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_7043696
_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_sum            'C52 H49 Cl2 F6 P4 Re'
_chemical_formula_weight         1168.89
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-06 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.00550(4)
_cell_length_b                   18.56730(7)
_cell_length_c                   24.45640(9)
_cell_measurement_reflns_used    47720
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      79.389
_cell_measurement_theta_min      2.985
_cell_volume                     4997.48(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27e (Rigaku OD, 2015)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            57867
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.687
_diffrn_reflns_theta_min         2.988
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.435
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       prism
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 4649 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         10772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+8.3449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                10651
_reflns_number_total             10772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02072d2.cif
_cod_data_source_block           GIM280517
_cod_database_code               7043696
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.332
_shelx_estimated_absorpt_t_max   0.755
_shelx_res_checksum              35886