Chemistry of the Rhenium-Azopyridine Family: An Oxo Parent and Derivatives Thereof Including a Novel Oxo-Imido Dimer
Sangeeta Banerjee; Sibaprasad Bhattacharyya; Bimal Kumar Dirghangi; Mahua Menon; Animesh Chakravorty; Inorganic Chemistry 39 (2000) 6–13; doi:10.1021/ic990465u

data_4300031
_publ_section_title
;
Chemistry of the Rhenium-Azopyridine Family: An Oxo Parent and
Derivatives Thereof Including a Novel Oxo-Imido Dimer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6
_journal_page_last               13
_journal_paper_doi               10.1021/ic990465u
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C17 H12 Cl5 N4 Re'
_chemical_formula_weight         635.76
_space_group_IT_number           2
_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                63.67(2)
_cell_angle_beta                 71.24(2)
_cell_angle_gamma                86.79(2)
_cell_formula_units_Z            2
_cell_length_a                   9.683(3)
_cell_length_b                   10.898(3)
_cell_length_c                   11.522(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      7
_cell_volume                     1026.4(6)
_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 using XP'
_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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5032
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.09
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.580
_exptl_absorpt_correction_T_max  0.583
_exptl_absorpt_correction_T_min  0.272
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    2.057
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.411
_refine_diff_density_min         -1.996
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       0.0091(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_obs          0.0339
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+0.4548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0812
_refine_ls_wR_factor_obs         0.0765
_reflns_number_observed          4118
_reflns_number_total             4749
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+0.4548P] 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^)+(0.0489P)^2^+0.4548P] 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:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.5 from 2014-11-21.

'_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        1026.4(5)
_cod_database_code               4300031