Synthesis of Heteroleptic Bis(diimine)carbonylchlororuthenium(II) Complexes from Photodecarbonylated Precursors
Christopher M. Kepert; Glen B. Deacon; Norma Sahely; Leone Spiccia; Gary D. Fallon; Brian W. Skelton; Allan H. White; Inorganic Chemistry 43 (2004) 2818–2827; doi:10.1021/ic0351895

data_4310911
_publ_contact_author_address
;
   Department of Chemistry
   University of Western Australia
   Crawley  
   Western Australia 6009
   Australia
;
_publ_contact_author_email       bws@crystal.uwa.edu.au
_publ_contact_author_fax         (+61)_08_9380_1118
_publ_contact_author_name        'Skelton, B. W.'
_publ_contact_author_phone       (+61)_08-9380_3481
_publ_section_title
;
 Synthesis of Heteroleptic Bis(diimine)carbonylchlororuthenium(II)
 Complexes from Photodecarbonylated Precursors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2818
_journal_page_last               2827
_journal_paper_doi               10.1021/ic0351895
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C23 H21 Cl2 N5 O5 Ru'
_chemical_formula_weight         619.43
_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'
_cell_angle_alpha                90.00000
_cell_angle_beta                 109.26(2)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   13.828(4)
_cell_length_b                   12.515(2)
_cell_length_c                   15.501(4)
_cell_measurement_reflns_used    8
_cell_measurement_temperature    293
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      19.5
_cell_volume                     2532.4(11)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal DIFDAT ABSORB SORTRF ADDREF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      293
_diffrn_measurement_device_type
;
      CAD4 diffractometer
;
_diffrn_measurement_method       '2\q-\w scans'
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .043
_diffrn_reflns_av_sigmaI/netI    .042
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6283
_diffrn_reflns_reduction_process 'perpendicular monochr Lp'
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         8
_exptl_absorpt_coefficient_mu    0.87
_exptl_absorpt_correction_T_max  .737
_exptl_absorpt_correction_T_min  .670
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 XTAL absorb               
;
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.25
_refine_diff_density_max         .751
_refine_diff_density_min         -.836
_refine_ls_extinction_coef       717(205)
_refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970'
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     339
_refine_ls_number_reflns         3770
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .056
_refine_ls_R_factor_gt           .047
_refine_ls_shift/su_max          .054
_refine_ls_shift/su_mean         .003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .052
_refine_ls_wR_factor_ref         .05
_reflns_d_resolution_high        .842
_reflns_d_resolution_low         13.054
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              -18
_reflns_number_gt                3823
_reflns_number_total             4433
_reflns_threshold_expression     'I    > 2.00 sig(I   )'
_cod_data_source_file            ic0351895si20040210_044127_7.cif
_cod_data_source_block           ck461b
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_original_formula_sum        'C23 H21 Cl2 N5 O5 Ru1'
_cod_database_code               4310911