Uranyl Carboxyphosphonates Derived from Hydrothermal in Situ Ligand Reaction: Syntheses, Structures, and Computational Investigations.
Wu, Dai; Bai, Xiaojing; Tian, Hong-Rui; Yang, Weiting; Li, Zewen; Huang, Qing; Du, Shiyu; Sun, Zhong-Ming; Inorganic chemistry 54 (2015) 8617–8624; doi:10.1021/acs.inorgchem.5b01266

data_4344081
_publ_section_title
;
 Uranyl Carboxyphosphonates Derived from Hydrothermal in Situ Ligand
 Reaction: Syntheses, Structures, and Computational Investigations.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8617
_journal_page_last               8624
_journal_paper_doi               10.1021/acs.inorgchem.5b01266
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C26 H18 N2 O30 P4 U3'
_chemical_formula_weight         1676.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                81.842(2)
_cell_angle_beta                 85.131(2)
_cell_angle_gamma                87.5750(10)
_cell_formula_units_Z            1
_cell_length_a                   9.6088(8)
_cell_length_b                   9.7439(8)
_cell_length_c                   11.0648(9)
_cell_measurement_reflns_used    2028
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.86
_cell_measurement_theta_min      2.62
_cell_volume                     1021.30(15)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6517
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.141
_diffrn_reflns_theta_min         1.865
_exptl_absorpt_coefficient_mu    12.128
_exptl_absorpt_correction_T_max  0.1953
_exptl_absorpt_correction_T_min  0.0909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.232
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         4038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0327P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3342
_reflns_number_total             4038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01266_si_002.cif
_cod_data_source_block           DPTP-U1
_cod_depositor_comments
'Adding full bibliography for 4344081--4344083.cif.'
_cod_database_code               4344081
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.091
_shelx_estimated_absorpt_t_max   0.195
_shelx_res_checksum              48749
_shelx_hkl_checksum              8780