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_4108575
_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            'C52 H36 F12 N4 O6 P4 Re2'
_chemical_formula_weight         1537.13
_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                94.00(2)
_cell_angle_beta                 94.03(2)
_cell_angle_gamma                103.22(2)
_cell_formula_units_Z            1
_cell_length_a                   11.927(3)
_cell_length_b                   12.952(3)
_cell_length_c                   9.752(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      16.8
_cell_measurement_theta_min      15.0
_cell_volume                     1457.2(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8155
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.348
_exptl_absorpt_correction_T_max  0.4768
_exptl_absorpt_correction_T_min  0.4768
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.675
_refine_diff_density_min         -2.132
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+4.2700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                6399
_reflns_number_total             6705
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8044579_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        1457.1(6)
_cod_database_code               4108575