Electrosynthesis of binuclear ruthenium complexes from [RuCl3(dppb)(L)] precursors [L = pyridine, 4-methylpyridine or dimethyl sulfoxide; dppb = 1,4-bis(diphenylphosphino)butane]
Wohnrath, Karen; de Araujo, Márcio Peres; Dinelli, Luis Rogério; Batista, Alzir Azevedo; de Sousa Moreira, Icaro; Castellano, Eduardo Ernesto; Ellena, Javier; Journal of the Chemical Society, Dalton Transactions  (2000) 3383–; doi:10.1039/b001422m

data_7009500
_publ_section_title
;
 Electrosynthesis of binuclear ruthenium complexes from
 [RuCl3(dppb)(L)] precursors [L&#x2005;=&#x2005;pyridine,
 4-methylpyridine or dimethyl sulfoxide;
 dppb&#x2005;=&#x2005;1,4-bis(diphenylphosphino)butane]
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3383
_journal_paper_doi               10.1039/b001422m
_journal_year                    2000
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C34 H34.5 Cl3 N P2 Ru 0.5(CH2Cl2)'
_chemical_formula_structural     'C34.50 H35.50 Cl4 N P2 Ru'
_chemical_formula_sum            'C34.5 H35.5 Cl4 N P2 Ru'
_chemical_formula_weight         768.95
_chemical_melting_point          476(1)
_chemical_name_systematic
;
Trans-1,4bis(diphenylphosphine)-4-methylpyridinetrichlororuthenium(III)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             1999-07-02T15:57:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.785(10)
_cell_length_b                   17.559(5)
_cell_length_c                   27.448(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      14
_cell_measurement_wavelength     1.541838
_cell_volume                     7126(5)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1992)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1992)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_sigmaI/netI    0.226
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            6567
_diffrn_reflns_theta_max         70
_diffrn_reflns_theta_min         3.22
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  30
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    7.356
_exptl_absorpt_correction_T_max  0.7599
_exptl_absorpt_correction_T_min  0.4755
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             3132
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.174999
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.189
_refine_ls_goodness_of_fit_gt    1.619
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6191
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.191
_refine_ls_restrained_S_obs      1.619
_refine_ls_R_factor_all          0.2352
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          -0.084
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w==1/[\s^2^(Fo^2^)+(0.0350P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1589
_refine_ls_wR_factor_gt          0.1228
_reflns_number_gt                2213
_reflns_number_total             6194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001422m.txt
_cod_data_source_block           s93
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w==1/[\s^2^(Fo^2^)+(0.0350P)^2^+4.0000P] 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^)+(0.0350P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C34.50 H35.50 Cl4 N P2 Ru'
_cod_database_code               7009500
_exptl_absorpt_correction_t_ave  0.6792
_diffrn_standards_decay_corr_max 1.108
_diffrn_standards_decay_corr_min 0.92