New Ruthenium(II) Complexes with Enantiomerically Pure Bis- and Tris(pinene)-Fused Tridentate Ligands. Synthesis, Characterization and Stereoisomeric Analysis
Xavier Sala; Albert Poater; Alexander von Zelewsky; Teodor Parella; Xavier Fontrodona; Isabel Romero; Miquel Solà; Montserrat Rodríguez; Antoni Llobet; Inorganic Chemistry 47 (2008) 8016–8024; doi:10.1021/ic800252f

data_4305292
_publ_contact_author_address
;Departament de Quimica
Universitat de Girona
campus de Montilivi
E-17071 Girona
;
_publ_contact_author_email       montse.rodriguez@udg.edu
_publ_contact_author_name        'Montserrat Rodriguez'
_publ_contact_author_phone       '0034 972 41 8333'
_publ_section_title
;
New Ruthenium(II) Complexes with Enantiomerically Pure Bis- and
Tris(pinene)-Fused Tridentate Ligands. Synthesis, Characterization and
Stereoisomeric Analysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8016
_journal_page_last               8024
_journal_paper_doi               10.1021/ic800252f
_journal_volume                  47
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C54 H61 Cl N3 P2 Ru, C4 H10 O, B F4'
_chemical_formula_sum            'C58 H71 B Cl F4 N3 O P2 Ru'
_chemical_formula_weight         1111.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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                63.165(3)
_cell_angle_beta                 87.923(3)
_cell_angle_gamma                87.683(3)
_cell_formula_units_Z            1
_cell_length_a                   10.695(2)
_cell_length_b                   11.316(2)
_cell_length_c                   12.455(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1343.7(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker Shelxtl'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.970
_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  0.0143
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20557
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.027(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         12340
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+1.1007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                12199
_reflns_number_total             12340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800252f-file002.cif
_cod_data_source_block           xs2381g
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1343.6(5)
_cod_database_code               4305292