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_4345385
_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         'C28 H20 O46 P8 U5, 3(H2 O)'
_chemical_formula_sum            'C28 H26 O49 P8 U5'
_chemical_formula_weight         2584.40
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                98.3060(10)
_cell_angle_beta                 93.8760(10)
_cell_angle_gamma                96.2960(10)
_cell_formula_units_Z            2
_cell_length_a                   14.3893(7)
_cell_length_b                   14.7147(7)
_cell_length_c                   15.3534(8)
_cell_measurement_reflns_used    5428
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      2.33
_cell_volume                     3185.8(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20337
_diffrn_reflns_theta_full        26.11
_diffrn_reflns_theta_max         26.11
_diffrn_reflns_theta_min         1.41
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    12.977
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1055 before and 0.0385 after correction.
The Ratio of minimum to maximum transmission is 0.6774.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2332
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         6.964
_refine_diff_density_min         -3.595
_refine_diff_density_rms         0.400
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         12583
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+34.3939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1460
_reflns_number_gt                10136
_reflns_number_total             12583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02765_si_002.cif
_cod_data_source_block           1
_cod_database_code               4345385
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H12_$1-H22_$2
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O34) \\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(O37) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O38) \\sim Ueq,
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O27) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O31) \\sim Ueq, Uanis(O32) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Free rotating group:
 O6W(H6WA,H6WB), O8W(H8WA,H8WB), O1AA(H1AA,H1AB)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C9(H9), C11(H11), C13(H13), C16(H16), C18(H18),
 C20(H20), C23(H23), C25(H25), C27(H27)
4.c Tetrahedral OH refined with riding coordinates:
 O12(H12), O17(H17), O22(H22), O28(H28), O30(H30), O33(H33), O35(H35), O38(H38)
;
_olex2_submission_special_instructions 'No special instructions were received'