CuPYDC Metalloligands and Postsynthetic Rearrangement/Metalation as Routes to Bimetallic Uranyl Containing Hybrid Materials: Syntheses, Structures, and Fluorescence
Kerr, Andrew T.; Cahill, Christopher L.; Crystal Growth & Design 14 (2014) 4094–; doi:10.1021/cg5007132

data_4511576
_publ_section_title
;
 CuPYDC Metalloligands and Postsynthetic Rearrangement/Metalation as
 Routes to Bimetallic Uranyl Containing Hybrid Materials: Syntheses,
 Structures, and Fluorescence
;
_journal_issue                   8
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4094
_journal_paper_doi               10.1021/cg5007132
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C14 H12 Cu N2 O13 U'
_chemical_formula_weight         717.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4363(11)
_cell_length_b                   13.1485(17)
_cell_length_c                   17.833(2)
_cell_measurement_reflns_used    29573
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      47.505
_cell_measurement_theta_min      4.533
_cell_volume                     1978.1(4)
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_collection       'APEX, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27739
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         30.270
_diffrn_reflns_theta_min         2.284
_diffrn_source                   'Fine-Focus Sealed Tube'
_diffrn_source_type              'Bruker APEXII'
_exptl_absorpt_coefficient_mu    9.324
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6193
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    2.410
_exptl_crystal_description       Prisim
_exptl_crystal_F_000             1340
_exptl_crystal_recrystallization_method Hydrothermal
_exptl_crystal_size_max          0.056
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.045
_refine_diff_density_max         2.952
_refine_diff_density_min         -2.243
_refine_diff_density_rms         0.219
_refine_ls_abs_structure_details
;
 Flack x determined using 1872 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.009(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         5633
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1023
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.945
_reflns_number_gt                4467
_reflns_number_total             5633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5007132_si_002.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 4511575--4511577.cif.'
_cod_database_code               4511576
_shelxl_version_number           2013-4
_shelx_res_checksum              62504
_shelx_hkl_checksum              41246