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_7712549
_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
'C47 H27 Cl3 F14 N2 P Re, [+ solvents]0.5[CH2Cl2]'
_chemical_formula_sum            'C47 H27 Cl3 F14 N2 P Re'
_chemical_formula_weight         1209.22
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-03-06 deposited with the CCDC.	2023-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   46.9293(10)
_cell_length_b                   46.9293(10)
_cell_length_c                   8.3649(2)
_cell_measurement_reflns_used    9334
_cell_measurement_temperature    105.0
_cell_measurement_theta_max      66.62
_cell_measurement_theta_min      2.66
_cell_volume                     18422.5(7)
_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      105.0
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'PHOTON 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Venture Duo'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            173200
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.620
_diffrn_reflns_theta_max         66.620
_diffrn_reflns_theta_min         5.332
_exptl_absorpt_coefficient_mu    7.935
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1159 before and 0.0740 after correction.
The Ratio of minimum to maximum transmission is 0.7334.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       block
_exptl_crystal_F_000             9440
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.476
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         8121
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+109.6705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7332
_reflns_number_total             8121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00446e2.cif
_cod_data_source_block           renphf_darf1
_cod_original_cell_volume        18422.5(9)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7712549
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.569
_shelx_estimated_absorpt_t_min   0.382
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F12A-C38 \\sim F14B-C38
 with sigma of 0.02
 C38-F14A \\sim C38-F12B
 with sigma of 0.02
 F13A-C38 \\sim F13B-C38
 with sigma of 0.02
 F9A-C37 \\sim F9B-C37
 with sigma of 0.02
 F11A-C37 \\sim F10B-C37
 with sigma of 0.02
 F10A-C37 \\sim F11B-C37
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F10A) = Uanis(F10B) = Uanis(F11A) = Uanis(F9B) = Uanis(F9A) = Uanis(F11B)
Uanis(F13B) = Uanis(F13A)
4. Others
 Sof(F14B)=Sof(F13B)=Sof(F12B)=1-FVAR(1)
 Sof(F12A)=Sof(F13A)=Sof(F14A)=FVAR(1)
 Sof(F11B)=Sof(F10B)=Sof(F9B)=1-FVAR(2)
 Sof(F9A)=Sof(F10A)=Sof(F11A)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C56(H56), C44(H44), C40(H40), C19(H19), C24(H24), C52(H52), C26(H26),
 C16(H16), C12(H12), C28(H28), C41(H41), C21(H21), C13(H13), C15(H15), C55(H55),
  C32(H32), C50(H50), C53(H53), C43(H43), C34(H34), C46(H46), C36(H36),
 C42(H42), C54(H54), C48(H48), C47(H47), C49(H49)
;
_shelx_res_checksum              25849
_olex2_submission_special_instructions 'No special instructions were received'