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_4108576
_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            'C91 H64 F19.5 N6.5 O8 P7.25 Re3'
_chemical_formula_weight         2530.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.9802(1)
_cell_length_b                   24.9802(1)
_cell_length_c                   30.8551(2)
_cell_measurement_temperature    293(2)
_cell_volume                     19253.90(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            91690
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    3.978
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             9830
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.877
_refine_diff_density_min         -2.327
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         13226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1164P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1598
_reflns_number_gt                10990
_reflns_number_total             13226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8044579_si_003.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;

2021-04-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         5060.24
_cod_original_formula_units_Z            4
_cod_original_formula_sum        'C182 H128 F39 N13 O16 P14.50 Re6'
_cod_database_code               4108576