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_4068536
_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            'C31 H32 Cl N4 O5 Re S16'
_chemical_formula_weight         1275.22
_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                78.393(4)
_cell_angle_beta                 78.397(4)
_cell_angle_gamma                72.951(4)
_cell_formula_units_Z            4
_cell_length_a                   14.886(3)
_cell_length_b                   15.115(3)
_cell_length_c                   24.448(5)
_cell_measurement_reflns_used    1563
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      1.8
_cell_volume                     5091.9(18)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.1086
_diffrn_reflns_av_sigmaI/netI    0.3235
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            24302
_diffrn_reflns_theta_full        24.50
_diffrn_reflns_theta_max         24.50
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    3.135
_exptl_absorpt_correction_T_max  0.5873
_exptl_absorpt_correction_T_min  0.5589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.658
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1057
_refine_ls_number_reflns         16692
_refine_ls_number_restraints     743
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.2184
_refine_ls_R_factor_gt           0.0744
_refine_ls_shift/su_max          0.092
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1798
_reflns_number_gt                5031
_reflns_number_total             16692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800919u_si_002.cif
_cod_data_source_block           5c
_cod_original_cell_volume        5091.9(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068536