Supermolecular Assembly of Tetra- and Hexanuclear Carbonyl Clusters Using a Novel Polydentate Pyridylphosphine Ligand
Koshevoy, Igor O.; Haukka, Matti; Pakkanen, Tapani A.; Tunik, Sergey P.; Vainiotalo, Pirjo; Organometallics 24 (2005) 3516–; doi:10.1021/om0502032

data_4075853
_publ_section_title
;
 Supermolecular Assembly of Tetra- and Hexanuclear Carbonyl Clusters Using
 a Novel Polydentate Pyridylphosphine Ligand
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3516
_journal_paper_doi               10.1021/om0502032
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C74.5 H50 Cl3 N2 O29 P2 Rh6 Ru6'
_chemical_formula_weight         2829.33
_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                 114.522(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.9444(4)
_cell_length_b                   17.9287(2)
_cell_length_c                   35.4368(5)
_cell_measurement_temperature    120(2)
_cell_volume                     17886.8(8)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL v.6.14 (Sheldrick, 2003)'
_computing_publication_material  'SHELXH-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f scans and \w scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            170091
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    2.259
_exptl_absorpt_correction_T_max  0.8329
_exptl_absorpt_correction_T_min  0.4330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Xprep in Shelxtl v.6.14 (Sheldrick, 2003)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    2.101
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       black
_exptl_crystal_F_000             10864
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.464
_refine_diff_density_min         -3.986
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2055
_refine_ls_number_reflns         31364
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+215.9122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                24425
_reflns_number_total             31364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0502032si20050318_060544.cif
_cod_data_source_block           structure_5
_cod_original_cell_volume        17886.8(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C74.50 H50 Cl3 N2 O29 P2 Rh6 Ru6'
_cod_database_code               4075853