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_7712548
_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         'C56 H54 Cl3 F N3 Re, 1.5[C7H8]'
_chemical_formula_sum            'C66.5 H66 Cl3 F N3 Re'
_chemical_formula_weight         1218.77
_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
_audit_creation_date             2023-03-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-03-03 deposited with the CCDC.	2023-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                77.386(4)
_cell_angle_beta                 86.283(4)
_cell_angle_gamma                64.117(4)
_cell_formula_units_Z            2
_cell_length_a                   12.5541(7)
_cell_length_b                   13.5237(7)
_cell_length_c                   20.8711(12)
_cell_measurement_reflns_used    31084
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      3.33
_cell_volume                     3109.2(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE RED'
_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    'XT n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25031
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.336
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.126
_exptl_absorpt_correction_T_max  0.9343
_exptl_absorpt_correction_T_min  0.4302
_exptl_absorpt_correction_type   none
_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    1.302
_exptl_crystal_description       needle
_exptl_crystal_F_000             1242
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.199
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         12158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10273
_reflns_number_total             12158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00446e2.cif
_cod_data_source_block           renphf_mes2
_cod_original_formula_sum        'C66.50 H66 Cl3 F N3 Re'
_cod_database_code               7712548
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.676
_shelx_estimated_absorpt_t_min   0.568
_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:
 C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C30(H30A,H30B,H30C), C29(H29A,H29B,
 H29C), C37(H37A,H37B,H37C), C63(H63A,H63B,H63C), C53(H53A,H53B,H53C), C28(H28A,
 H28B,H28C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C38(H38A,H38B,H38C)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C12(H12), C50(H50), C16(H16), C33(H33), C13(H13), C35(H35), C26(H26),
 C48(H48), C19(H19), C42(H42), C15(H15), C21(H21), C44(H44), C20(H20), C57(H57),
  C43(H43), C59(H59)
2.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 154 electrons were 
found in a volume of 789\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[C7H8] per Asymmetric Unit 
which account for 150 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37395
_shelx_fab_checksum              54413
_olex2_submission_special_instructions 'No special instructions were received'