Entangled Uranyl Organic Frameworks with (10,3)-b Topology and Polythreading Network: Structure, Luminescence, and Computational Investigation.
Liu, Chao; Gao, Chao-Ying; Yang, Weiting; Chen, Fang-Yuan; Pan, Qing-Jiang; Li, Jiyang; Sun, Zhong-Ming; Inorganic chemistry 55 (2016) 5540–5548; doi:10.1021/acs.inorgchem.6b00582

data_4347764
_publ_section_title
;
 Entangled Uranyl Organic Frameworks with (10,3)-b Topology and
 Polythreading Network: Structure, Luminescence, and Computational
 Investigation.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5540
_journal_page_last               5548
_journal_paper_doi               10.1021/acs.inorgchem.6b00582
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C54 H34 O16 Si2 U2, 2(C12 H8 N2), 3.5(H2 O), O'
_chemical_formula_sum            'C78 H61 N4 O20.5 Si2 U2'
_chemical_formula_weight         1910.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-04-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                81.665(2)
_cell_angle_beta                 82.260(3)
_cell_angle_gamma                71.667(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4237(13)
_cell_length_b                   14.7281(17)
_cell_length_c                   25.599(3)
_cell_measurement_reflns_used    2016
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.075
_cell_measurement_theta_min      0.868
_cell_volume                     3674.5(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0376
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            21009
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         0.808
_exptl_absorpt_coefficient_mu    4.512
_exptl_absorpt_correction_T_max  0.258
_exptl_absorpt_correction_T_min  0.132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 - Bruker AXS was used for absorption correction. wR2(int) was 0.0672 before and 0.0527 after correction. The Ratio of minimum to maximum transmission is 0.8148. The  Lambda/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1858
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.771
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         12871
_refine_ls_number_restraints     299
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+9.6193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9477
_reflns_number_total             12871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00582_si_002.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C78 H61 N4 O20.50 Si2 U2'
_cod_database_code               4347764
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C83-C84
 1.4 with sigma of 0.02
 C79-C78
 1.4 with sigma of 0.02
 H2WA-N2
 1.8 with sigma of 0.02
 H2WB-O4
 2 with sigma of 0.02
 H2WB-O2W
 0.82 with sigma of 0.02
 O2W-H2WA
 0.82 with sigma of 0.02
 O12_$1-H1WA
 2 with sigma of 0.02
 H1WA-O2W
 2 with sigma of 0.02
 C65-C70
 1.4 with sigma of 0.02
 C69-C70
 1.45 with sigma of 0.001
 H3WA-O5W
 2.2 with sigma of 0.02
 H3WB-O4W
 2.2 with sigma of 0.02
 N6-N5 \\sim C79-C76
 with sigma of 0.02
3. Rigid bond restraints
 N6, C83, C79, C80, C81, C82, C76, C84, N5, C73, C74, C75, C77, C78
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 N4, C61, C62, C63, C64, C65, N3, C66, C67, C68, C69, C70, C71, C72
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Uiso/Uaniso restraints and constraints
Uanis(C77) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C75)
\\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C74) \\sim Ueq,
Uanis(C78) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C79)
\\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C67) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(N3)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C64) \\sim Ueq,
Uanis(C70) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(N4)
\\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C66) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: N6(0.5) C83(0.5) C79(0.5) C80(0.5) H80(0.5) C81(0.5) H81(0.5)
 C82(0.5) H82(0.5) C76(0.5) C84(0.5) N5(0.5) C73(0.5) H73(0.5) C74(0.5)
 H74(0.5) C75(0.5) H75(0.5) C77(0.5) H77(0.5) C78(0.5) H78(0.5) N4(0.5)
 C61(0.5) H61(0.5) C62(0.5) H62(0.5) C63(0.5) H63(0.5) C64(0.5) C65(0.5)
 N3(0.5) C66(0.5) H66(0.5) C67(0.5) H67(0.5) C68(0.5) H68(0.5) C69(0.5)
 C70(0.5) C71(0.5) H71(0.5) C72(0.5) H72(0.5) O3W(0.5) H3WA(0.5) H3WB(0.5)
 O7W(0.5) O6W(0.5) H6WA(0.5) H6WB(0.5) O4W(0.5) H4WA(0.5) H4WB(0.5) O5W(0.5)
6.a Riding coordinates:
 O3W(H3WA,H3WB), O2W(H2WA,H2WB), O1W(H1WA,H1WB), O6W(H6WA,H6WB), O4W(H4WA,H4WB)
6.b Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C1AA(H1AA), C3(H3), C4(H4), C4AA(H4AA), C6(H6), C7(H7),
 C7AA(H7AA), C10(H10), C11(H11), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C26(H26), C27(H27), C30(H30),
  C31(H31), C33(H33), C34(H34), C37(H37), C38(H38), C40(H40), C41(H41),
 C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C80(H80), C81(H81), C82(H82),
  C73(H73), C74(H74), C75(H75), C77(H77), C78(H78), C61(H61), C62(H62),
 C63(H63), C66(H66), C67(H67), C68(H68), C71(H71), C72(H72), C48(H48), C49(H49),
  C50(H50), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59)
6.c Fitted hexagon refined as free rotating group:
 N6(C83,C79,C80,C81,C82), C76(C84,N5,C73,C74,C75), C61(C62,C63,C64,C65,N3)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'