Stereochemically Controlled Synthesis of Ruthenium(II) Complexes Containing Bis(oxazolin-2'-yl)pyridine Ligands. X-ray Crystal Structures of trans-[RuCl2(PPh3){κ3-N,N,N-(S,S)-iPr-pybox}] and [RuCl(CCCPh2)(PPh3){κ3-N,N,N-(S,S)-iPr-pybox}][PF6] ((S,S)-iPr-pybox= 2,6-Bis[4'-(S)-isopropyloxazolin-2'-yl]pyridine)
Victorio Cadierno; M. Pilar Gamasa; José Gimeno; Luis Iglesias; Santiago García-Granda; Inorganic Chemistry 38 (1999) 2874–2879; doi:10.1021/ic9813258

data_4322077
_publ_contact_author
;
      Santiago Garc\'ia-Granda
      Departamento de Qu\'imica F\'isica y Anal\'itica
      Facultad de Qu\'imica
      Universidad de Oviedo
      Avda. Juli\'an Claver\'ia, 8
      33071 Oviedo
      Spain
;
_publ_contact_author_email       sgg@sauron.quimica.uniovi.es
_publ_contact_author_fax         '0034 98 5103125'
_publ_contact_author_phone       '0034 98 5103477'
_publ_section_title
;
 Stereochemically Controlled Synthesis of Ruthenium(II) Complexes
 Containing Bis(oxazolin-2'-yl)pyridine Ligands. X-ray Crystal Structures
 of trans-[RuCl2(PPh3){\k3-N,N,N-(S,S)-iPr-pybox}] and
 [RuCl(CCCPh2)(PPh3){\k3-N,N,N-(S,S)-iPr-pybox}][PF6] ((S,S)-iPr-pybox=
 2,6-Bis[4'-(S)-isopropyloxazolin-2'-yl]pyridine)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2874
_journal_page_last               2879
_journal_paper_doi               10.1021/ic9813258
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C35 H38 Cl2 N3 O2 P Ru, C H Cl3'
_chemical_formula_sum            'C36 H39 Cl5 N3 O2 P Ru'
_chemical_formula_weight         854.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.772(6)
_cell_length_b                   15.208(5)
_cell_length_c                   19.601(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      6
_cell_volume                     3807(3)
_computing_cell_refinement       'CRYSDA (Beurskens et al, 1992)'
_computing_data_collection
;
 Nonius CAD-4 Diffractometer Control Software. Data collection with
 profile analysis over all reflections (Lehman and Larsen, 1974; 
 Grant and Gable, 1978)
;
_computing_data_reduction        'THE REFLEX (local program)'
_computing_molecular_graphics    'EUCLID (Spek, 1982)'
_computing_publication_material
;
 SHELXL-97 (Sheldrick, 1997). All calculations made at the University 
 of Oviedo on the Scientific Computer Center and X-Ray group 
 DEC/AXP-computers.
;
_computing_structure_refinement
;
SHELXL-97 (Sheldrick, 1997). Geometrical calculations made with 
PARST (Nardelli, 1983).
;
_computing_structure_solution
;
 Patterson methods using DIRDIF (Beurskens, 1992)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Nonius CAD4
;
_diffrn_measurement_method       \w-2\Q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0839
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            4164
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        8
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
XABS2 (Parkin et al., 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         4164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+5.1625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1086
_reflns_number_gt                3277
_reflns_number_total             4164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9813258_1.cif
_cod_data_source_block           liv31(3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+5.1625P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+5.1625P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322077