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_4318178
_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            'C27 H18 Cl F15 N5 O Re'
_chemical_formula_weight         935.11
_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                72.20(3)
_cell_angle_beta                 74.91(3)
_cell_angle_gamma                89.59(3)
_cell_formula_units_Z            2
_cell_length_a                   7.912(2)
_cell_length_b                   14.281(3)
_cell_length_c                   14.801(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.44
_cell_volume                     1532.6(7)
_computing_cell_refinement       'Siemens SAINT (V. 6.08b, BRUKER 1999)'
_computing_data_collection       'Siemens SMART (V.5.050, Siemens 1998)'
_computing_data_reduction        'Siemens SAINT (V. 6.08b, BRUKER 1999)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'STOE-Siemens-Huber four circle diffractometer'
_diffrn_measurement_method       'phi and omega 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  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11982
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.176
_exptl_absorpt_correction_T_max  0.6802
_exptl_absorpt_correction_T_min  0.4889
_exptl_absorpt_correction_type   semiempirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00208(19)
_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   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7583
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0189
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.8761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0482
_reflns_number_gt                7266
_reflns_number_total             7583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025572u_s1_1.cif
_cod_data_source_block           ast
_cod_original_cell_volume        1532.6(6)
_cod_database_code               4318178