Rhenium Chemistry of Diazabutadienes and Derived Iminoacetamides Spanning the Valence Domain II-VI. Synthesis, Characterization, and Metal-Promoted Regiospecific Imine Oxidation
Samir Das; Indranil Chakraborty; Animesh Chakravorty; Inorganic Chemistry 42 (2003) 6545–6555; doi:10.1021/ic034586c

data_4314376
_publ_section_title
;
 Rhenium Chemistry of Diazabutadienes and Derived Iminoacetamides Spanning
 the Valence Domain II-VI. Synthesis, Characterization, and Metal-Promoted
 Regiospecific Imine Oxidation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6545
_journal_page_last               6555
_journal_paper_doi               10.1021/ic034586c
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C22 H31 Cl4 N3 O Re'
_chemical_formula_weight         681.50
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.99(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.257(2)
_cell_length_b                   12.922(3)
_cell_length_c                   18.295(4)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     2570.7(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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       'CCD area detector'
_diffrn_measurement_method       'phi and \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  0.0208
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_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
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_diffrn_reflns_theta_max         27.74
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    5.162
_exptl_absorpt_correction_T_max  0.206
_exptl_absorpt_correction_T_min  0.119
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
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_refine_diff_density_max         1.609
_refine_diff_density_min         -0.567
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_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+3.0804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0770
_refine_ls_wR_factor_obs         0.0703
_reflns_number_observed          4568
_reflns_number_total             5624
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic034586csi20030819_123709_3.cif
_cod_data_source_block           rea1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+3.0804P] 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^)+(0.0363P)^2^+3.0804P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

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_original_cell_volume        2570.8(9)
_cod_database_code               4314376