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

data_7122364
_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         'C42 H49 N2 O5 U'
_chemical_formula_sum            'C42 H49 N2 O5 U'
_chemical_formula_weight         899.86
_chemical_name_systematic        'UO2 4 tOct Ph'
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-27
_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                   29.7978(13)
_cell_length_b                   29.7978(13)
_cell_length_c                   21.0965(10)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.369
_cell_measurement_theta_min      2.27
_cell_volume                     18731.8(15)
_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      90.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0632
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33974
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.371
_diffrn_reflns_theta_min         1.808
_exptl_absorpt_coefficient_mu    3.503
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1286 before and 0.0528 after correction. The Ratio of minimum to maximum transmission is 0.7626. 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    1.276
_exptl_crystal_description       plate
_exptl_crystal_F_000             7152
_exptl_crystal_preparation
'UO2 salt mixed with my monomer in ethanol and refluxed.'
_exptl_crystal_recrystallization_method
'Vapour diffusion of pentane into acetone'
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.584
_refine_diff_density_min         -1.347
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         8591
_refine_ls_number_restraints     1222
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+204.7400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5569
_reflns_number_total             8591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07269h2.cif
_cod_data_source_block           mm391_sq
_cod_original_cell_volume        18731.8(19)
_cod_database_code               7122364
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.571
_shelx_estimated_absorpt_t_min   0.249
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-C51 = C28-C51 = C29-C51 = C29-C31 = C32-C31 = C30-C31 = C31-C33
 1.54 with sigma of 0.02
 C52-C51 = C53-C51 = C54-C51 = C54-C55 = C55-C57 = C58-C55 = C55-C56
 1.54 with sigma of 0.02
 C7-C5 = C6-C5 = C8-C5 = C9-C8 = C9-C10 = C9-C12 = C9-C11
 1.54 with sigma of 0.02
 C43-C44 = C43-C45 = C46-C43 = C46-C47 = C50-C47 = C49-C47 = C47-C48
 1.54 with sigma of 0.02
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
Uanis(C39) = Uanis(C37)
Uanis(C50) = Uanis(C47)
Uanis(C37) = Uanis(C38) = Uanis(C39)
Uanis(C12) = Uanis(C9) = Uanis(C10) = Uanis(C11)
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(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C55)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=
 1-FVAR(1)
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 FVAR(1)
 Sof(C43)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45)=Sof(H45A)=Sof(H45B)=
 Sof(H45C)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(C48)=Sof(H48A)=Sof(H48B)=
 Sof(H48C)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C50)=Sof(H50A)=Sof(H50B)=
 Sof(H50C)=1-FVAR(2)
 Sof(C5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C29(H29A,H29B), C46(H46A,H46B), C54(H54A,H54B)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C19(H19), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21),
 C23(H23), C40(H40), C39(H39), C38(H38), C37(H37), C36(H36), C42(H42)
6.c Fitted hexagon refined as free rotating group:
 C19(C14,C15,C16,C17,C18), C35(C40,C39,C38,C37,C36)
6.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              43093
_shelx_fab_checksum              55539
_olex2_submission_special_instructions 'No special instructions were received'