(C6C) = Uanis(C5C)
Uanis(C7B) = Uanis(C7C)
5. Others
 Fixed Sof: U1B(0.5) U1C(0.5) O1B(0.5) O1C(0.5) O2B(0.5) O2C(0.5) O3B(0.5)
 O3C(0.5) O4B(0.5) O4C(0.5) O11B(0.5) H11A(0.5) H11B(0.5) O11C(0.5) H11C(0.5)
 H11D(0.5) C1B(0.5) H1B(0.5) C1C(0.5) H1C(0.5) C2B(0.5) C2C(0.5) C3B(0.5)
 H3B(0.5) C3C(0.5) H3C(0.5) C4B(0.5) H4B(0.5) C4C(0.5) H4C(0.5) C5B(0.5)
 H5B(0.5) C5C(0.5) H5C(0.5) C6B(0.5) H6B(0.5) C6C(0.5) H6C(0.5) C7B(0.5)
 C7C(0.5)
6.a Rotating group:
 O11B(H11A,H11B), O11C(H11C,H11D)
6.b Secondary CH2 refined with riding coordinates:
 C21B(H21A,H21B), C22B(H22A,H22B), C23B(H23A,H23B), C24B(H24A,H24B), C25B(H25A,
 H25B), C26B(H26A,H26B), C27B(H27A,H27B), C28B(H28A,H28B), C21A(H21C,H21D),
 C22A(H22C,H22D), C23A(H23C,H23D), C24A(H24C,H24D), C25A(H25C,H25D), C26A(H26C,
 H26D), C27A(H27C,H27D), C28A(H28C,H28D)
6.c Aromatic/amide H refined with riding coordinates:
 C1B(H1B), C1C(H1C), C3B(H3B), C3C(H3C), C4B(H4B), C4C(H4C), C5B(H5B),
 C5C(H5C), C6B(H6B), C6C(H6C), C8B(H8B), C10B(H10B), C11B(H11E), C12B(H12B),
 C13B(H13B), C17B(H17B), C20B(H20B), C1A(H1A), C3A(H3A), C4A(H4A), C5A(H5A),
 C6A(H6A), C8A(H8A), C10A(H10A), C11A(H11F), C12A(H12A), C13A(H13A), C17A(H17A),
  C20A(H20A)
6.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'