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_7712553
_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         'C61 H68 Cl3 F N2 P Re, C4 H8 O'
_chemical_formula_sum            'C65 H76 Cl3 F N2 O P Re'
_chemical_formula_weight         1243.79
_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             2023-01-12
_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                77.64(3)
_cell_angle_beta                 75.03(3)
_cell_angle_gamma                81.35(3)
_cell_formula_units_Z            2
_cell_length_a                   10.858(2)
_cell_length_b                   14.422(3)
_cell_length_c                   20.631(4)
_cell_measurement_reflns_used    14346
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.23
_cell_measurement_theta_min      3.33
_cell_volume                     3033.2(12)
_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
;
 214 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  0.0721
_diffrn_reflns_av_unetI/netI     0.1409
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25108
_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         3.365
_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    2.206
_exptl_absorpt_correction_T_max  0.8662
_exptl_absorpt_correction_T_min  0.6590
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       needle
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.755
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         11861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.755
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0417
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7913
_reflns_number_total             11861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00446e2.cif
_cod_data_source_block           renphf_tripp1
_cod_database_code               7712553
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.539
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H64(0.046) H16(0.047) H42(0.051) H54(0.043) H63(0.056) H50(0.047)
 H12(0.042) H19(0.043) H30A(0.083) H30B(0.083) H30C(0.083) H60(0.049)
 H70(0.061) H58(0.048) H29(0.042) H13(0.051) H66(0.05) H21(0.048) H27(0.048)
 H55(0.053) H33A(0.103) H33B(0.103) H33C(0.103) H15(0.055) H62(0.066)
 H46A(0.105) H46B(0.105) H46C(0.105) H35(0.055) H40(0.056) H56(0.064)
 H32(0.058) H44(0.063) H57(0.06) H25(0.044) H20(0.055) H47(0.072) H31A(0.08)
 H31B(0.08) H31C(0.08) H67(0.066) H34A(0.101) H34B(0.101) H34C(0.101)
 H61(0.064) H69(0.079) H51A(0.091) H51B(0.091) H51C(0.091) H48A(0.123)
 H48B(0.123) H48C(0.123) H68(0.078) H52A(0.087) H52B(0.087) H52C(0.087)
 H10A(0.09) H10B(0.09) H37A(0.133) H37B(0.133) H37C(0.133) H10C(0.103)
 H10D(0.103) H36A(0.123) H36B(0.123) H36C(0.123) H49A(0.149) H49B(0.149)
 H49C(0.149) H10E(0.123) H10F(0.123) H45A(0.122) H45B(0.122) H45C(0.122)
 H10G(0.141) H10H(0.141)
 Fixed X: H64(0.556855) H16(0.538791) H42(0.598521) H54(0.857848)
 H63(0.336579) H50(0.45367) H12(0.855276) H19(0.448522) H30A(0.739855)
 H30B(0.847693) H30C(0.701892) H60(0.578767) H70(0.600484) H58(0.785551)
 H29(0.75582) H13(0.722267) H66(0.979299) H21(0.576696) H27(0.255131)
 H55(0.909578) H33A(0.44249) H33B(0.535282) H33C(0.534901) H15(0.40854)
