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_7712557
_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         'C31 H23 Cl3 F2 N2 P Re'
_chemical_formula_sum            'C31 H23 Cl3 F2 N2 P Re'
_chemical_formula_weight         785.03
_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             2023-01-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-01-17 deposited with the CCDC.	2023-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.82(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.170(2)
_cell_length_b                   21.178(4)
_cell_length_c                   12.895(3)
_cell_measurement_reflns_used    150
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.79
_cell_volume                     2962.1(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    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
 152 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_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  0.0596
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17347
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.008
_diffrn_reflns_theta_min         3.313
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.464
_exptl_absorpt_correction_T_max  0.7656
_exptl_absorpt_correction_T_min  0.4060
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.436
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.00141(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3979
_reflns_number_total             5800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00446e2.cif
_cod_data_source_block           ReNPh_PhF
_cod_database_code               7712557
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.454
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H22(0.057) H16(0.054) H36(0.044) H18(0.052) H15(0.063) H21(0.062)
 H12(0.055) H19(0.059) H13(0.065) H25(0.052) H40(0.051) H26(0.054) H24(0.045)
 H37(0.053) H28(0.046) H27(0.052) H38(0.062) H39(0.06) H30(0.047) H34(0.053)
 H31(0.054) H32(0.057) H33(0.06)
 Fixed X: H22(0.616) H16(0.710138) H36(0.573918) H18(0.803182) H15(0.868881)
 H21(0.709296) H12(0.7028) H19(0.897047) H13(0.866553) H25(0.505223)
 H40(0.239815) H26(0.541576) H24(0.434521) H37(0.615261) H28(0.424448)
 H27(0.495206) H38(0.470645) H39(0.285754) H30(0.165291) H34(0.198777) H31(-
 0.046304) H32(-0.13455) H33(-0.013325)
 Fixed Y: H22(0.386177) H16(0.14856) H36(0.278974) H18(0.337535) H15(0.086936)
 H21(0.485975) H12(0.035554) H19(0.43647) H13(-0.024046) H25(0.181329)
 H40(0.320658) H26(0.073606) H24(0.238795) H37(0.385636) H28(0.076909)
 H27(0.020982) H38(0.460731) H39(0.428411) H30(0.152178) H34(0.241132)
 H31(0.141832) H32(0.179021) H33(0.228898)
 Fixed Z: H22(0.25119) H16(0.65742) H36(0.62019) H18(0.550558) H15(0.759861)
 H21(0.274309) H12(0.401686) H19(0.571372) H13(0.501925) H25(0.884812)
 H40(0.430223) H26(0.877442) H24(0.725982) H37(0.649446) H28(0.556391)
 H27(0.71414) H38(0.563027) H39(0.451871) H30(0.332503) H34(0.616515)
 H31(0.316606) H32(0.450913) H33(0.601151)
;
_shelx_res_checksum              77384
_olex2_submission_special_instructions 'No special instructions were received'