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_4300030
_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            'C29 H23 Cl4 N3 O P Re'
_chemical_formula_weight         788.47
_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                 94.21(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.264(7)
_cell_length_b                   15.221(9)
_cell_length_c                   17.628(9)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     3014(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 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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0908
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4237
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         1.77
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.467
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.5373
_exptl_absorpt_correction_type   'Semi empirical'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.856
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.100
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         3960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_restrained_S_obs      1.100
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_obs          0.0616
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0865P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1666
_refine_ls_wR_factor_obs         0.1355
_reflns_number_observed          2648
_reflns_number_total             3962
_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^)+(0.0865P)^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^)+(0.0865P)^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 

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 2.4.5 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        3014.2(20)
_cod_database_code               4300030