Trinuclear and Tetranuclear Re(I) Rings Connected with Phenylene, Vinylene, and Ethynylene Chains: Synthesis, Photophysics, and Redox Properties.
Rohacova, Jana; Sekine, Akiko; Kawano, Tsubasa; Tamari, Sho; Ishitani, Osamu; Inorganic chemistry 54 (2015) 8769–8777; doi:10.1021/acs.inorgchem.5b01397

data_4344085
_publ_section_title
;
 Trinuclear and Tetranuclear Re(I) Rings Connected with Phenylene,
 Vinylene, and Ethynylene Chains: Synthesis, Photophysics, and Redox
 Properties.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8769
_journal_page_last               8777
_journal_paper_doi               10.1021/acs.inorgchem.5b01397
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C114 H88 F18 N6 O6 P9 Re3'
_chemical_formula_weight         2817.23
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   29.0902(5)
_cell_length_b                   29.0902(5)
_cell_length_c                   14.1738(3)
_cell_measurement_reflns_used    118987
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.231
_cell_measurement_theta_min      3.038
_cell_volume                     10387.5(3)
_computing_cell_refinement       'RAPID-AUTO  (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO  (Rigaku, 1998)'
_computing_data_reduction        'RAPID-AUTO  (Rigaku, 1998)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97(Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'RIGAKU R-AXIS RAPID-II with VariMax007'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.3023
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            118987
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.231
_diffrn_reflns_theta_min         3.038
_diffrn_source                   'sealed tube x-ray'
_exptl_absorpt_coefficient_mu    6.604
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ABSCOR,T.Higashi,RIGAKU
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       prism
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.076
_refine_diff_density_max         1.461
_refine_diff_density_min         -1.633
_refine_diff_density_rms         0.235
_refine_ls_abs_structure_details
;
 Flack x determined using 3829 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         12645
_refine_ls_number_restraints     287
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1672P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2252
_refine_ls_wR_factor_ref         0.2371
_reflns_Friedel_coverage         0.878
_reflns_friedel_fraction_full    0.997
_reflns_friedel_fraction_max     0.996
_reflns_number_gt                10026
_reflns_number_total             12645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01397_si_002.cif
_cod_data_source_block           R3vi
_cod_depositor_comments
'Adding full bibliography for 4344084--4344087.cif.'
_cod_original_cell_volume        10387.5(4)
_cod_database_code               4344085
_shelx_estimated_absorpt_t_min   0.412
_shelx_estimated_absorpt_t_max   0.634
_shelx_res_checksum              23192
_shelx_hkl_checksum              63910