Uranium(VI) complexes with isonicotinic acid: from monomer to 2D polymer with unique U-N bonding
Zhang, Yingjie; Karatchevtseva, Inna; Price, Jason R.; aharonovich, igor; Kadi, Fatima; Lumpkin, Gregory R.; Li, Feng; RSC Adv.  (2015) –; doi:10.1039/C5RA01272D

data_7220055
_publ_section_title
;
 Uranium(VI) complexes with isonicotinic acid: from monomer to 2D polymer
 with unique U-N bonding
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA01272D
_journal_year                    2015
_chemical_formula_moiety         'C6 H5 N O5 U'
_chemical_formula_sum            'C6 H5 N O5 U'
_chemical_formula_weight         409.14
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-03
_audit_creation_method
;
 ?
;
_audit_update_record
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2015-03-06 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.191(2)
_cell_length_b                   8.6030(17)
_cell_length_c                   18.665(4)
_cell_measurement_temperature    100(2)
_cell_volume                     1636.4(6)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.885
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7293
_diffrn_reflns_av_R_equivalents  0.1003
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.885
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17201
_diffrn_reflns_point_group_measured_fraction_full 0.885
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         2.239
_diffrn_source                   'Synchrotron BM'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.108
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.321
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.437
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.304
_refine_ls_extinction_coef       0.00174(18)
_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   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         1321
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0330
_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^)+(0.0430P)^2^+8.9320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1200
_reflns_number_total             1321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra01272d2.cif
_cod_data_source_block           pbca
_cod_database_code               7220055
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.839
_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6)
Uanis(O1) = Uanis(O2) = Uanis(O3)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C6(H6)
;
_shelx_res_checksum              12403
_olex2_submission_special_instructions 'No special instructions were received'