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_4345389
_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         'C17 H14 Co N2 O8 P2 U, 0.5(H2 O)'
_chemical_formula_sum            'C17 H15 Co N2 O8.5 P2 U'
_chemical_formula_weight         742.21
_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                 94.020(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.689(2)
_cell_length_b                   10.786(2)
_cell_length_c                   18.730(4)
_cell_measurement_reflns_used    3065
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.599
_cell_measurement_theta_min      2.686
_cell_volume                     2154.1(7)
_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 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13367
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.157
_diffrn_reflns_theta_min         1.910
_exptl_absorpt_coefficient_mu    8.477
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1314 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.5599.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.599
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         4303
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0367P)^2^+0.4988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3518
_reflns_number_total             4303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02765_si_002.cif
_cod_data_source_block           5
_cod_original_cell_volume        2154.0(7)
_cod_original_formula_sum        'C17 H15 Co N2 O8.50 P2 U'
_cod_database_code               4345389
_shelx_estimated_absorpt_t_max   0.282
_shelx_estimated_absorpt_t_min   0.200
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid body (RIGU) restrains
 C19, C18, C16, C1, C7, N2, Co1, N1, C5, C3, C2, C17, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C1, C2, C3, C4, C5, C7, C16, C17, C18, N1A, C2A, C3A, C4A, C5A, C7A, C17A,
  C16A, C1A, N2, C19, N2A, C18A, C19A, Co1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(N1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=
 Sof(C7A)=Sof(C17A)=Sof(H17A)=Sof(N2A)=Sof(C16A)=Sof(H16A)=Sof(C18A)=Sof(H18A)=
 Sof(C19A)=Sof(H19A)=Sof(C1A)=Sof(H1A)=1-FVAR(1)
 Sof(N1)=Sof(N2)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=
 Sof(H4)=Sof(C5)=Sof(C7)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=
 Sof(C19)=Sof(H19)=FVAR(1)
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB)
4.b Me refined with riding coordinates:
 C6(H6A,H6B,H6C)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C11(H11), C13(H13), C16(H16),
 C17(H17), C18(H18), C19(H19), C2A(H2A), C3A(H3A), C4A(H4A), C17A(H17A),
 C16A(H16A), C18A(H18A), C19A(H19A), C1A(H1A)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'