Structure and Reactivities of Rhenium and Technetium bis-Arene Sandwich Complexes [M(η6-arene)2]+
Alberto, Roger; Meola, Giuseppe; Braband, Henrik; Jordi, Sara; Fox, Thomas; Blacque, Oliver; Spingler, Bernhard; Dalton Trans.  (2017) –; doi:10.1039/C7DT02072D

data_7043690
_publ_section_title
;
 Structure and Reactivities of Rhenium and Technetium bis-Arene Sandwich
 Complexes [M(\h6-arene)2]+
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02072D
_journal_year                    2017
_chemical_formula_moiety         'C17 H21 Br Tc, Cl'
_chemical_formula_sum            'C17 H21 Br Cl Tc'
_chemical_formula_weight         438.70
_chemical_name_common            '[Tc(Me5Ph)(PhBr)]Cl'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-06-06 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                87.599(5)
_cell_angle_beta                 86.191(5)
_cell_angle_gamma                85.980(4)
_cell_formula_units_Z            2
_cell_length_a                   7.0418(4)
_cell_length_b                   9.2033(5)
_cell_length_c                   12.4028(7)
_cell_measurement_reflns_used    3675
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      29.8600
_cell_measurement_theta_min      2.8260
_cell_volume                     799.49(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.16a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.16a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.16a (Rigaku OD, 2015)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 200000
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8837
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    3.554
_exptl_absorpt_correction_T_max  0.9859
_exptl_absorpt_correction_T_min  0.4953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.16a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.495
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+0.0678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                3075
_reflns_number_total             3914
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt02072d2.cif
_cod_data_source_block           hb130217
_cod_original_cell_volume        799.48(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7043690