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_1561960
_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         '0.25(C80 H16 O92 U12), 11.67(O0.6)'
_chemical_formula_sum            'C20 H4 O30 U3'
_chemical_formula_weight         1438.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-04-27
_audit_creation_method
;
 ?
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.683(2)
_cell_length_b                   16.583(3)
_cell_length_c                   22.832(5)
_cell_measurement_temperature    100(2)
_cell_volume                     4423.5(15)
_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 0.886
_diffrn_measured_fraction_theta_max 0.978
_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  0.0656
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.886
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49380
_diffrn_reflns_point_group_measured_fraction_full 0.886
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.950
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         1.830
_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    5.102
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.160
_exptl_crystal_description       needles
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.242
_refine_diff_density_min         -2.214
_refine_diff_density_rms         0.233
_refine_ls_extinction_coef       0.00113(10)
_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   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3669
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+83.3679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1206
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3461
_reflns_number_total             3669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Complex3.cif.cif
_cod_data_source_block           pnma
_cod_database_code               1561960
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.515
_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C4 \\sim C5: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) = Uanis(C5) = Uanis(C6)
Uanis(C2) = Uanis(C9) = Uanis(C1)
Uanis(O4) = Uanis(O3) = Uanis(O8)
Uanis(O2) = Uanis(O5) = Uanis(O7)
3. Others
 Fixed Sof: O2W(0.35) O3W(0.25) O4W(0.15) O5W(0.25) O6W(0.5) O7W(0.5) O8W(0.5)
 O9W(0.125) O10W(0.25) O11W(0.25) O12W(0.125) O13W(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8)
;