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

data_7122363
_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         'C102 H100 N6 O12 U2, 8(C2 D6 O S)'
_chemical_formula_sum            'C118 H100 D48 N6 O20 S8 U2'
_chemical_formula_weight         2751.25
_chemical_name_systematic        'UO2 2 tBu'
_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   geom
_audit_creation_date             2018-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-08-16 deposited with the CCDC.
2018-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                74.352(3)
_cell_angle_beta                 89.153(3)
_cell_angle_gamma                79.490(3)
_cell_formula_units_Z            1
_cell_length_a                   14.1675(13)
_cell_length_b                   15.6425(13)
_cell_length_c                   15.7252(14)
_cell_measurement_reflns_used    9740
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.366
_cell_measurement_theta_min      2.333
_cell_volume                     3297.3(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_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  0.0710
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47685
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.450
_diffrn_reflns_theta_min         1.463
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.641
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0740 before and 0.0588 after correction. The Ratio of minimum to maximum transmission is 0.8549. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       plate
_exptl_crystal_F_000             1370
_exptl_crystal_preparation
'Refluxing a mixture of UO2 salt and the monomer'
_exptl_crystal_recrystallization_method 'Slow evaporation for DMSO-d6'
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.794
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         12100
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0775P)^2^+5.1048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9722
_reflns_number_total             12100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07269h2.cif
_cod_data_source_block           mm428_sq_sq
_cod_database_code               7122363
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.655
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 U2-O8 = U2-O7
 1.7 with sigma of 0.02
 O9-O9_$1
 2.6 with sigma of 0.02
 U2_$1-N3_$1
 2.8 with sigma of 0.02
 U2-O9_$1 \\sim U2_$1-O9_$1
 with sigma of 0.01
 S5-C1A \\sim S5-C1B
 with sigma of 0.02
 C1A-O14 \\sim C1B-O14
 with sigma of 0.04
 S3-O12 \\sim S5-O14
 with sigma of 0.02
 S5-C1A \\sim S5-C1B \\sim S3-C56 \\sim S3-C57
 with sigma of 0.02
3. Restrained planarity
 U2, U2_$1, O1, O1_$1, O2_$1, O2, O9_$1, O9
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O14 \\sim S5 \\sim C1A \\sim C1B: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(O6) = Uanis(U1) = Uanis(O5) = Uanis(O4)
Uanis(O8) = Uanis(U2) = Uanis(O7) = Uanis(O9)
Uanis(C13) = Uanis(C12) = Uanis(C17) = Uanis(C11)
Uanis(C59) = Uanis(C58)
5. Rigid body (RIGU) restrains
 O14, S5, C1A, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(U2)=Sof(O7)=Sof(O8)=Sof(O9)=Sof(H1)=1-FVAR(1)
 Sof(U1)=Sof(H3)=Sof(O4)=Sof(O5)=Sof(O6)=FVAR(1)
 Sof(O14)=Sof(S5)=Sof(C1A)=Sof(D1AA)=Sof(D1AB)=Sof(D1AC)=Sof(C1B)=Sof(D1BA)=
 Sof(D1BB)=Sof(D1BC)=1-FVAR(2)
 Sof(S3)=Sof(O12)=Sof(C56)=Sof(D56A)=Sof(D56B)=Sof(D56C)=Sof(C57)=Sof(D57A)=
 Sof(D57B)=Sof(D57C)=FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), C3(H3A), C5(H5), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C21(H21), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C38(H38), C40(H40), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51)
7.b 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), C52(D52A,D52B,D52C), C53(D53A,D53B,D53C), C54(D54A,
 D54B,D54C), C55(D55A,D55B,D55C), C56(D56A,D56B,D56C), C57(D57A,D57B,D57C),
 C58(D58A,D58B,D58C), C59(D59A,D59B,D59C), C1A(D1AA,D1AB,D1AC), C1B(D1BA,D1BB,
 D1BC)
;
_olex2_date_sample_data_collection 2018-07-05
_olex2_date_sample_submission    2018-07-05
_olex2_exptl_crystal_mounting_method
'The crystal was mounted onto a mylar loop using oil'
_olex2_submission_original_sample_id 'UO2 2 tBu'
_olex2_submission_special_instructions 'No special instructions were received'