Synthesis and Characterization of New Trimeric Rhenium(I) Complexes. The Influence of Steric Factors on the Size of Pyrazolonaterhenium(I) Metallomacrocycles
Barbazán, Paula; Carballo, Rosa; Casas, José S.; García-Martínez, Emilia; Pereiras-Gabián, Gumersindo; Sánchez, Agustín; Vázquez-López, Ezequiel M.; Inorganic Chemistry 45 (2006) 7323–7330; doi:10.1021/ic061080w

data_4332915
_publ_section_title
;
 Synthesis and Characterization of New Trimeric Rhenium(I) Complexes. The
 Influence of Steric Factors on the Size of Pyrazolonaterhenium(I)
 Metallomacrocycles
;
_journal_issue                   18
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7323
_journal_page_last               7330
_journal_paper_doi               10.1021/ic061080w
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C42 H30 N9 O12 Re3 S3'
_chemical_formula_weight         1507.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.146(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0752(15)
_cell_length_b                   16.8519(13)
_cell_length_c                   19.3670(15)
_cell_measurement_temperature    293(2)
_cell_volume                     5766.3(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.924
_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  0.1038
_diffrn_reflns_av_sigmaI/netI    0.2340
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31573
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    6.449
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2856
_refine_diff_density_max         1.851
_refine_diff_density_min         -1.698
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         12926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.852
_refine_ls_R_factor_all          0.1714
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0582P)^2^+0.0000sin\q/\l] 
 where P = 0.33300Fo^2^ + 0.66700Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1591
_reflns_number_gt                5210
_reflns_number_total             12926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061080wsup1.cif
_cod_data_source_block           1c
_cod_database_code               4332915