Phenylimido Complexes of Rhenium: Fluorine Substituents Provide Protection, Reactivity and Solubility
Claude, Guilhem; Kulitzki, Erika; Hagenbach, Adelheid; Roca Jungfer, Maximilian; Figueroa, Joshua S.; Abram, Ulrich; Dalton Transactions  (2023) –; doi:10.1039/D3DT00446E

data_7712551
_publ_section_title
;
 Phenylimido Complexes of Rhenium: Fluorine Substituents Provide
 Protection, Reactivity and Solubility
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00446E
_journal_year                    2023
_chemical_formula_moiety         '2(C40 H51 Cl1.5 F0.5 N1.5 Re0.5)'
_chemical_formula_sum            'C80 H102 Cl3 F N3 Re'
_chemical_formula_weight         1417.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-08
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2023-01-17 deposited with the CCDC.	2023-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.962(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.4087(9)
_cell_length_b                   25.0277(7)
_cell_length_c                   28.2885(13)
_cell_measurement_reflns_used    42512
_cell_measurement_temperature    200
_cell_measurement_theta_max      28.83
_cell_measurement_theta_min      3.25
_cell_volume                     16343.5(11)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL n/a (Sheldrick, 2008)'
_computing_structure_solution    'XT n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
 172 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.1020
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            107340
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.309
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           35
_diffrn_source_power             1.75
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.626
_exptl_absorpt_correction_T_max  0.5367
_exptl_absorpt_correction_T_min  0.3661
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
P. Coppens in "Crystallographic Computing" ed F.R Ahmed, S.R. Hall 
and C.P.Huber, Copenhagen, Munksgaard, (1979) pp 255-270
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_description       block
_exptl_crystal_F_000             5904
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.171
_refine_diff_density_min         -1.513
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1595
_refine_ls_number_reflns         32003
_refine_ls_number_restraints     2108
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0629P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17424
_reflns_number_total             32003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00446e2.cif
_cod_data_source_block           renphf_tripp2
_cod_database_code               7712551
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.497
_shelx_estimated_absorpt_t_min   0.322
_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
 C78-C85 \\sim C78-C85A
 with sigma of 0.02
 C86-C85 \\sim C86A-C85A
 with sigma of 0.02
 C85-C87 \\sim C85A-C87A
 with sigma of 0.02
 C78-C86 \\sim C78-C86A
 with sigma of 0.04
 C78-C87 \\sim C78-C87A
 with sigma of 0.04
 C86-C87 \\sim C86A-C87A
 with sigma of 0.04
 C122-C128 \\sim C122-C5
 with sigma of 0.02
 C130-C128 \\sim C8-C5
 with sigma of 0.02
 C129-C128 \\sim C7-C5
 with sigma of 0.02
 C122-C130 \\sim C122-C8
 with sigma of 0.04
 C122-C129 \\sim C122-C7
 with sigma of 0.04
 C130-C129 \\sim C8-C7
 with sigma of 0.04
 C6-C112 \\sim C114-C1D
 with sigma of 0.02
 C106-C166 \\sim C106-C1E
 with sigma of 0.04
 C106-C112 \\sim C106-C1D
 with sigma of 0.02
 C112-C166 \\sim C1D-C1E
 with sigma of 0.02
 C6-C106 \\sim C114-C106
 with sigma of 0.04
 C6-C166 \\sim C114-C1E
 with sigma of 0.04
 C26-C9 \\sim C26-C9A
 with sigma of 0.02
 C9-C15 \\sim C9A-C15A
 with sigma of 0.02
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
 C26-C15 \\sim C26-C15A
 with sigma of 0.04
 C26-C10 \\sim C26-C10A
 with sigma of 0.04
