Triruthenium and Triosmium Carbonyl Cluster Complexes Containing Bridging Ligands Derived from 2-Amino-7,8-benzoquinoline
Cabeza, Javier A.; del Río, Ignacio; García-Granda, Santiago; Riera, Víctor; Suárez, Marta; Organometallics 21 (2002) 5055–; doi:10.1021/om0205647

data_4077081
_publ_section_title
;
 Triruthenium and Triosmium Carbonyl Cluster Complexes Containing Bridging
 Ligands Derived from 2-Amino-7,8-benzoquinoline
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5055
_journal_paper_doi               10.1021/om0205647
_journal_volume                  21
_journal_year                    2002
_chemical_compound_source
;
Synthesis. Crystallization from a 
dichloromethane/hexane solution 
at room temperature by slow liquid-liquid difussion.
;
_chemical_formula_moiety         'C32 H18 N4 O6 Ru3, C H2 Cl2'
_chemical_formula_sum            'C33 H20 Cl2 N4 O6 Ru3'
_chemical_formula_weight         942.64
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.985(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2841(3)
_cell_length_b                   10.6019(3)
_cell_length_c                   22.6787(5)
_cell_measurement_reflns_used    5856
_cell_measurement_temperature    120(2)
_cell_volume                     3192.08(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'EUCLID (Spek, 1982)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17646
_diffrn_reflns_theta_full        68.38
_diffrn_reflns_theta_max         68.38
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    13.343
_exptl_absorpt_correction_T_max  0.176
_exptl_absorpt_correction_T_min  0.103
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.685
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         5854
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0951p)^2^+12.5933p] where p=(fo^2^+2fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1593
_reflns_number_gt                5478
_reflns_number_total             5854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0205647.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_ambient_temperature' value '1202)' was changed to '120(2)' -
precision was estimated.

'_refine_ls_structure_factor_coef' value
'fsqd' changed to 'Fsqd' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4077081