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_4318180
_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            'C25 H15 Br2 F15 N4 Re'
_chemical_formula_weight         1002.43
_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                80.86(2)
_cell_angle_beta                 86.87(2)
_cell_angle_gamma                77.18(2)
_cell_formula_units_Z            4
_cell_length_a                   13.797(2)
_cell_length_b                   13.959(2)
_cell_length_c                   15.722(2)
_cell_measurement_reflns_used    8099
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.15
_cell_volume                     2914.4(8)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43858
_diffrn_reflns_theta_full        27.85
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    7.034
_exptl_absorpt_correction_T_max  0.3336
_exptl_absorpt_correction_T_min  0.1269
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.172
_refine_diff_density_min         -2.809
_refine_diff_density_rms         0.231
_refine_ls_extinction_coef       0.00133(11)
_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   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         13657
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0694P)^2^+5.8655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1263
_reflns_number_gt                10226
_reflns_number_total             13657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025572u_s1_3.cif
_cod_data_source_block           l
_cod_original_cell_volume        2914.4(7)
_cod_database_code               4318180