Uranyl ion coordination with rigid aromatic carboxylates and structural characterization of their complexes
Aaron C. Sather; Orion B. Berryman; Curtis E. Moore; Julius Rebek; Chem.Commun. 49 (2013) 6379–; doi:10.1039/c3cc43358g

data_7109483
_publ_section_title
;
 Uranyl ion coordination with rigid aromatic carboxylates and structural
 characterization of their complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              6379
_journal_paper_doi               10.1039/c3cc43358g
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C72 H57 O8 U, C6 H16 N, 4(C H4 O)'
_chemical_formula_sum            'C82 H89 N O12 U'
_chemical_formula_weight         1518.57
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-23
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.484(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2622(12)
_cell_length_b                   18.6958(15)
_cell_length_c                   26.384(2)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.810
_cell_measurement_theta_min      5.960
_cell_volume                     7022.1(10)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2 v2011.4-0 (Bruker, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL-2012, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'Bruker APEX2 v2011.4-0 (Bruker, 2011)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            56112
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         67.167
_diffrn_reflns_theta_min         2.899
_diffrn_source                   'Micro Focus Sealed Tube'
_diffrn_source_type              'Bruker/Incotec Imus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.021
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.4520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1230 before and 0.0409 after correction.
The Ratio of minimum to maximum transmission is 0.6003.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_colour_primary    Colorless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       Rod
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         12372
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0228
_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^)+(0.0283P)^2^+7.4709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11660
_reflns_number_total             12372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc43358g.txt
_cod_data_source_block           final_04
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        7022.2(10)
_cod_database_code               7109483
_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, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 N1B-C75B
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O4S) = Uanis(O4SB)
Uanis(C73B) = Uanis(C73)
Uanis(N1B) = Uanis(N1)
Uanis(C77) = Uanis(C77B)
Uanis(C75B) = Uanis(C75)
Uanis(C76) = Uanis(C76B)
4. Others
 Sof(H4SD)=Sof(H4SE)=Sof(H4SF)=Sof(O4SB)=Sof(H4SG)=1-FVAR(1)
 Sof(H4SA)=Sof(H4SB)=Sof(H4SC)=Sof(O4S)=Sof(H4S)=FVAR(1)
 Sof(H74D)=Sof(H74E)=Sof(H74F)=Sof(H78D)=Sof(H78E)=Sof(H78F)=Sof(N1B)=Sof(H1B)=
 Sof(C75B)=Sof(H75C)=Sof(H75D)=Sof(C76B)=Sof(H76D)=Sof(H76E)=Sof(H76F)=
 Sof(C77B)=Sof(H77C)=Sof(H77D)=Sof(C73B)=Sof(H73C)=Sof(H73D)=1-FVAR(2)
 Sof(N1)=Sof(H1)=Sof(H74A)=Sof(H74B)=Sof(H74C)=Sof(C73)=Sof(H73A)=Sof(H73B)=
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=Sof(H78A)=
 Sof(H78B)=Sof(H78C)=Sof(C77)=Sof(H77A)=Sof(H77B)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 N1(H1), N1B(H1B)
5.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C16(H16A,H16B), C38(H38A,H38B), C59(H59A,H59B), C61(H61A,
 H61B), C63(H63A,H63B), C73(H73A,H73B), C75(H75A,H75B), C77(H77A,H77B),
 C75B(H75C,H75D), C77B(H77C,H77D), C73B(H73C,H73D)
5.c Me refined with riding coordinates:
 C4S(H4SA,H4SB,H4SC), C4S(H4SD,H4SE,H4SF)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C18(H18), C19(H19), C21(H21),
 C22(H22), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C40(H40), C41(H41), C43(H43), C44(H44), C46(H46), C47(H47),
 C48(H48), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C65(H65), C66(H66),
  C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
5.e Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C3S(H3SA,H3SB,
 H3SC), C74(H74A,H74B,H74C), C74(H74D,H74E,H74F), C76(H76A,H76B,H76C), C78(H78A,
 H78B,H78C), C78(H78D,H78E,H78F), C2S(H2SA,H2SB,H2SC), C1S(H1SA,H1SB,H1SC),
 C76B(H76D,H76E,H76F)
5.f Idealised tetrahedral OH refined as rotating group:
 O3S(H3S), O2S(H2S), O1S(H1S), O4S(H4S), O4SB(H4SG)
;
_shelx_estimated_absorpt_t_max   0.720
_shelx_estimated_absorpt_t_min   0.227
_shelx_hkl_checksum              42722
_shelx_res_checksum              58324
_shelxl_version_number           2013-3