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_4345386
_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 H9 O24 P4 U3, C12 H9 N2, C12 H8 N2, H2 O'
_chemical_formula_sum            'C38 H33 N4 O24 P4 U3'
_chemical_formula_weight         1767.65
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.9910(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8008(9)
_cell_length_b                   12.2543(7)
_cell_length_c                   30.2243(19)
_cell_measurement_reflns_used    5345
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.16
_cell_volume                     5481.1(6)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      296.15
_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_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30964
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.35
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    9.039
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.3272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1512 before and 0.0613 after correction.
The Ratio of minimum to maximum transmission is 0.4390.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3268
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         5.591
_refine_diff_density_min         -3.713
_refine_diff_density_rms         0.485
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         9652
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0633
_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^)+(0.0764P)^2^+143.1207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1651
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                7414
_reflns_number_total             9652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02765_si_002.cif
_cod_data_source_block           2
_cod_database_code               4345386
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 O22A-O23A
 2.3 with sigma of 0.02
 H1T-H22A
 2.2 with sigma of 0.02
 O20B-U3 \\sim U3-O20A
 with sigma of 0.02
 O18A-U3 \\sim U3-O18B
 with sigma of 0.02
 C1AA-C16 \\sim C16-C1AB
 with sigma of 0.02
 O22B-C1AA \\sim C1AA-O23B
 with sigma of 0.02
 O22A-C1AB \\sim C1AB-O23A
 with sigma of 0.02
3. Rigid bond restraints
 C1C, C11, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C1, C19, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C1T) \\sim Ueq, Uanis(C1R) \\sim Ueq, Uanis(C1P) \\sim Ueq, Uanis(C1H)
\\sim Ueq, Uanis(C1U) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(C1E) \\sim Ueq, Uanis(C1D) \\sim Ueq, Uanis(N4)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C1Q) \\sim Ueq,
Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C1G) \\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(C1F)
\\sim Ueq, Uanis(C1N) \\sim Ueq, Uanis(C1L) \\sim Ueq, Uanis(C1I) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1O) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1AA) \\sim Ueq, Uanis(C1AB) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O23A) \\sim Ueq, Uanis(O23B) \\sim Ueq, Uanis(O22B) \\sim Ueq,
Uanis(O22A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O18B) \\sim Ueq, Uanis(O18A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O21B) \\sim Ueq, Uanis(O21A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O19B) \\sim Ueq, Uanis(O19A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C1C) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(O18B) = Uanis(O18A)
Uanis(O19A) = Uanis(O19B)
Uanis(O21B) = Uanis(O21A)
Uanis(O20A) = Uanis(O20B)
Uanis(C1AB) = Uanis(C1AA)
Uanis(O23A) = Uanis(O23B)
Uanis(O22B) = Uanis(O22A)
5. Others
 Sof(O19B)=Sof(O20B)=Sof(O21A)=Sof(H21A)=Sof(O18B)=1-FVAR(1)
 Sof(O19A)=Sof(O20A)=Sof(O18A)=Sof(O21B)=Sof(H21B)=FVAR(1)
 Sof(O23A)=Sof(O22A)=Sof(H22A)=Sof(C1AB)=1-FVAR(2)
 Sof(C1AA)=Sof(O22B)=Sof(H22B)=Sof(O23B)=FVAR(2)
6.a Free rotating group:
 O19(H19A,H19B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C2(H2), C7(H7), N2(H2A), C19(H19), C1C(H1C), C1F(H1F),
 C1I(H1I), C18(H18), C1L(H1L), C1N(H1N), C1H(H1H), C14(H14), C1U(H1U), C10(H10),
  C1B(H1B), C1Q(H1Q), C8(H8), C1G(H1G), C1R(H1R), C1S(H1S), C1T(H1T)
6.c Fitted hexagon refined as free rotating group:
 C1P(C1H,C14,C1U,N3,C1E)
6.d Idealised tetrahedral OH refined as rotating group:
 O12(H12), O21A(H21A), O22A(H22A), O21B(H21B), O22B(H22B)
;
_olex2_submission_special_instructions 'No special instructions were received'