Molecular and Electronic Structures of Eight-Coordinate Uranium Bipyridine Complexes: A Rare Example of a Bipy(2-) Ligand Coordinated to a U(4+) Ion.
Rosenzweig, Michael W.; Heinemann, Frank W.; Maron, Laurent; Meyer, Karsten; Inorganic chemistry 56 (2017) 2792–2800; doi:10.1021/acs.inorgchem.6b02954

data_4345208
_publ_section_title
;
 Molecular and Electronic Structures of Eight-Coordinate Uranium
 Bipyridine Complexes: A Rare Example of a Bipy(2-) Ligand Coordinated to
 a U(4+) Ion.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2792
_journal_page_last               2800
_journal_paper_doi               10.1021/acs.inorgchem.6b02954
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C79 H104 N5 O3 U, 2(C4 H10 O2)'
_chemical_formula_sum            'C87 H124 N5 O7 U'
_chemical_formula_weight         1589.93
_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
_audit_creation_date             2016-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267)
;
_cell_angle_alpha                84.638(4)
_cell_angle_beta                 67.832(3)
_cell_angle_gamma                89.539(4)
_cell_formula_units_Z            2
_cell_length_a                   14.7489(11)
_cell_length_b                   15.1110(12)
_cell_length_c                   18.6349(14)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.61
_cell_volume                     3827.7(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker Smart APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            99073
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.659
_diffrn_reflns_theta_min         1.985
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.179
_exptl_absorpt_correction_T_max  0.5630
_exptl_absorpt_correction_T_min  0.4348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0665 before and 0.0431 after correction.
The Ratio of minimum to maximum transmission is 0.7723.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1658
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.276
_refine_diff_density_min         -1.698
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1086
_refine_ls_number_reflns         17475
_refine_ls_number_restraints     713
_refine_ls_restrained_S_all      1.244
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+9.1675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16546
_reflns_number_total             17475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02954_si_002.cif
_cod_data_source_block           mr1304
_cod_depositor_comments
'Adding full bibliography for 4345208--4345209.cif.'
_cod_database_code               4345208
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.612
_shelx_estimated_absorpt_t_min   0.409
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C101 \\sim O102 \\sim C103 \\sim C104 \\sim O105 \\sim C106 \\sim C111 \\sim
O112 \\sim C113 \\sim C114 \\sim O115 \\sim C116 \\sim C121 \\sim O122 \\sim
C123 \\sim C124 \\sim O125 \\sim C126: within 2A with sigma of 0.003 and sigma
for terminal atoms of 0.006
C201 \\sim O202 \\sim C203 \\sim C204 \\sim O205 \\sim C206 \\sim C211 \\sim
O212 \\sim C213 \\sim C214 \\sim O215 \\sim C216: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(C116) \\sim Ueq, Uanis(C126) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
3. Same fragment restrains
