Redox-induced reversible P-P coupling in a uranium complex
Fang, Wei; Carpentier, Ambre; Sun, Xiong; Zhao, Yue; Maron, Laurent; Zhu, Congqing; Chemical Communications  (2021) –; doi:10.1039/D1CC04765E

data_7129176
_publ_section_title
;
 Redox-induced reversible P-P coupling in a uranium complex
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC04765E
_journal_year                    2021
_chemical_formula_moiety         'C48 H72 N6 P4 U'
_chemical_formula_sum            'C48 H72 N6 P4 U'
_chemical_formula_weight         1095.02
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-08-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-11 deposited with the CCDC.	2021-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.9960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.2995(9)
_cell_length_b                   18.4153(8)
_cell_length_c                   26.0924(10)
_cell_measurement_reflns_used    8826
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.27
_cell_volume                     9863.4(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1085
_diffrn_reflns_av_unetI/netI     0.1197
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            71494
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         1.941
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.460
_exptl_absorpt_correction_T_max  0.4915
_exptl_absorpt_correction_T_min  0.4176
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1747 before and 0.0821 after correction.
The Ratio of minimum to maximum transmission is 0.8496.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             4432
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.040
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1106
_refine_ls_number_reflns         22594
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.0687
_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^)+68.9451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1356
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13528
_reflns_number_total             22594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04765e2.cif
_cod_data_source_block           sx2020091501_0m
_cod_database_code               7129176
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.724
_shelx_estimated_absorpt_t_min   0.682
_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
2. Restrained distances
 C87A-C85 \\sim C87-C85
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C87A \\sim C87: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
4. Rigid body (RIGU) restrains
 C87A, C87, C85
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C87A)=Sof(H87A)=Sof(H87B)=Sof(H87C)=1-FVAR(1)
 Sof(H85)=Sof(C87)=Sof(H87D)=Sof(H87E)=Sof(H87F)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C61(H61), C19(H19), C22(H22), C40(H40), C43(H43), C37(H37), C16(H16),
 C46(H46), C70(H70), C67(H67), C64(H64), C94(H94), C13(H13), C91(H91), C88(H88),
  C85(H85)
6.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C50(H50), C26(H26), C80(H80), C77(H77), C29(H29), C53(H53), C2(H2),
 C76(H76), C8(H8), C9(H9), C57(H57), C32(H32), C28(H28), C52(H52), C59(H59),
 C11(H11), C33(H33), C81(H81), C56(H56), C27(H27), C34(H34), C51(H51), C83(H83),
  C74(H74), C4(H4), C3(H3), C58(H58), C10(H10), C75(H75), C5(H5), C82(H82)
6.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C65(H65A,H65B,H65C), C38(H38A,H38B,H38C), C63(H63A,H63B,
 H63C), C95(H95A,H95B,H95C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C17(H17A,
 H17B,H17C), C68(H68A,H68B,H68C), C66(H66A,H66B,H66C), C39(H39A,H39B,H39C),
 C92(H92A,H92B,H92C), C42(H42A,H42B,H42C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C41(H41A,H41B,H41C), C47(H47A,H47B,H47C), C44(H44A,H44B,H44C), C72(H72A,
 H72B,H72C), C48(H48A,H48B,H48C), C45(H45A,H45B,H45C), C69(H69A,H69B,H69C),
 C15(H15A,H15B,H15C), C89(H89A,H89B,H89C), C62(H62A,H62B,H62C), C71(H71A,H71B,
 H71C), C96(H96A,H96B,H96C), C14(H14A,H14B,H14C), C86(H86A,H86B,H86C), C90(H90A,
 H90B,H90C), C93(H93A,H93B,H93C), C87A(H87A,H87B,H87C), C87(H87D,H87E,H87F)
;
_shelx_res_checksum              27853
_olex2_submission_special_instructions 'No special instructions were received'