Synthesis and characterization of ruthenium(ii) complexes with the new ligand 2-phenylazopyridine-5-sulfonic acid (Hsazpy): in search for new anticancer agents
Hotze, Anna C. G.; Kooijman, Huub; Spek, Anthony L.; Haasnoot, Jaap G.; Reedijk, Jan; New Journal of Chemistry 28 (2004) 565–; doi:10.1039/b313746e

data_7050246
_publ_section_title
;
 Synthesis and characterization of ruthenium(ii) complexes with the new
 ligand 2-phenylazopyridine-5-sulfonic acid (Hsazpy): in search for new
 anticancer agents
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              565
_journal_paper_doi               10.1039/b313746e
_journal_volume                  28
_journal_year                    2004
_chemical_absolute_configuration ad
_chemical_compound_source        'see text'
_chemical_formula_moiety
'C22 H16 Cl2 N6 O6 Ru S2, 2(C8 H20 N), 2(H2 O)'
_chemical_formula_sum            'C38 H60 Cl2 N8 O8 Ru S2'
_chemical_formula_weight         993.05
_chemical_name_systematic        ' ?'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90.81(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3614(12)
_cell_length_b                   9.8737(12)
_cell_length_c                   24.449(4)
_cell_measurement_reflns_used    1108
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     2259.6(5)
_computing_cell_refinement       'Denzo (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2002)'
_computing_publication_material  'PLATON (Spek, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 18.4
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius Kappa CCD area detector'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20733
_diffrn_reflns_reduction_process ' ?'
_diffrn_reflns_theta_full        25.26
_diffrn_reflns_theta_max         25.26
_diffrn_reflns_theta_min         1.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.357
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
The crystal is both a racemic AND a pseudo-merohedral twin (2-rotation
around a), see _refine_special_details. The Flack parameter is
indirectly incorporated in the 4-component twin model. The value
reported in _refine_ls_abs_structure_Flack is therefore meaningless.
;
_refine_ls_abs_structure_Flack   0.0
_refine_ls_extinction_method     'none             '
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         8023
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(F~o~^2^)+(0.0010P)^2^+14.0P] where P=(F~o~^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                7131
_reflns_number_total             8023
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b313746e.txt
_cod_data_source_block           1
_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 2.4.1 from
2010-06-29.

'_atom_sites_solution_hydrogens' value 'geom ' changed to
'geom' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_sites_solution_primary' value 'direct ' changed to
'direct' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_sites_solution_secondary' value 'difmap ' changed to
'difmap' according to '/home/saulius/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 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7050246