Pyridylazole Chelation of Oxorhenium(V) and Imidorhenium(V). Rates and Trends of Oxygen Atom Transfer from ReVO to Tertiary Phosphines
Jaydip Gangopadhyay; Suman Sengupta; Sibaprasad Bhattacharyya; Indranil Chakraborty; Animesh Chakravorty; Inorganic Chemistry 41 (2002) 2616–2622; doi:10.1021/ic011064t

data_4317926
_publ_section_title
;
 Pyridylazole Chelation of Oxorhenium(V) and Imidorhenium(V). Rates and
 Trends of Oxygen Atom Transfer from ReVO to Tertiary Phosphines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2616
_journal_page_last               2622
_journal_paper_doi               10.1021/ic011064t
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C30 H23 Cl3 N2 O P Re S'
_chemical_formula_weight         783.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                91.08(4)
_cell_angle_beta                 89.92(5)
_cell_angle_gamma                106.98(5)
_cell_formula_units_Z            2
_cell_length_a                   10.369(8)
_cell_length_b                   11.459(6)
_cell_length_c                   13.787(5)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7
_cell_volume                     1566.4(16)
_computing_cell_refinement       'Siemens P3/P4-PC V4.27'
_computing_data_collection       'Siemens P3/P4-PC V4.27'
_computing_data_reduction        'Siemens P3/P4-PC V4.27'
_computing_molecular_graphics    'Siemens SHELXTL V5.03 PC'
_computing_publication_material  'Siemens SHELXTL V5.03 PC'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       '\w 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4361
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.278
_exptl_absorpt_correction_T_max  0.211
_exptl_absorpt_correction_T_min  0.146
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            dark_violet
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       parallelopied
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         4.845
_refine_diff_density_min         -4.040
_refine_diff_density_rms         0.440
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.670
_refine_ls_goodness_of_fit_obs   2.447
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         4355
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      2.718
_refine_ls_restrained_S_obs      2.446
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_obs          0.1070
_refine_ls_shift/esd_max         0.856
_refine_ls_shift/esd_mean        0.144
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc 
 [0.00000+1.00000exp(10.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+43.1625*P+(0.2487P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_wR_factor_all         0.3036
_refine_ls_wR_factor_obs         0.2526
_reflns_number_observed          3701
_reflns_number_total             4361
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic011064t_3.cif
_cod_data_source_block           sj6[Re(OPPh3)Cl3(pbt)]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Heavy atom method' was changed
to 'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4317926