Synthesis of a Ruthenium(II) Complex Containing an [11]ane-P2CNHC(NHC = Imidazolidin-2-ylidene) Macrocycle
Flores-Figueroa, Aarón; Kaufhold, Oliver; Hepp, Alexander; Fröhlich, Roland; Hahn, F. Ekkehardt; Organometallics 28 (2009) 6362–; doi:10.1021/om900703q

data_4070308
_publ_section_title
;
 Synthesis of a Ruthenium(II) Complex Containing an [11]ane-P2CNHC(NHC =
 Imidazolidin-2-ylidene) Macrocycle
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6362
_journal_paper_doi               10.1021/om900703q
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C39 H32 Cl3 F2 N2 O0.5 P2 Ru'
_chemical_formula_weight         844.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   'at O from difmap, others geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.580(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.0186(5)
_cell_length_b                   22.1164(7)
_cell_length_c                   18.4397(7)
_cell_measurement_reflns_used    6697
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     7782.7(4)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       -21
_diffrn_reflns_limit_l_min       21
_diffrn_reflns_number            30449
_diffrn_reflns_theta_full        67.88
_diffrn_reflns_theta_max         67.88
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    6.270
_exptl_absorpt_correction_T_max  0.6339
_exptl_absorpt_correction_T_min  0.3669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3416
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;

;
_refine_diff_density_max         1.087
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0886P)^2^+23.6823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1532
_reflns_number_gt                5711
_reflns_number_total             6859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900703q_si_002.cif
_cod_data_source_block           han-complex-1
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C39 H32 Cl3 F2 N2 O0.50 P2 Ru'
_cod_database_code               4070308