Chemical Control on the Coordination Mode of Benzaldehyde Semicarbazone Ligands. Synthesis, Structure, and Redox Properties of Ruthenium Complexes
Falguni Basuli; Shie-Ming Peng; Samaresh Bhattacharya; Inorganic Chemistry 40 (2001) 1126–1133; doi:10.1021/ic000915e

data_4319362
_publ_section_title
;
 Chemical Control on the Coordination Mode of Benzaldehyde Semicarbazone
 Ligands. Synthesis, Structure, and Redox Properties of Ruthenium
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1126
_journal_page_last               1133
_journal_paper_doi               10.1021/ic000915e
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C50 H42.5 Cl2 N4 O4 P2 Ru'
_chemical_formula_weight         997.29
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                74.937(1)
_cell_angle_beta                 67.473(1)
_cell_angle_gamma                80.209(1)
_cell_formula_units_Z            4
_cell_length_a                   16.9298(2)
_cell_length_b                   17.6296(2)
_cell_length_c                   17.9285(1)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    295(2)
_cell_volume                     4757.99(9)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0668
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51412
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.20
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.9280
_exptl_absorpt_correction_T_min  0.8263
_exptl_absorpt_correction_type   ' empirical used sadabs'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2042
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.0026(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.048
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1077
_refine_ls_number_reflns         18802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_obs          0.0647
_refine_ls_shift/esd_max         0.020
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0882P)^2^+5.5635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1749
_refine_ls_wR_factor_obs         0.1538
_reflns_number_observed          13570
_reflns_number_total             18802
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000915e_3.cif
_cod_data_source_block           ic6832
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0882P)^2^+5.5635P] 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^)+(0.0882P)^2^+5.5635P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4758.00(8)
_cod_original_formula_sum        'C50 H42.50 Cl2 N4 O4 P2 Ru'
_cod_database_code               4319362