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

data_7122365
_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         'C126 H146 N6 O12 U2, 10(C3 H6 O)'
_chemical_formula_sum            'C156 H206 N6 O22 U2'
_chemical_formula_weight         2993.32
_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             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                69.218(4)
_cell_angle_beta                 72.211(4)
_cell_angle_gamma                83.081(4)
_cell_formula_units_Z            1
_cell_length_a                   14.0254(19)
_cell_length_b                   16.697(3)
_cell_length_c                   18.000(3)
_cell_measurement_reflns_used    9592
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.62
_cell_measurement_theta_min      3.03
_cell_volume                     3752.2(11)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      90.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.975
_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  0.0509
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            64659
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.841
_diffrn_reflns_theta_min         2.098
_exptl_absorpt_coefficient_mu    2.221
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0797 before and 0.0576 after correction. The Ratio of minimum to maximum transmission is 0.7396. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear reddish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       plate
_exptl_crystal_F_000             1544
_exptl_crystal_preparation
'Monomer mixed with the appropiate amount of uranyl acetate in EtOH and refluxed.'
_exptl_crystal_recrystallization_method
'Slow evaporation with water and acetone'
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.33
_refine_diff_density_max         8.273
_refine_diff_density_min         -2.776
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         19157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0784P)^2^+31.3140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1468
_refine_ls_wR_factor_ref         0.1580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16470
_reflns_number_total             19157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07269h2.cif
_cod_data_source_block           mo_mm389_0m
_cod_original_cell_volume        3752.3(9)
_cod_database_code               7122365
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.528
_shelx_estimated_absorpt_t_min   0.386
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H10A,H10B} of C10, {H31A,H31B} of C31, {H58A,H58B} of C58,
   All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H8A,H8B} of C8
2. Uiso/Uaniso restraints and constraints
Uanis(C81) = Uanis(C79) = Uanis(C80)
Uanis(C82) = Uanis(C83) = Uanis(C84)
Uanis(C36) = Uanis(C37) = Uanis(C38) = Uanis(C42) = Uanis(C41) = Uanis(C40) =
Uanis(C39)
Uanis(C6) = Uanis(C15) = Uanis(N1)
Uanis(C17) = Uanis(C16) = Uanis(C21)
3. Others
 Fixed Sof: C37(0.5) C42(0.5) H42(0.5) C41(0.5) H41(0.5) C40(0.5) H40(0.5)
 C39(0.5) H39(0.5) C38(0.5) H38(0.5) C43(0.5) C48(0.5) H48(0.5) C47(0.5)
 H47(0.5) C46(0.5) H46(0.5) C45(0.5) H45(0.5) C44(0.5) H44(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C31(H31A,H31B), C58(H58A,H58B)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C3(H3A), C5(H5), C17(H17), C18(H18), C19(H19), C20(H20),
 C21(H21), C24(H24), C26(H26), C42(H42), C41(H41), C40(H40), C39(H39), C38(H38),
  C48(H48), C47(H47), C46(H46), C45(H45), C44(H44), C52(H52), C54(H54),
 C65(H65), C66(H66), C67(H67), C68(H68), C69(H69)
4.c Fitted hexagon refined as free rotating group:
 C37(C42,C41,C40,C39,C38), C43(C48,C47,C46,C45,C44)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C71(H71A,H71B,
 H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C77(H77A,
 H77B,H77C), C78(H78A,H78B,H78C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C),
 C83(H83A,H83B,H83C), C84(H84A,H84B,H84C)
;
_shelx_res_checksum              98141
_olex2_submission_special_instructions 'No special instructions were received'