Syntheses, Structures, and Properties of Tricarbonyl (Chloro) Rhenium(I) Complexes with Redox-Active Tetrathiafulvalene−Pyrazole Ligands
Liu, Wei; Xiong, Jing; Wang, Yong; Zhou, Xin-Hui; Wang, Ru; Zuo, Jing-Lin; You, Xiao-Zeng; Organometallics 28 (2009) 755–; doi:10.1021/om800919u

data_4068537
_publ_section_title
;
 Syntheses, Structures, and Properties of Tricarbonyl (Chloro) Rhenium(I)
 Complexes with Redox-Active Tetrathiafulvalene&#x2212;Pyrazole Ligands
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              755
_journal_paper_doi               10.1021/om800919u
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C33 H34 Cl N4 O4 Re S16'
_chemical_formula_weight         1285.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 90.204(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.888(2)
_cell_length_b                   30.026(4)
_cell_length_c                   13.2625(17)
_cell_measurement_reflns_used    1465
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      2.8
_cell_volume                     6326.9(14)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0938
_diffrn_reflns_av_sigmaI/netI    0.0913
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31462
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    2.523
_exptl_absorpt_correction_T_max  0.6194
_exptl_absorpt_correction_T_min  0.5712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.166
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         11112
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0821
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1367P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2273
_refine_ls_wR_factor_ref         0.2473
_reflns_number_gt                6948
_reflns_number_total             11112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800919u_si_002.cif
_cod_data_source_block           5d
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4068537