Synthesis, structural characterization and catalytic properties of a novel monomeric rhenium(V)methyl(oxo)bis(η2-picolinato) complex: [CH3Re(O)(pic)2] †
Deloffre, Alexis; Halut, Sabine; Salles, Laurent; Brégeault, Jean-Marie; Gregorio, José Ribeiro; Denise, Bernard; Rudler, Henri; Journal of the Chemical Society, Dalton Transactions  (1999) 2897–; doi:10.1039/a904952e

data_7027623
_publ_section_title
;
 Synthesis, structural characterization and catalytic properties of a
 novel monomeric rhenium(V)methyl(oxo)bis(\h2-picolinato) complex:
 [CH3Re(O)(pic)2]&#x200A;&#x2020;
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2897
_journal_paper_doi               10.1039/a904952e
_journal_year                    1999
_chemical_formula_moiety         ' C13 H11 Re1 O5 N2 '
_chemical_formula_sum            'C13 H11 N2 O5 Re'
_chemical_formula_weight         461.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             99-02-01
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90
_cell_angle_beta                 111.75(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.339(7)
_cell_length_b                   7.070(3)
_cell_length_c                   15.124(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      14.5
_cell_measurement_theta_min      14
_cell_volume                     2814.5(15)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       '  Enraf-nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.06
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2835
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  ' one hour '
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    8.77
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            ' green '
_exptl_crystal_density_diffrn    2.18
_exptl_crystal_description       ' parallelepiped '
_exptl_crystal_F_000             1731.22
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.03
_refine_diff_density_min         -1.07
_refine_ls_extinction_coef       43.
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.0467
_refine_ls_hydrogen_treatment
;
 H atoms placed geometrically after each cycle
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2072
_refine_ls_R_factor_obs          0.0320
_refine_ls_shift/esd_max         0.032062
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_wR_factor_obs         0.0392
_reflns_limit_h_max              31
_reflns_limit_h_min              -33
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_observed          2072
_reflns_number_total             2607
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            904952esup1.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-08-09

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Psiscan ' changed to
'psi-scan' 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 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct_Methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2814(2)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        ' C13 H11 Re1 O5 N2 '
_cod_database_code               7027623