An Example of Unusual Pyridine Donor Schiff Base Uranyl (UO22+) Complexes
Hardy, Emily Elizabeth; Wyss, Kevin M.; Eddy, Madeleine A.; Gorden, Anne E. V.; Chem. Commun.  (2017) –; doi:10.1039/C7CC02747H

data_7120065
_publ_section_title
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 An Example of Unusual Pyridine Donor Schiff Base Uranyl (UO22+) Complexes
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02747H
_journal_year                    2017
_chemical_formula_moiety         'C29 H21 N3 O4 U'
_chemical_formula_sum            'C29 H21 N3 O4 U'
_chemical_formula_weight         713.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-01 deposited with the CCDC.
2017-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.3343(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.8062(10)
_cell_length_b                   7.2736(3)
_cell_length_c                   14.7805(6)
_cell_measurement_reflns_used    9264
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      31.474
_cell_measurement_theta_min      2.779
_cell_volume                     2431.78(18)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.45
_diffrn_measured_fraction_theta_full 0.9983
_diffrn_measured_fraction_theta_max 0.9983
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            61345
_diffrn_reflns_theta_full        31.5228
_diffrn_reflns_theta_max         31.52
_diffrn_reflns_theta_min         1.80
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.720
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.4479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1304 before and 0.0486 after correction.
The Ratio of minimum to maximum transmission is 0.6002.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.9488
_exptl_crystal_description       block
_exptl_crystal_F_000             1320.1908
_exptl_crystal_recrystallization_method 'slow evaporation of DCM'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.1844
_refine_diff_density_min         -5.5836
_refine_diff_density_rms         0.2739
_refine_ls_d_res_high            0.6797
_refine_ls_d_res_low             11.3098
_refine_ls_goodness_of_fit_ref   1.0836
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     333
_refine_ls_number_reflns         8098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0836
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+13.6822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              32
_reflns_limit_h_min              -33
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                7226
_reflns_number_total             8098
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7cc02747h2.cif
_cod_data_source_block           Emily051916_0ma
_cod_database_code               7120065
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b), C18(H18a,H18b)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C15(H15), C14(H14), C6(H6), C2(H2), C11(H11), C3(H3), C7(H7),
 C8(H8), C5(H5), C19(H19), C28(H28), C27(H27), C25(H25), C24(H24), C22(H22),
 C23(H23)
;
_olex2_exptl_crystal_mounting_method
'mounted on a glass fibre in paratone-n oil'
_olex2_submission_special_instructions 'No special instructions were received'