Toward Equatorial Planarity about Uranyl: Synthesis and Structure of Tridentate Nitrogen-Donor {UO2}(2+) Complexes.
Copping, Roy; Jeon, Byoungseon; Pemmaraju, C. Das; Wang, Shuao; Teat, Simon J.; Janousch, Markus; Tyliszczak, Tolek; Canning, Andrew; Grønbech-Jensen, Niels; Prendergast, David; Shuh, David K.; Inorganic chemistry 53 (2014) 2506–2515; doi:10.1021/ic4026359

data_4337757
_publ_section_title
;
 Toward Equatorial Planarity about Uranyl: Synthesis and Structure of
 Tridentate Nitrogen-Donor {UO2}(2+) Complexes.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2506
_journal_page_last               2515
_journal_paper_doi               10.1021/ic4026359
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C29 H21 N7 O2 U'
_chemical_formula_weight         737.56
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7287(17)
_cell_length_b                   12.9878(16)
_cell_length_c                   14.8038(19)
_cell_measurement_reflns_used    6115
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.58
_cell_measurement_theta_min      4.55
_cell_volume                     2639.6(6)
_computing_cell_refinement       'Bruker SAINT v7.56a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v7.56a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26389
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         33.07
_diffrn_reflns_theta_min         3.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.343
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 Bruker AXS Madison WI USA'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.164
_refine_diff_density_min         -1.901
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+12.7957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0585
_reflns_number_gt                2305
_reflns_number_total             3860
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic4026359_si_003.cif
_cod_data_source_block           compound3
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               4337757