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_7012394
_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         ' C19 H26 Cl1 N8 O1 Re1 S2 '
_chemical_formula_sum            'C19 H26 Cl N8 O Re S2'
_chemical_formula_weight         668.24
_chemical_melting_point          ?
_chemical_name_systematic
;                                                                          
?                                                                          
;
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 96.2545(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8385(5)
_cell_length_b                   8.5154(3)
_cell_length_c                   22.3598(8)
_cell_measurement_reflns_used    22649
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     2429.93(15)
_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 0.976
_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  0.060
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22649
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         5.12
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.311
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' dark brown '
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' fragment '
_exptl_crystal_F_000             1307.255
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.68
_refine_diff_density_min         -1.94
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0055
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3696
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.010940
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 4 parameters (Carruthers & Watkin , 1979) 
4.01    0.529     3.35    0.763    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0461
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                3696
_reflns_number_total             5728
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            b210540n.txt
_cod_data_source_block           CRYSTALS_2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
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        2429.9
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C19 H26 Cl1 N8 O1 Re1 S2 '
_cod_database_code               7012394