Spectroscopic and Structural Elucidation of Uranium Dioxophenoxazine Complexes.
Pattenaude, Scott A.; Kuehner, Christopher S.; Dorfner, Walter L.; Schelter, Eric J.; Fanwick, Phillip E.; Bart, Suzanne C.; Inorganic chemistry 54 (2015) 6520–6527; doi:10.1021/acs.inorgchem.5b00855

data_4343433
_publ_section_title
;
 Spectroscopic and Structural Elucidation of Uranium Dioxophenoxazine
 Complexes.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6520
_journal_page_last               6527
_journal_paper_doi               10.1021/acs.inorgchem.5b00855
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'U1,8(H2 O1),2(N1),8(C1),C77 N47'
_chemical_formula_sum            'C56 H76 N2 O8 U'
_chemical_formula_weight         1143.21
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 109.155(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9010(8)
_cell_length_b                   11.2184(3)
_cell_length_c                   27.7219(6)
_cell_measurement_reflns_used    33915
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      67.837
_cell_measurement_theta_min      3.313
_cell_volume                     5846.5(3)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL3000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            33915
_diffrn_reflns_point_group_measured_fraction_full 0.895
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.837
_diffrn_reflns_theta_min         3.313
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    8.201
_exptl_absorpt_correction_T_max  0.611
_exptl_absorpt_correction_T_min  0.025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.429
_refine_diff_density_min         -3.969
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         9494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1481P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.1887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7970
_reflns_number_total             9494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00855_si_001.cif
_cod_data_source_block           SAP243
_cod_depositor_comments
'Adding full bibliography for 4343432--4343434.cif.'
_cod_database_code               4343433
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.291
_shelx_estimated_absorpt_t_max   0.639
_shelx_res_checksum              98906
_shelx_hkl_checksum              12920
_shelx_fab_checksum              68852