Expanded Campestarene Hosts for Tetra- and Dinuclear Uranyl(VI) Complexes
Chaudhry, Mohammad; Lelj, Francesco; MacLachlan, Mark; Chemical Communications  (2018) –; doi:10.1039/C8CC07269H

data_7122366
_publ_section_title
;
 Expanded Campestarene Hosts for Tetra- and Dinuclear Uranyl(VI) Complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC07269H
_journal_year                    2018
_chemical_formula_moiety         '0.5(C136 H136 N8 O20 U4)'
_chemical_formula_sum            'C68 H68 N4 O10 U2'
_chemical_formula_weight         1577.32
_chemical_name_systematic        'UO2 4 tBu Ph'
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d'
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-08-16 deposited with the CCDC.
2018-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   35.7713(16)
_cell_length_b                   35.7713(16)
_cell_length_c                   28.7439(13)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    90
_cell_measurement_theta_max      23.61
_cell_measurement_theta_min      2.27
_cell_volume                     36780(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            43768
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.362
_diffrn_reflns_theta_min         2.172
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.560
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0755 before and 0.0523 after correction. The Ratio of minimum to maximum transmission is 0.8246. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       rod
_exptl_crystal_F_000             12288
_exptl_crystal_preparation
'Uranyl(VI) acetate in refluxing ethanol with my monomer'
_exptl_crystal_recrystallization_method
'Vapour diffusion of heptane into 1,2-dichloroethane.'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.583
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         8388
_refine_ls_number_restraints     1293
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0392P)^2^+615.4437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1522
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5198
_reflns_number_total             8388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07269h2.cif
_cod_data_source_block           mm388_sq
_cod_original_cell_volume        36780(4)
_cod_database_code               7122366
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.617
_shelx_estimated_absorpt_t_min   0.447
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, H20 of C20, H5A of C5, H3 of C3, H22 of C22, H47A of C47A,
  H48A of C48A, H49A of C49A, H48 of C48, H51 of C51, H39 of C39, H51A of C51A,
  H50 of C50, H49 of C49, H37 of C37, H47 of C47, H50A of C50A, H33 of C33, H32
  of C32, H30 of C30, H34 of C34, H31 of C31
 At 1.5 times of:
  All C(H,H,H) groups, H5 of C0AA
2. Restrained distances
 C43-C41 \\sim C44-C41 \\sim C42-C41
 with sigma of 0.01
 C9-C7 \\sim C8-C7 \\sim C7-C10
 with sigma of 0.01
 C53-C52 \\sim C54-C52 \\sim C55-C52
 with sigma of 0.01
 C52-C25 \\sim C52-C26 \\sim C52-C27
 with sigma of 0.01
 C8-C9 \\sim C9-C10 \\sim C8-C10
 with sigma of 0.01
 C42-C43 \\sim C43-C44 \\sim C44-C42
 with sigma of 0.01
 C25-C26 \\sim C25-C27 \\sim C26-C27
 with sigma of 0.01
 C53-C54 \\sim C54-C55 \\sim C53-C55
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=1-FVAR(1)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(1)
 Sof(C41)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C43)=Sof(H43A)=Sof(H43B)=
 Sof(H43C)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=1-FVAR(2)
 Sof(C7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(2)
 Fixed Sof: C6(0.5) C5(0.5) H5A(0.5) C4(0.5) C3(0.5) H3(0.5) C2(0.5) C1(0.5)
 C35(0.5) C40(0.5) C39(0.5) H39(0.5) C38(0.5) C37(0.5) H37(0.5) C36(0.5)
 C47(0.5) H47(0.5) C48(0.5) H48(0.5) C49(0.5) H49(0.5) C50(0.5) H50(0.5)
 C51(0.5) H51(0.5) C46(0.5) C50A(0.5) H50A(0.5) C51A(0.5) H51A(0.5) C46A(0.5)
 C47A(0.5) H47A(0.5) C48A(0.5) H48A(0.5) C49A(0.5) H49A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C5(H5A), C3(H3), C20(H20), C22(H22), C34(H34), C33(H33), C32(H32),
 C31(H31), C30(H30), C39(H39), C37(H37), C47(H47), C48(H48), C49(H49), C50(H50),
  C51(H51), C50A(H50A), C51A(H51A), C47A(H47A), C48A(H48A), C49A(H49A)
6.b Fitted hexagon refined as free rotating group:
 C6(C5,C4,C3,C2,C1), C20(C19,C18,C23,C22,C21), C29(C34,C33,C32,C31,C30),
 C35(C40,C39,C38,C37,C36), C47(C48,C49,C50,C51,C46), C50A(C51A,C46A,C47A,C48A,
 C49A)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C25(H25A,H25B,H25C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C44(H44A,H44B,H44C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C)
;
_shelx_res_checksum              63704
_shelx_fab_checksum              81284
_olex2_submission_original_sample_id 'UO2 4 tBu Ph'
_olex2_submission_special_instructions 'No special instructions were received'