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_4344087
_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_moiety         'C168 H128 N8 O8 P8 Re4, 4(F6 P), 4.5(C4 H8 O)'
_chemical_formula_sum            'C186 H164 F24 N8 O12.5 P12 Re4'
_chemical_formula_weight         4283.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.3980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6709(4)
_cell_length_b                   32.5748(6)
_cell_length_c                   29.0674(5)
_cell_measurement_reflns_used    118091
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.11
_cell_volume                     18040.7(6)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'RAPID-AUTO (Rigaku, 1998)'
_computing_molecular_graphics    'Mercury (Macrae, 2008)'
_computing_publication_material  'SHELXL-2014/07 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'RIGAKU R-AXIS RAPID-II with VariMax007'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.1136
_diffrn_reflns_av_unetI/netI     0.1043
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            209965
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         3.107
_diffrn_source                   'sealed tube x-ray'
_exptl_absorpt_coefficient_mu    6.858
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ABSCOR,T.Higashi,RIGAKU
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       prism
_exptl_crystal_F_000             8528
_exptl_crystal_size_max          0.048
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.768
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2005
_refine_ls_number_reflns         32763
_refine_ls_number_restraints     773
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1767
_refine_ls_R_factor_gt           0.0882
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1566P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2348
_refine_ls_wR_factor_ref         0.2935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13685
_reflns_number_total             32763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01397_si_002.cif
_cod_data_source_block           R4ph
_cod_depositor_comments
'Adding full bibliography for 4344084--4344087.cif.'
_cod_original_formula_sum        'C186 H164 F24 N8 O12.50 P12 Re4'
_cod_database_code               4344087
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.734
_shelx_estimated_absorpt_t_max   0.904
_shelx_res_checksum              38975
_shelx_hkl_checksum              21349