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_4332914
_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            'C56 H46 N9 O12 Re3 S3'
_chemical_formula_weight         1691.80
_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                 104.497(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2386(11)
_cell_length_b                   13.0484(8)
_cell_length_c                   27.6698(17)
_cell_measurement_temperature    293(2)
_cell_volume                     6025.8(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0904
_diffrn_reflns_av_sigmaI/netI    0.2927
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            32147
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    6.182
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.888868
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.691
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         13329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.691
_refine_ls_R_factor_all          0.2007
_refine_ls_R_factor_gt           0.0446
_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 w=1/[\s^2^(Fo^2^)+(0.0110P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0801
_reflns_number_gt                4470
_reflns_number_total             13329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061080wsup1.cif
_cod_data_source_block           1c.2C7H8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        6025.8(6)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4332914