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_7712552
_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 F N3 O2 P Re'
_chemical_formula_sum            'C31 H23 Cl3 F N3 O2 P Re'
_chemical_formula_weight         812.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-01-10
_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                 99.20(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0634(18)
_cell_length_b                   25.461(5)
_cell_length_c                   13.352(3)
_cell_measurement_reflns_used    12604
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.52
_cell_measurement_theta_min      3.35
_cell_volume                     3041.5(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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
 148 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  0.0637
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17337
_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         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
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.352
_exptl_absorpt_correction_T_max  0.7514
_exptl_absorpt_correction_T_min  0.2378
_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    1.773
_exptl_crystal_description       plate
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.822
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.822
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0101P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0423
_refine_ls_wR_factor_ref         0.0459
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4098
_reflns_number_total             5953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00446e2.cif
_cod_data_source_block           renphf_phno2
_cod_original_cell_volume        3041.4(11)
_cod_database_code               7712552
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.328
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H18(0.04) H24(0.04) H34(0.043) H19(0.047) H40(0.038) H16(0.05)
 H30(0.044) H15(0.053) H37(0.053) H36(0.047) H22(0.064) H31(0.057) H12(0.043)
 H28(0.054) H39(0.05) H38(0.053) H27(0.061) H25(0.048) H13(0.049) H21(0.069)
 H26(0.058) H32(0.059) H33(0.057)
 Fixed X: H18(0.908033) H24(0.59035) H34(0.240439) H19(0.938817) H40(0.49663)
 H16(0.900199) H30(0.497484) H15(1.009639) H37(0.044453) H36(0.205546)
 H22(0.604077) H31(0.377557) H12(0.860073) H28(0.349488) H39(0.333331)
 H38(0.107512) H27(0.347195) H25(0.5749) H13(0.97292) H21(0.633536)
 H26(0.455154) H32(0.195128) H33(0.128495)
 Fixed Y: H18(0.325493) H24(0.05096) H34(0.204718) H19(0.414537) H40(0.116968)
 H16(0.221331) H30(0.233791) H15(0.211032) H37(0.052703) H36(0.097887)
 H22(0.365474) H31(0.314092) H12(0.063276) H28(0.161321) H39(0.071316)
 H38(0.039763) H27(0.105984) H25(-0.003781) H13(0.053757) H21(0.454324)
 H26(0.023315) H32(0.340709) H33(0.286109)
 Fixed Z: H18(0.432702) H24(0.504936) H34(0.621123) H19(0.394411) H40(0.76121)
 H16(0.399334) H30(0.405207) H15(0.253114) H37(0.5903) H36(0.500519)
 H22(0.612818) H31(0.369377) H12(0.418997) H28(0.329702) H39(0.848931)
 H38(0.762264) H27(0.188318) H25(0.364981) H13(0.273217) H21(0.569729)
 H26(0.208313) H32(0.463007) H33(0.588028)
;
_shelx_res_checksum              97988
_olex2_submission_special_instructions 'No special instructions were received'