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_7129177
_publ_section_title
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 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         'C148 H224 K5 N18 O P12 U3'
_chemical_formula_sum            'C148 H224 K5 N18 O P12 U3'
_chemical_formula_weight         3552.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-11 deposited with the CCDC.	2021-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.2940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.9263(10)
_cell_length_b                   26.2249(9)
_cell_length_c                   25.9999(14)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    192.99
_cell_measurement_theta_max      53.920
_cell_measurement_theta_min      2.932
_cell_volume                     19184.4(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      192.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            125416
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.939
_diffrn_reflns_theta_min         2.004
_diffrn_source_current           2.86
_diffrn_source_power             0.1993706
_diffrn_source_voltage           69.71
_exptl_absorpt_coefficient_mu    6.591
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.4477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1635 before and 0.0887 after correction.
The Ratio of minimum to maximum transmission is 0.5965.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             7188
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.270
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         17602
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0703P)^2^+35.9306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15267
_reflns_number_total             17602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04765e2.cif
_cod_data_source_block           1_a
_cod_database_code               7129177
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.559
_shelx_estimated_absorpt_t_min   0.505
_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. Restrained distances
 C32B-C33A
 2.65 with sigma of 0.002
 P2-C34A \\sim P2-C34B
 with sigma of 0.02
 O1-C32 \\sim O1-C31
 with sigma of 0.02
 C33B-C31B \\sim C33A-C31A \\sim C32A-C31B \\sim C32B-C31A
 with sigma of 0.02
 C35B-C34B \\sim C35A-C34A \\sim C36A-C34A \\sim C36B-C34B
 with sigma of 0.02
 P2-C31B \\sim P2-C31A
 with sigma of 0.02
 P3-C40A \\sim P3-C40B
 with sigma of 0.02
 C41A-C40B \\sim C41B-C40A \\sim C42B-C40B \\sim C42A-C40A
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C33 \\sim C31 \\sim O1 \\sim C32 \\sim C34 \\sim K1: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004 within 2A
C31A \\sim C31B \\sim C32A \\sim C32B \\sim C33A \\sim C33B: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C34A \\sim C34B \\sim C35A \\sim C35B \\sim C36A \\sim C36B: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004 within 2A
P3 \\sim C40A \\sim C40B \\sim C41A \\sim C41B \\sim C42A \\sim C42B: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
Uanis(C33) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C35A) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C36A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 P2, C34A, C34B, C35A, C35B, C36A, C36B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C34B)=Sof(H34B)=Sof(C35B)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36B)=
 Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36A)=
 Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
 Sof(C40B)=Sof(H40B)=Sof(C41B)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42B)=
 Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(2)
 Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42A)=
 Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(2)
 Sof(C31B)=Sof(H31D)=Sof(C32B)=Sof(H32F)=Sof(H32G)=Sof(H32H)=Sof(C33B)=
 Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(3)
 Sof(C31A)=Sof(H31C)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(H32E)=Sof(C33A)=
 Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(3)
 Fixed Sof: K1(0.5) O1(0.5) H5(0.5) C31(0.5) H31A(0.5) H31B(0.5) C32(0.5)
 H32A(0.5) H32B(0.5) H44B(0.5) C34(0.5) H34C(0.5) H34D(0.5) H34E(0.5) C33(0.5)
 H33G(0.5) H33H(0.5) H33I(0.5)
6.a Riding coordinates:
 C32B(H32F,H32G,H32H), C35A(H35A,H35B,H35C), C41B(H41D,H41E,H41F)
6.b Ternary CH refined with riding coordinates:
 C25(H25), C28(H28), C31A(H31C), C31B(H31D), C34A(H34A), C34B(H34B), C37(H37),
 C40A(H40A), C40B(H40B), C43(H43), C46(H46), C61(H61), C64(H64), C67(H67),
 C70(H70)
6.c Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C50(H50),
  C51(H51), C52(H52), C53(H53), C57(H57), C58(H58), C59(H59), C60(H60)
6.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C32A(H32C,H32D,H32E), C33A(H33A,H33B,H33C), C33B(H33D,H33E,H33F),
 C35B(H35D,H35E,H35F), C36A(H36A,H36B,H36C), C36B(H36D,H36E,H36F), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C41A(H41A,H41B,H41C), C42A(H42A,H42B,H42C),
 C42B(H42D,H42E,H42F), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,
 H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C),
 C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C34(H34C,H34D,H34E), C33(H33G,H33H,
 H33I)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              70595
_shelx_fab_checksum              23560
_olex2_submission_special_instructions 'No special instructions were received'