Unsymmetrical Tren-Based Ligands: Synthesis and Reactivity of Rhenium Complexes
Nadia C. Mösch-Zanetti; Sinje Köpke; Regine Herbst-Irmer; Manuel Hewitt; Inorganic Chemistry 41 (2002) 3513–3520; doi:10.1021/ic025572u

data_4318179
_publ_section_title
;
 Unsymmetrical Tren-Based Ligands: Synthesis and Reactivity of Rhenium
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3513
_journal_page_last               3520
_journal_paper_doi               10.1021/ic025572u
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C56 H42 Br Cl14 F30 N8 O Re2'
_chemical_formula_weight         2361.59
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                76.00(2)
_cell_angle_beta                 81.54(2)
_cell_angle_gamma                68.25(2)
_cell_formula_units_Z            2
_cell_length_a                   13.316(2)
_cell_length_b                   17.316(2)
_cell_length_c                   18.332(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      2.29
_cell_volume                     3801.7(10)
_computing_cell_refinement       'Siemens SAINT (V. 5.00, Siemens 1998)'
_computing_data_collection       'Siemens SMART (V. 4.202, Siemens 1996)'
_computing_data_reduction        'Siemens SAINT (V. 5.00, Siemens 1998)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (V. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Stoe-Siemens-Huber four circle diffractometer'
_diffrn_measurement_method       'phi and omega scan'
_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  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            102817
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    4.319
_exptl_absorpt_correction_T_max  0.6720
_exptl_absorpt_correction_T_min  0.2213
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.063
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lamina
_exptl_crystal_F_000             2270
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.147
_refine_diff_density_min         -2.173
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.00035(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1103
_refine_ls_number_reflns         17483
_refine_ls_number_restraints     320
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0294P)^2^+11.1217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                15148
_reflns_number_total             17483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025572u_s1_2.cif
_cod_data_source_block           klexti
_cod_original_cell_volume        3801.7(8)
_cod_database_code               4318179