A new reactivity pattern of low-valent transition-metal hydroxo complexes: straightforward synthesis of hydrosulfido complexes via reaction with carbon disulfide
Gerbino, Darío C.; Hevia, Eva; Morales, Dolores; Clemente, M. Elena Navarro; Pérez, Julio; Riera, Lucía; Riera, Víctor; Miguel, Daniel; Chemical Communications (Cambridge, United Kingdom)  (2003) 328–329; doi:10.1039/b210860g

data_7113689
_publ_section_title
;
 A new reactivity pattern of low-valent transition-metal hydroxo
 complexes: straightforward synthesis of hydrosulfido complexes via
 reaction with carbon disulfide
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   3
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              328
_journal_page_last               329
_journal_paper_doi               10.1039/b210860g
_journal_year                    2003
_chemical_formula_sum            'C13 H9 N2 O3 Re S'
_chemical_formula_weight         459.48
_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                100.773(9)
_cell_angle_beta                 103.413(9)
_cell_angle_gamma                93.959(9)
_cell_formula_units_Z            2
_cell_length_a                   8.174(5)
_cell_length_b                   8.372(5)
_cell_length_c                   10.931(7)
_cell_measurement_temperature    299(2)
_cell_volume                     709.8(8)
_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      299(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3249
_diffrn_reflns_theta_full        23.62
_diffrn_reflns_theta_max         23.62
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    8.713
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.589750
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    2.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.420
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       0.0006(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0433P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                1861
_reflns_number_total             2051
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103951
_cod_data_source_file            b210860g.txt
_cod_data_source_block           Compound_4_(d3am)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7113689