Synthesis, structure and redox behaviour of facial [ReIIIL(PPh3)Cl3] and its stereoretentive conversion to [ReIVL′(PPh3)Cl3] via metal promoted aldimine → amide oxidation (L = pyridine-2-aldimine; L′ = pyridine-2-carboxamide)
Bhattacharyya, Sibaprasad; Banerjee, Sangeeta; Kumar Dirghangi, Bimal; Menon, Mahua; Chakravorty, Animesh; Journal of the Chemical Society, Dalton Transactions  (1999) 155–; doi:10.1039/a806346j

data_7027052
_publ_section_title
;
 Synthesis, structure and redox behaviour of facial [ReIIIL(PPh3)Cl3] and
 its stereoretentive conversion to [ReIVL&#x2032;(PPh3)Cl3] via metal
 promoted aldimine&#x2005;\\rightarrow &#x2005;amide oxidation
 (L&#x2005;=&#x2005;pyridine-2-aldimine;
 L&#x2032;&#x2005;=&#x2005;pyridine-2-carboxamide)
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              155
_journal_paper_doi               10.1039/a806346j
_journal_year                    1999
_chemical_formula_sum            'C30 H25 Cl3 N2 P Re'
_chemical_formula_weight         737.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     'Patterson Heavy Atom'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.66(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.505(6)
_cell_length_b                   13.545(5)
_cell_length_c                   18.720(11)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     2891(3)
_computing_cell_refinement       'Siemens SHELXTL-PLUS P3'
_computing_data_collection       'Siemens SHELXTL-PLUS P3'
_computing_data_reduction        'Siemens SHELXTL-PLUS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4105
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        nil
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.558
_exptl_absorpt_correction_T_max  0.3566
_exptl_absorpt_correction_T_min  0.1998
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Dark
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       Parallelopiped
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.072
_refine_ls_hydrogen_treatment    'Ridding Model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         3797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_restrained_S_obs      1.072
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_obs          0.0316
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0851
_refine_ls_wR_factor_obs         0.0680
_reflns_number_observed          3065
_reflns_number_total             3801
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            806346Jsup1.cif
_cod_data_source_block           fac-ReL1
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2891.2(25)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027052