Synthesis and characterisation of new homoleptic rhenium thiosemicarbazone complexes
Cowley, Andrew R.; Dilworth, Jonathan R.; Donnelly, Paul S.; Woollard-Shore, John; Dalton Transactions  (2003) 748–; doi:10.1039/b210540n

data_7012395
_publ_section_title
;
 Synthesis and characterisation of new homoleptic rhenium
 thiosemicarbazone complexes
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              748
_journal_paper_doi               10.1039/b210540n
_journal_year                    2003
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C21 H30 Cl1 N8 O1 Re1 S2 '
_chemical_formula_sum            'C21 H30 Cl N8 O Re S2'
_chemical_formula_weight         696.32
_chemical_melting_point          ?
_chemical_name_systematic
;                                                                          
?                                                                          
;
_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     direct
_cell_angle_alpha                96.4542(11)
_cell_angle_beta                 93.2383(11)
_cell_angle_gamma                103.1595(9)
_cell_formula_units_Z            2
_cell_length_a                   8.8775(2)
_cell_length_b                   11.9729(2)
_cell_length_c                   12.6197(3)
_cell_measurement_reflns_used    21583
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     1293.16(5)
_computing_cell_refinement
;                                                                          
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)                       
;
_computing_data_collection
;                                                                          
KappaCCD software 'Collect' (Nonius, 2000)                                 
;
_computing_data_reduction
;                                                                          
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)                       
;
_computing_publication_material
;                                                                          
CRYSTALS (Watkin et al, 2001)                                              
;
_computing_structure_refinement
;                                                                          
CRYSTALS (Watkin et al, 2001)                                              
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;                                                                          
Nonius KappaCCD                                                            
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21583
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         5.10
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.989
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' dark brown '
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             685.624
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.10
_refine_diff_density_min         -1.65
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9856
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5177
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.019954
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979) 
2.39    -.476     1.36    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0316
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                5177
_reflns_number_total             5857
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            b210540n.txt
_cod_data_source_block           CRYSTALS_3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic ' changed to 'triclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        1293.2
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C21 H30 Cl1 N8 O1 Re1 S2 '
_cod_database_code               7012395