Systematic Synthesis, Isolation, and Photophysical Properties of Linear-Shaped Re(I) Oligomers and Polymers with 2-20 Units
Youhei Yamamoto; Shuhei Sawa; Yusuke Funada; Tatsuki Morimoto; Magnus Falkenström; Hiroshi Miyasaka; Sayaka Shishido; Tomoji Ozeki; Kazuhide Koike; Osamu Ishitani; Journal of the American Chemical Society 130 (2008) 14659–14674; doi:10.1021/ja8044579

data_4108578
_publ_section_title
;
 Systematic Synthesis, Isolation, and Photophysical Properties of
 Linear-Shaped Re(I) Oligomers and Polymers with 2-20 Units
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14659
_journal_page_last               14674
_journal_paper_doi               10.1021/ja8044579
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C128 H104 F24 N8 O10 P10 Re4'
_chemical_formula_weight         3424.74
_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                78.1431(14)
_cell_angle_beta                 85.046(2)
_cell_angle_gamma                83.545(5)
_cell_formula_units_Z            2
_cell_length_a                   15.8437(7)
_cell_length_b                   16.8427(5)
_cell_length_c                   25.4088(10)
_cell_measurement_reflns_used    18085
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.5754
_cell_measurement_theta_min      1.6435
_cell_volume                     6579.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 14.8068
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phio scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0840
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40705
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    3.883
_exptl_absorpt_correction_T_max  0.8923
_exptl_absorpt_correction_T_min  0.6122
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.010
_refine_diff_density_min         -1.540
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1657
_refine_ls_number_reflns         24255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0992P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1559
_reflns_number_gt                17996
_reflns_number_total             24255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8044579_si_005.cif
_cod_data_source_block           l4e2
_cod_database_code               4108578