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_7043694
_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_absolute_configuration ad
_chemical_formula_moiety         'C18 H25 N Tc, F6 P'
_chemical_formula_sum            'C18 H25 F6 N P Tc'
_chemical_formula_weight         498.36
_chemical_name_systematic        'to be completed'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-06 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.370(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1171(4)
_cell_length_b                   15.7539(7)
_cell_length_c                   15.0788(7)
_cell_measurement_reflns_used    13209
_cell_measurement_temperature    183(1)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      2.5
_cell_volume                     1927.67(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      183(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -18.00  78.00   0.50   60.00    --    4.71  77.00 -60.00  192
  2  \w     47.00  77.00   0.50   60.00    --    4.71  57.00-120.00   60
  3  \w     21.00  57.00   0.50   60.00    --   -5.80  57.00 -30.00   72
  4  \w     -7.00  82.00   0.50   60.00    --    4.71  38.00 -30.00  178
  5  \w     -1.00  82.00   0.50   60.00    --    4.71  38.00 120.00  166
  6  \w    -25.00  19.00   0.50   60.00    --   -5.80 -99.00  90.00   88
  7  \w     44.00  82.00   0.50   60.00    --    4.71-169.00 128.00   76
  8  \w    -68.00  20.00   0.50   60.00    --    4.71 -57.00 -90.00  176
  9  \w     -9.00  36.00   0.50   60.00    --    4.71  57.00-120.00   90
 10  \w     38.00  84.00   0.50   60.00    --    4.71 178.00-180.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0400644000
_diffrn_orient_matrix_UB_12      -0.0325304000
_diffrn_orient_matrix_UB_13      0.0237757000
_diffrn_orient_matrix_UB_21      -0.0253260000
_diffrn_orient_matrix_UB_22      0.0302432000
_diffrn_orient_matrix_UB_23      0.0317558000
_diffrn_orient_matrix_UB_31      -0.0734474000
_diffrn_orient_matrix_UB_32      0.0073652000
_diffrn_orient_matrix_UB_33      -0.0253035000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21006
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.401
_diffrn_reflns_theta_min         2.586
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.13a (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       needle
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         21006
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1125P)^2^+0.3289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1356
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                20410
_reflns_number_total             21006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02072d2.cif
_cod_data_source_block           hb300517_twin1_hklf5
_cod_database_code               7043694
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
2.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;