Uranium(VI) coordination polymers with pyromellitate ligand: Unique 1D channel structures and diverse fluorescence
Zhang, Yingjie; Bhadbhade, Mohan; Karatchevtseva, Inna; Price, Jason R.; Liu, Hao; Zhang, Zhaoming; Kong, Linggen; Čejka, Jiří; Lu, Kim; Lumpkin, Gregory R.; Journal of Solid State Chemistry 226 (2015) 42–49; doi:10.1016/j.jssc.2015.01.033

data_1561959
_publ_section_title
;
 Uranium(VI) coordination polymers with pyromellitate ligand: Unique 1D
 channel structures and diverse fluorescence
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              42
_journal_page_last               49
_journal_paper_doi               10.1016/j.jssc.2015.01.033
_journal_volume                  226
_journal_year                    2015
_chemical_formula_moiety         'C5 H O14 U3, N, 2.83(O)'
_chemical_formula_sum            'C5 H N O16.83 U3'
_chemical_formula_weight         1058.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-04-14
_audit_creation_method
;
 ?
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.647(3)
_cell_length_b                   13.284(3)
_cell_length_c                   24.926(5)
_cell_measurement_temperature    100(2)
_cell_volume                     4187.6(16)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BLU-ICE (McPhillips et al., 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008) and OLEX-2 (Dolomanov <i>et al</i>., 2009)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_type            'ADSC Quantum 210r'
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7293
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.893
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            48240
_diffrn_reflns_point_group_measured_fraction_full 0.893
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.950
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.782
_diffrn_source                   'Synchrotron BM'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.650
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.358
_exptl_crystal_description       needles
_exptl_crystal_F_000             3589
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         6.681
_refine_diff_density_min         -3.870
_refine_diff_density_rms         0.460
_refine_ls_extinction_coef       0.00048(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3469
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0228P)^2^+571.7494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1424
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3342
_reflns_number_total             3469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Complex_2.cif.cif
_cod_data_source_block           pnnm
_cod_original_cell_volume        4187.6(15)
_cod_database_code               1561959
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.618
_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 O13, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C5 \\sim C6: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C1 \\sim C2 \\sim O11 \\sim O10: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O13 \\sim C4: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Others
 Fixed Sof: O1W(0.33333) O2W(0.16667) O3W(0.33333) O4W(0.33333) O5W(0.33333)
 O7W(0.33333)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6)
;
_shelx_res_checksum              54115
_shelx_hkl_checksum              2015