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_4305228
_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 described'
_chemical_formula_moiety         'C34 H36 N5 O4 P1 Ru1, 2 (C H2 Cl2)'
_chemical_formula_sum            'C36 H40 Cl4 N5 O4 P Ru'
_chemical_formula_weight         880.57
_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             2007-03-01T14:23:59-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                88.22(4)
_cell_angle_beta                 75.73(7)
_cell_angle_gamma                85.50(4)
_cell_formula_units_Z            2
_cell_length_a                   9.792(4)
_cell_length_b                   12.224(5)
_cell_length_c                   16.944(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      14.144
_cell_measurement_theta_min      11.299
_cell_measurement_wavelength     0.71073
_cell_volume                     1959.4(15)
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.037731
_diffrn_orient_matrix_UB_12      0.075554
_diffrn_orient_matrix_UB_13      -0.011532
_diffrn_orient_matrix_UB_21      -0.083003
_diffrn_orient_matrix_UB_22      -0.006846
_diffrn_orient_matrix_UB_23      0.047569
_diffrn_orient_matrix_UB_31      0.053391
_diffrn_orient_matrix_UB_32      0.031209
_diffrn_orient_matrix_UB_33      0.036179
_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
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9271
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.24
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        7
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_T_max  0.8399
_exptl_absorpt_correction_T_min  0.5624
_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    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.23
_refine_diff_density_max         2.343
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8965
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1937
_refine_ls_wR_factor_ref         0.2088
_reflns_number_gt                6605
_reflns_number_total             8965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8000224-file002_2.cif
_cod_data_source_block           complex5a
_cod_original_cell_volume        1959.3(13)
_cod_database_code               4305228