 H62(0.237054) H46A(1.069439) H46B(1.067217) H46C(1.023988) H35(0.317141)
 H40(0.93291) H56(0.903478) H32(0.323453) H44(0.848475) H57(0.83792)
 H25(0.61404) H20(0.477197) H47(0.75417) H31A(0.818728) H31B(0.809652)
 H31C(0.916067) H67(1.019144) H34A(0.226977) H34B(0.254883) H34C(0.346904)
 H61(0.357838) H69(0.639997) H51A(0.27813) H51B(0.384169) H51C(0.378209)
 H48A(0.890944) H48B(0.803445) H48C(0.948404) H68(0.849832) H52A(0.404848)
 H52B(0.47067) H52C(0.32591) H10A(0.198653) H10B(0.105934) H37A(0.207309)
 H37B(0.109316) H37C(0.122749) H10C(0.335866) H10D(0.209008) H36A(0.149072)
 H36B(0.169435) H36C(0.278152) H49A(0.98589) H49B(0.875357) H49C(0.961777)
 H10E(0.259831) H10F(0.4038) H45A(0.798821) H45B(0.944778) H45C(0.912531)
 H10G(0.314431) H10H(0.421641)
 Fixed Y: H64(0.218457) H16(0.459643) H42(-0.05692) H54(0.431408)
 H63(0.260598) H50(0.173965) H12(0.594939) H19(0.434545) H30A(0.583624)
 H30B(0.495492) H30C(0.476707) H60(0.36875) H70(0.099918) H58(0.185087)
 H29(0.449544) H13(0.735263) H66(0.12068) H21(0.157065) H27(0.614849)
 H55(0.494268) H33A(0.896537) H33B(0.806087) H33C(0.837727) H15(0.60014)
 H62(0.357936) H46A(0.085007) H46B(0.198662) H46C(0.148527) H35(0.369516) H40(-
 0.021615) H56(0.400301) H32(0.768688) H44(0.22094) H57(0.248838) H25(0.682732)
 H20(0.29421) H47(-0.182895) H31A(0.642266) H31B(0.581725) H31C(0.548952) H67(-
 0.042116) H34A(0.768914) H34B(0.874366) H34C(0.815239) H61(0.414521) H69(-
 0.064077) H51A(0.100018) H51B(0.120429) H51C(0.014715) H48A(-0.284712) H48B(-
 0.220624) H48C(-0.19928) H68(-0.135377) H52A(-0.00545) H52B(0.074067)
 H52C(0.095288) H10A(0.966604) H10B(1.018733) H37A(0.463853) H37B(0.410797)
 H37C(0.52176) H10C(1.074489) H10D(1.140906) H36A(0.487643) H36B(0.37353)
 H36C(0.433021) H49A(-0.106439) H49B(-0.120899) H49C(-0.211565) H10E(1.124074)
 H10F(1.112684) H45A(0.145487) H45B(0.168652) H45C(0.062441) H10G(0.981481)
 H10H(0.960507)
 Fixed Z: H64(0.70569) H16(0.67578) H42(0.847496) H54(0.506479) H63(0.732238)
 H50(0.857235) H12(0.570491) H19(0.985184) H30A(0.908705) H30B(0.899891)
 H30C(0.935398) H60(0.514382) H70(0.614953) H58(0.465249) H29(0.822807)
 H13(0.547956) H66(0.571802) H21(1.019748) H27(0.813833) H55(0.38971)
 H33A(0.719353) H33B(0.696539) H33C(0.766359) H15(0.649359) H62(0.651575)
 H46A(0.888199) H46B(0.874703) H46C(0.823196) H35(0.884111) H40(0.882444)
 H56(0.311536) H32(0.741259) H44(0.903209) H57(0.348545) H25(0.783446)
 H20(1.059949) H47(0.841941) H31A(0.785793) H31B(0.73091) H31C(0.774577)
 H67(0.575087) H34A(0.858522) H34B(0.818333) H34C(0.865455) H61(0.541724)
 H69(0.619328) H51A(0.93709) H51B(0.972204) H51C(0.961399) H48A(0.894044)
 H48B(0.946493) H48C(0.911092) H68(0.597845) H52A(0.837288) H52B(0.776656)
 H52C(0.817751) H10A(0.717272) H10B(0.668369) H37A(0.967675) H37B(0.945823)
 H37C(0.916208) H10C(0.67655) H10D(0.66136) H36A(0.807171) H36B(0.822301)
 H36C(0.769308) H49A(0.778604) H49B(0.744317) H49C(0.774455) H10E(0.549169)
 H10F(0.560053) H45A(1.016792) H45B(0.998331) H45C(1.002841) H10G(0.528629)
 H10H(0.572026)
;
_shelx_res_checksum              69478
_olex2_submission_special_instructions 'No special instructions were received'