Synthesis, Structure, and Reactivity of Ruthenium Carboxylato and 2-Oxocarboxylato Complexes Bearing the Bis(3,5-dimethylpyrazol-1-yl)acetato Ligand
Stefan Tampier; Rainer Müller; Andrea Thorn; Eike Hübner; Nicolai Burzlaff; Inorganic Chemistry 47 (2008) 9624–9641; doi:10.1021/ic8000224

data_4305230
_publ_contact_author             'Burzlaff, Nicolai'
_publ_contact_author_email       burzlaff@chemie.uni-erlangen.de
_publ_section_title
;
Synthesis, Structure, and Reactivity of Ruthenium Carboxylato and
2-Oxocarboxylato Complexes Bearing the Bis(3,5-dimethylpyrazol-1-yl)acetato
Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9624
_journal_page_last               9641
_journal_paper_doi               10.1021/ic8000224
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'synthesis as decribed'
_chemical_formula_moiety         'C39 H40 N5 O5 P Ru, C H2 Cl2'
_chemical_formula_sum            'C40 H42 Cl2 N5 O5 P Ru'
_chemical_formula_weight         875.73
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2007-03-14T16:25:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                87.39(10)
_cell_angle_beta                 73.93(13)
_cell_angle_gamma                74.72(9)
_cell_formula_units_Z            2
_cell_length_a                   10.403(14)
_cell_length_b                   14.176(10)
_cell_length_c                   14.692(19)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      10.110
_cell_measurement_theta_min      6.126
_cell_measurement_wavelength     0.71073
_cell_volume                     2008(4)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.077449
_diffrn_orient_matrix_UB_12      -0.001455
_diffrn_orient_matrix_UB_13      0.028446
_diffrn_orient_matrix_UB_21      -0.028118
_diffrn_orient_matrix_UB_22      -0.050984
_diffrn_orient_matrix_UB_23      0.044631
_diffrn_orient_matrix_UB_31      0.063074
_diffrn_orient_matrix_UB_32      -0.052396
_diffrn_orient_matrix_UB_33      -0.047185
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9208
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         2.04
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.6011
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.263
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         8732
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.7429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                6925
_reflns_number_total             8732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8000224-file002_4.cif
_cod_data_source_block           complex8b
_cod_database_code               4305230