A rhenium(V)‒arylimide species incorporating pyridine-2-aldimine chelation
Banerjee, Sangeeta; Bhattacharyya, Sibaprasad; Chakraborty, Indranil; Dirghangi, Bimal Kumar; Acta Crystallographica Section C 55 (1999) 2000–2002; doi:10.1107/S0108270199010732

data_2009250
_publ_section_title
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 A rhenium(V)--arylimide species incorporating pyridine-2-aldimine
 chelation
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2000
_journal_page_last               2002
_journal_paper_doi               10.1107/S0108270199010732
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Re (C6 H6 N2) Cl3 (C12 H9 Cl1 N2)]'
_chemical_formula_sum            'C18 H15 Cl4 N4 Re'
_chemical_formula_weight         615.34
_chemical_melting_point          548.1(10)
_chemical_name_systematic
;
Trichloro((p-aminophenyl)imido)(N-pchloro-pyridine-2-aldimine)rhenium(V).
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                110.23(7)
_cell_angle_beta                 92.65(7)
_cell_angle_gamma                103.34(7)
_cell_formula_units_Z            2
_cell_length_a                   8.533(8)
_cell_length_b                   10.643(8)
_cell_length_c                   12.287(12)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     1009.0(17)
_computing_cell_refinement       SHELXTL-Plus90
_computing_data_collection       'SHELXTL-Plus90 (Sheldrick, 1990)'
_computing_data_reduction        SHELXTL-Plus90
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  SHELXTL/PC
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       \w
_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  0.020
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3924
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.562
_exptl_absorpt_correction_T_max  0.194
_exptl_absorpt_correction_T_min  0.096
_exptl_absorpt_correction_type   '\y scan (North et al., 1968)'
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.04
_refine_diff_density_min         -1.50
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.077
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.030
_refine_ls_R_factor_gt           0.026
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0416P)^2^+0.4494P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.067
_refine_ls_wR_factor_ref         0.061
_reflns_number_gt                3307
_reflns_number_total             3586
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            de1115.cif
_cod_data_source_block           601re
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '274--276 C' was changed to
'548.1(10)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

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

The following automatic conversions were performed:

'_chemical_melting_point' value '274--276 C' was changed to
'548.1(10)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0416P)^2^+0.4494P] 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^)+(0.0416P)^2^+0.4494P] 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        1009.0(16)
_cod_database_code               2009250