Synthesis, structure and properties of [ReVL(O)Cl3], [ReVL(NR)Cl3], [ReIIIL(OPPh3)Cl3], and [ReIIIL(PPh3)Cl3] [L = 2-(arylazo)-1-methylimidazole, R = aryl] †
Chakraborty, Indranil; Bhattacharyya, Sibaprasad; Banerjee, Sangeeta; Kumar Dirghangi, Bimal; Chakravorty, Animesh; Journal of the Chemical Society, Dalton Transactions  (1999) 3747–; doi:10.1039/a906460e

data_7027761
_publ_section_title
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 Synthesis, structure and properties of [ReVL(O)Cl3], [ReVL(NR)Cl3],
 [ReIIIL(OPPh3)Cl3], and [ReIIIL(PPh3)Cl3]
 [L&#x2005;=&#x2005;2-(arylazo)-1-methylimidazole,
 R&#x2005;=&#x2005;aryl]&#x200A;&#x2020;
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_journal_issue                   21
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3747
_journal_paper_doi               10.1039/a906460e
_journal_year                    1999
_chemical_formula_sum            'C10 H10 Cl3 N4 O Re'
_chemical_formula_weight         494.77
_chemical_name_systematic
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 ? 
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_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Heavey atom method'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.41(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.231(7)
_cell_length_b                   7.716(3)
_cell_length_c                   13.409(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     1443.3(11)
_computing_cell_refinement       'Siemens p3'
_computing_data_collection       'Siemens p3'
_computing_data_reduction        'Siemens P3'
_computing_molecular_graphics    'Siemens SHELXTL V-5.03 (Sheldrick, 1994)'
_computing_publication_material  'Siemens SHELXTL V-5.03 (Sheldrick, 1994)'
_computing_structure_refinement  'Siemens SHELXTL V-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'Siemens SHELXTL V-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  '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  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2477
_diffrn_reflns_theta_max         24.93
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        nil
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    8.970
_exptl_absorpt_correction_T_max  0.129
_exptl_absorpt_correction_T_min  0.068
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    2.277
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.068
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.068
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_obs          0.0301
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0693
_refine_ls_wR_factor_obs         0.0637
_reflns_number_observed          1881
_reflns_number_total             2287
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            906460esup1.cif
_cod_data_source_block           '[ReL1(O)Cl3,2a'
_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^)+(0.0371P)^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^)+(0.0371P)^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_sg_symbol_H-M      P2(1)/c
_cod_database_code               7027761