{C101, O102, C103, C104, O105, C106} sigma for 1-2: 0.02, 1-3: 0.04
{C116, O115, C114, C113, O112, C111} sigma for 1-2: 0.02, 1-3: 0.04
as
{C111, O112, C113, C114, O115, C116}
{C101, O102, C103, C104, O105, C106} sigma for 1-2: 0.02, 1-3: 0.04
{C126, O125, C124, C123, O122, C121} sigma for 1-2: 0.02, 1-3: 0.04
as
{C121, O122, C123, C124, O125, C126}
{C101, O102, C103, C104, O105, C106} sigma for 1-2: 0.02, 1-3: 0.04
{C206, O205, C204, C203, O202, C201} sigma for 1-2: 0.02, 1-3: 0.04
as
{C201, O202, C203, C204, O205, C206}
{C101, O102, C103, C104, O105, C106} sigma for 1-2: 0.02, 1-3: 0.04
as
{C211, O212, C213, C214, O215, C216}
4. Others
 1*[Sof(C101)+Sof(H10A)+Sof(H10B)+Sof(H10C)+Sof(O102)+Sof(C103)+Sof(H10D)+
 Sof(H10E)+Sof(C104)+Sof(H10F)+Sof(H10G)+Sof(O105)+Sof(C106)+Sof(H10H)+
 Sof(H10I)+Sof(H10J)]+1*[Sof(C111)+Sof(H11A)+Sof(H11B)+Sof(H11C)+Sof(O112)+
 Sof(C113)+Sof(H11D)+Sof(H11E)+Sof(C114)+Sof(H11F)+Sof(H11G)+Sof(O115)+
 Sof(C116)+Sof(H11H)+Sof(H11I)+Sof(H11J)]+1*[Sof(C121)+Sof(H12A)+Sof(H12B)+
 Sof(H12C)+Sof(O122)+Sof(C123)+Sof(H12D)+Sof(H12E)+Sof(C124)+Sof(H12F)+
 Sof(H12G)+Sof(O125)+Sof(C126)+Sof(H12H)+Sof(H12I)+Sof(H12J)]=1 with esd of
 0.0001
 Sof(C101)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(O102)=Sof(C103)=Sof(H10D)=
 Sof(H10E)=Sof(C104)=Sof(H10F)=Sof(H10G)=Sof(O105)=Sof(C106)=Sof(H10H)=
 Sof(H10I)=Sof(H10J)=FVAR(1)
 Sof(C111)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(O112)=Sof(C113)=Sof(H11D)=
 Sof(H11E)=Sof(C114)=Sof(H11F)=Sof(H11G)=Sof(O115)=Sof(C116)=Sof(H11H)=
 Sof(H11I)=Sof(H11J)=FVAR(2)
 Sof(C121)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(O122)=Sof(C123)=Sof(H12D)=
 Sof(H12E)=Sof(C124)=Sof(H12F)=Sof(H12G)=Sof(O125)=Sof(C126)=Sof(H12H)=
 Sof(H12I)=Sof(H12J)=FVAR(3)
 Sof(C211)=Sof(H21C)=Sof(H21D)=Sof(H21E)=Sof(O212)=Sof(C213)=Sof(H21F)=
 Sof(H21G)=Sof(C214)=Sof(H21H)=Sof(H21I)=Sof(O215)=Sof(C216)=Sof(H21J)=
 Sof(H21K)=Sof(H21L)=1-FVAR(4)
 Sof(C201)=Sof(H20C)=Sof(H20D)=Sof(H20E)=Sof(O202)=Sof(C203)=Sof(H20F)=
 Sof(H20G)=Sof(C204)=Sof(H20H)=Sof(H20I)=Sof(O205)=Sof(C206)=Sof(H20J)=
 Sof(H20K)=Sof(H20L)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C36(H36), C37(H37), C38(H38), C57(H57),
 C58(H58), C59(H59)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B), C28(H28A,H28B), C39(H39A,H39B), C40(H40A,H40B),
  C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C49(H49A,
 H49B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B),
 C64(H64A,H64B), C65(H65A,H65B), C103(H10D,H10E), C104(H10F,H10G), C113(H11D,
 H11E), C114(H11F,H11G), C123(H12D,H12E), C124(H12F,H12G), C203(H20F,H20G),
 C204(H20H,H20I), C213(H21F,H21G), C214(H21H,H21I)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C32(H32), C34(H34), C53(H53), C55(H55), C70(H70),
 C71(H71), C72(H72), C73(H73), C76(H76), C77(H77), C78(H78), C79(H79)
5.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C67(H67A,H67B,H67C), C68(H68A,
 H68B,H68C), C69(H69A,H69B,H69C), C101(H10A,H10B,H10C), C106(H10H,H10I,H10J),
 C111(H11A,H11B,H11C), C116(H11H,H11I,H11J), C121(H12A,H12B,H12C), C126(H12H,
 H12I,H12J), C201(H20C,H20D,H20E), C206(H20J,H20K,H20L), C211(H21C,H21D,H21E),
 C216(H21J,H21K,H21L)
;
_shelx_res_checksum              16250
_shelx_hkl_checksum              56114
_olex2_submission_special_instructions 'No special instructions were received'