Microwave-Assisted Synthesis of Functionalized Shvo-Type Complexes
Cesari, Cristiana; Sambri, Letizia; Zacchini, Stefano; Zanotti, Valerio; Mazzoni, Rita; Organometallics 33 (2014) 2814–; doi:10.1021/om500335m

data_4083408
_publ_section_title
;
 Microwave-Assisted Synthesis of Functionalized Shvo-Type Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2814
_journal_paper_doi               10.1021/om500335m
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C67 H52 Cl2 O10 Ru2'
_chemical_formula_weight         1290.13
_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-97
_cell_angle_alpha                118.895(3)
_cell_angle_beta                 97.620(3)
_cell_angle_gamma                101.411(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5361(19)
_cell_length_b                   17.408(3)
_cell_length_c                   17.936(5)
_cell_measurement_reflns_used    3435
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.921
_cell_measurement_theta_min      2.246
_cell_volume                     2979.9(11)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0942
_diffrn_reflns_av_sigmaI/netI    0.1363
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28343
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.9255
_exptl_absorpt_correction_T_min  0.8856
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.0786 (selected reflections only, before parameter refinement)
 R(int) =  0.0530 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         10500
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1693
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1056P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.2177
_reflns_number_gt                5006
_reflns_number_total             10500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500335m_si_001.cif
_cod_data_source_block           4b
_cod_depositor_comments
'Adding full bibliography for 4083408--4083409.cif.'
_cod_original_cell_volume        2979.9(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4083408