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_4337754
_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 H23 Cl2 N7 O2 U'
_chemical_formula_weight         810.47
_chemical_name_systematic
;
 ?
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 115.091(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2371(9)
_cell_length_b                   18.0253(13)
_cell_length_c                   14.2323(10)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.52
_cell_measurement_theta_min      3.15
_cell_volume                     2843.1(4)
_computing_cell_refinement       'Bruker SAINT v7.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v7.34a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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     0.7749
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40576
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         33.591
_diffrn_reflns_theta_min         2.464
_exptl_absorpt_coefficient_mu    3.345
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 Bruker AXS Madison WI USA'
_exptl_crystal_colour            Green/yellow
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         8643
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0307P)^2^+0.7625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7610
_reflns_number_total             8643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic4026359_si_003.cif
_cod_data_source_block           compound1
_cod_database_code               4337754
_shelx_estimated_absorpt_t_min   0.753
_shelx_estimated_absorpt_t_max   0.851