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_7712550
_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         'C37 H36 Cl3 F N2 P Re'
_chemical_formula_sum            'C37 H36 Cl3 F N2 P Re'
_chemical_formula_weight         851.20
_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
_atom_sites_solution_primary     dual
_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                 99.46(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.349(4)
_cell_length_b                   10.552(2)
_cell_length_c                   19.299(4)
_cell_measurement_reflns_used    35908
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      3.35
_cell_volume                     3685.8(13)
_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 0.991
_diffrn_measurement_details
;
 285 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  0.0401
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26788
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.351
_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    3.590
_exptl_absorpt_correction_T_max  0.6075
_exptl_absorpt_correction_T_min  0.2534
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         7171
_refine_ls_number_restraints     500
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0331P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0565
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5929
_reflns_number_total             7171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00446e2.cif
_cod_data_source_block           renphf_iprop2
_cod_original_cell_volume        3686.1(13)
_cod_database_code               7712550
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.653
_shelx_estimated_absorpt_t_min   0.230
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H40(0.056) H34(0.06) H33(0.072) H46(0.062) H36(0.058) H30(0.06)
 H42(0.065) H37(0.073) H45(0.078) H38(0.077) H39(0.069) H31(0.071) H32(0.07)
 H21(0.08) H13(0.086) H12(0.081) H44(0.09) H16(0.075) H43(0.087) H15(0.094)
 H20(0.09) H19(0.092) H23(0.106) H28A(0.147) H28B(0.147) H28C(0.147) H26(0.103)
 H25A(0.184) H25B(0.184) H25C(0.184) H24A(0.187) H24B(0.187) H24C(0.187)
 H27A(0.203) H27B(0.203) H27C(0.203)
 Fixed X: H40(0.28375) H34(0.392312) H33(0.489169) H46(0.301945) H36(0.384543)
 H30(0.477898) H42(0.487236) H37(0.359102) H45(0.35162) H38(0.296742)
 H39(0.260038) H31(0.575769) H32(0.578408) H21(0.177141) H13(0.131263)
 H12(0.209936) H44(0.467294) H16(0.044701) H43(0.534765) H15(-0.03382)
 H20(0.090909) H19(0.050283) H23(0.10437) H28A(0.340096) H28B(0.357477)
 H28C(0.305307) H26(0.270138) H25A(0.126573) H25B(0.122237) H25C(0.188593)
 H24A(-0.017044) H24B(-0.001833) H24C(-0.007793) H27A(0.197056) H27B(0.259891)
 H27C(0.18378)
 Fixed Y: H40(0.237694) H34(0.576454) H33(0.61523) H46(0.265809) H36(0.102492)
 H30(0.22895) H42(0.439428) H37(-0.104856) H45(0.264742) H38(-0.140255)
 H39(0.030928) H31(0.271675) H32(0.462933) H21(0.750395) H13(-0.060546)
 H12(0.113913) H44(0.351578) H16(0.314685) H43(0.439911) H15(0.140601)
 H20(0.622254) H19(0.437782) H23(0.339376) H28A(0.65247) H28B(0.787424)
 H28C(0.778473) H26(0.67789) H25A(0.203399) H25B(0.141199) H25C(0.235187)
 H24A(0.37291) H24B(0.223557) H24C(0.295682) H27A(0.889477) H27B(0.90454)
 H27C(0.835351)
 Fixed Z: H40(0.837407) H34(0.825275) H33(0.917281) H46(0.592878)
 H36(0.681011) H30(0.799338) H42(0.691486) H37(0.713532) H45(0.488267)
 H38(0.806622) H39(0.87) H31(0.890063) H32(0.951559) H21(0.369439)
 H13(0.642665) H12(0.664657) H44(0.485801) H16(0.728107) H43(0.586353)
 H15(0.702636) H20(0.304079) H19(0.349314) H23(0.532519) H28A(0.458459)
 H28B(0.495311) H28C(0.420393) H26(0.547101) H25A(0.411847) H25B(0.486687)
 H25C(0.47802) H24A(0.484973) H24B(0.489243) H24C(0.415582) H27A(0.474357)
 H27B(0.541925) H27C(0.548737)
;
_shelx_res_checksum              48929
_olex2_submission_special_instructions 'No special instructions were received'