Construction of Uranyl Organic Hybrids by Phosphonate and in Situ Generated Carboxyphosphonate Ligands.
Liu, Chao; Yang, Weiting; Qu, Ning; Li, Lei-Jiao; Pan, Qing-Jiang; Sun, Zhong-Ming; Inorganic chemistry 56 (2017) 1669–1678; doi:10.1021/acs.inorgchem.6b02765

data_4345387
_publ_section_title
;
 Construction of Uranyl Organic Hybrids by Phosphonate and in Situ
 Generated Carboxyphosphonate Ligands.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1669
_journal_page_last               1678
_journal_paper_doi               10.1021/acs.inorgchem.6b02765
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C14 H12 O18 P4 U3, C10 H10 N2, H2 O'
_chemical_formula_sum            'C24 H24 N2 O19 P4 U3'
_chemical_formula_weight         1482.42
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-10-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.6360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9899(6)
_cell_length_b                   17.4465(9)
_cell_length_c                   17.2385(9)
_cell_measurement_reflns_used    3415
_cell_measurement_temperature    200
_cell_measurement_theta_max      26.006
_cell_measurement_theta_min      2.288
_cell_volume                     3581.8(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0648
_diffrn_reflns_av_unetI/netI     0.0787
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20372
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.666
_exptl_absorpt_coefficient_mu    13.790
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.3998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1124 before and 0.0654 after correction.
The Ratio of minimum to maximum transmission is 0.5364.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.837
_refine_diff_density_min         -2.864
_refine_diff_density_rms         0.399
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         6340
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0752P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1390
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4830
_reflns_number_total             6340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02765_si_002.cif
_cod_data_source_block           3
_cod_database_code               4345387
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Riding coordinates:
 O1W(H1WA,H1WB)
3.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C9(H9), C11(H11), C13(H13), C15(H15), C16(H16),
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), N1(H1), N2(H2A)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'