 C15-C10 \\sim C15A-C10A
 with sigma of 0.04
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C122) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C120) \\sim Ueq,
Uanis(C119) \\sim Ueq, Uanis(C124) \\sim Ueq, Uanis(C123) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(C118) = Uanis(C116) = Uanis(C117)
Uanis(C109) = Uanis(C110) = Uanis(C111)
Uanis(C85) = Uanis(C85A) = Uanis(C86A) = Uanis(C86) = Uanis(C87A) = Uanis(C87)
Uanis(C128) = Uanis(C129) = Uanis(C130)
Uanis(C130) = Uanis(C8) = Uanis(C5) = Uanis(C128) = Uanis(C7) = Uanis(C129)
Uanis(C9A) = Uanis(C9) = Uanis(C10) = Uanis(C10A) = Uanis(C15A) = Uanis(C15)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C114)=Sof(H11M)=Sof(H11N)=Sof(H11O)=Sof(C1D)=Sof(H1D)=Sof(C1E)=Sof(H1EA)=
 Sof(H1EB)=Sof(H1EC)=1-FVAR(1)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C112)=Sof(H112)=Sof(C166)=Sof(H16P)=
 Sof(H16Q)=Sof(H16R)=FVAR(1)
 Sof(C5)=Sof(H5)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=
 Sof(H8C)=1-FVAR(2)
 Sof(C130)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C129)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=Sof(C128)=Sof(H128)=FVAR(2)
 Sof(C87A)=Sof(H87D)=Sof(H87E)=Sof(H87F)=Sof(C85A)=Sof(H85A)=Sof(C86A)=
 Sof(H86D)=Sof(H86E)=Sof(H86F)=1-FVAR(3)
 Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(H86C)=Sof(C85)=Sof(H85)=Sof(C87)=Sof(H87A)=
 Sof(H87B)=Sof(H87C)=FVAR(3)
 Sof(C9A)=Sof(H9A)=Sof(C15A)=Sof(H15P)=Sof(H15Q)=Sof(H15R)=Sof(C10A)=Sof(H10D)=
 Sof(H10E)=Sof(H10F)=1-FVAR(4)
 Sof(C9)=Sof(H9)=Sof(C15)=Sof(H15M)=Sof(H15N)=Sof(H15O)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=Sof(H10C)=FVAR(4)
7.a Ternary CH refined with riding coordinates:
 C50(H50), C29(H29), C65(H65), C146(H146), C44(H44), C88(H88), C152(H152),
 C71(H71), C131(H131), C35(H35), C167(H167), C82(H82), C161(H161), C68(H68),
 C164(H164), C109(H109), C149(H149), C47(H47), C116(H116), C125(H125),
 C112(H112), C128(H128), C85(H85), C1D(H1D), C5(H5), C85A(H85A), C9(H9),
 C9A(H9A)
7.b Me refined with riding coordinates:
 C51(H51A,H51B,H51C), C147(H14A,H14B,H14C), C45(H45A,H45B,H45C), C74(H74A,H74B,
 H74C), C90(H90A,H90B,H90C), C148(H14D,H14E,H14F), C52(H52A,H52B,H52C),
 C72(H72A,H72B,H72C), C89(H89A,H89B,H89C), C6(H6A,H6B,H6C), C73(H73A,H73B,H73C),
  C67(H67A,H67B,H67C), C83(H83A,H83B,H83C), C37(H37A,H37B,H37C), C163(H16A,H16B,
 H16C), C153(H15A,H15B,H15C), C36(H36A,H36B,H36C), C168(H16D,H16E,H16F),
 C154(H15D,H15E,H15F), C165(H16G,H16H,H16I), C31(H31A,H31B,H31C), C169(H16J,
 H16K,H16L), C162(H16M,H16N,H16O), C69(H69A,H69B,H69C), C46(H46A,H46B,H46C),
 C30(H30A,H30B,H30C), C70(H70A,H70B,H70C), C111(H11A,H11B,H11C), C118(H11D,H11E,
 H11F), C166(H16P,H16Q,H16R), C110(H11G,H11H,H11I), C126(H12D,H12E,H12F),
 C117(H11J,H11K,H11L), C127(H12G,H12H,H12I), C132(H13D,H13E,H13F), C133(H13G,
 H13H,H13I), C66(H66A,H66B,H66C), C84(H84A,H84B,H84C), C151(H15G,H15H,H15I),
 C48(H48A,H48B,H48C), C150(H15J,H15K,H15L), C49(H49A,H49B,H49C), C114(H11M,H11N,
 H11O), C1E(H1EA,H1EB,H1EC)
7.c Aromatic/amide H refined with riding coordinates:
 C57(H57), C56(H56), C42(H42), C55(H55), C79(H79), C77(H77), C137(H137),
 C19(H19), C138(H138), C157(H157), C21(H21), C61(H61), C142(H142), C20(H20),
 C144(H144), C63(H63), C159(H159), C16(H16), C92(H92), C99(H99), C25(H25),
 C27(H27), C100(H100), C12(H12), C40(H40), C101(H101), C107(H107), C96(H96),
 C136(H136), C95(H95), C121(H121), C93(H93), C123(H123), C105(H105), C14(H14),
 C13(H13)
7.d Idealised Me refined as rotating group:
 C86(H86A,H86B,H86C), C130(H13A,H13B,H13C), C129(H12A,H12B,H12C), C87(H87A,
 H87B,H87C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C87A(H87D,H87E,H87F), C86A(H86D,
 H86E,H86F), C15(H15M,H15N,H15O), C10(H10A,H10B,H10C), C15A(H15P,H15Q,H15R),
 C10A(H10D,H10E,H10F)
;
_shelx_res_checksum              39640
_olex2_submission_special_instructions 'No special instructions were received'