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_7712547
_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(C14.5 H14 Cl1.5 F0.5 N P0.5 Re0.5)'
_chemical_formula_sum            'C29 H28 Cl3 F N2 P Re'
_chemical_formula_weight         747.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-04
_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                70.369(4)
_cell_angle_beta                 83.840(5)
_cell_angle_gamma                89.494(5)
_cell_formula_units_Z            4
_cell_length_a                   10.2945(6)
_cell_length_b                   14.5070(8)
_cell_length_c                   21.6560(12)
_cell_measurement_reflns_used    23487
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      3.34
_cell_volume                     3027.3(3)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
 23 frames, detector distance = 120 mm
;
_diffrn_measurement_device       'STOE IPDS 2T'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25804
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.077
_diffrn_reflns_theta_min         3.345
_exptl_absorpt_coefficient_mu    4.358
_exptl_absorpt_correction_T_max  0.7537
_exptl_absorpt_correction_T_min  0.4635
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         11870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0178P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0411
_refine_ls_wR_factor_ref         0.0439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9046
_reflns_number_total             11870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00446e2.cif
_cod_data_source_block           renphf_tbi
_cod_database_code               7712547
_shelx_shelxl_version_number     2017/1
_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.a Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
2.b Aromatic/amide H refined with riding coordinates:
 C40(H40), C44(H44), C43(H43), C41(H41), C12(H12), C13(H13), C16(H16),
 C15(H15), C58(H58), C61(H61), C52(H52), C50(H50), C46(H46), C62(H62), C48(H48),
  C54(H54), C49(H49), C56(H56), C60(H60), C47(H47), C53(H53), C59(H59),
 C55(H55), C32(H32), C22(H22), C26(H26), C38(H38), C35(H35), C34(H34), C25(H25),
  C37(H37), C30(H30), C28(H28), C29(H29), C36(H36), C31(H31), C23(H23), C24(H24)
;
_shelx_res_checksum              34653
_olex2_submission_special_instructions 'No special instructions were received'