Synthesis and Structural Characterization of Novel Re(I) Tricarbonyl Complexes Anchored on a Phosphinoarylbenzylamine and a Phosphinoaryloxazoline Generated in Situ
Torsten Kniess; João D. G. Correia; Ângela Domingos; Elisa Palma; Isabel Santos; Inorganic Chemistry 42 (2003) 6130–6135; doi:10.1021/ic034372v

data_4314245
_publ_section_title
;
 Synthesis and Structural Characterization of Novel Re(I) Tricarbonyl
 Complexes Anchored on a Phosphinoarylbenzylamine and a
 Phosphinoaryloxazoline Generated in Situ
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6130
_journal_page_last               6135
_journal_paper_doi               10.1021/ic034372v
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C24 H18 Br N O4 P Re'
_chemical_formula_sum            'C24 H18 Br N O4 P Re'
_chemical_formula_weight         681.47
_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                71.370(11)
_cell_angle_beta                 88.316(10)
_cell_angle_gamma                87.786(8)
_cell_formula_units_Z            4
_cell_length_a                   11.2502(11)
_cell_length_b                   14.7436(15)
_cell_length_c                   15.029(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.9
_cell_measurement_theta_min      7.9
_cell_volume                     2360.1(5)
_computing_cell_refinement       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_collection       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_reduction        process-MolEN(Fair,1990)
_computing_molecular_graphics    ORTEP-3(Farrugia,1997)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick,1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  CAD4-Enraf-Nonius
_diffrn_measurement_method       \w/2\qscans
_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    0.0547
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12195
_diffrn_reflns_theta_full        28.51
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.940
_exptl_absorpt_correction_T_max  0.9992
_exptl_absorpt_correction_T_min  0.2702
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.262
_refine_diff_density_min         -1.965
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         11785
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0621P)^2^+18.7305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1529
_reflns_number_gt                8258
_reflns_number_total             11785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034372vsi20030407_013301_2.cif
_cod_data_source_block           ks382
_cod_original_cell_volume        2360.0(5)
_cod_database_code               4314245