Assembling metals and clusters around an octaphosphine ligand based on N-substituted bis(diphenylphosphanyl)amines: structural characterization of dendrimer-like Co~12~ and Co~16~ branched clusters
Rodriguez-Zubiri, Mireia; Gallo, Vito; Rosé, Jacky; Welter, Richard; Braunstein, Pierre; Chemical Communications (Cambridge, United Kingdom)  (2008) 64–66; doi:10.1039/b713540h

data_7113165
_publ_section_title
;
 Assembling metals and clusters around an octaphosphine ligand based on
 N-substituted bis(diphenylphosphanyl)amines: structural characterization
 of dendrimer-like Co~12~ and Co~16~ branched clusters
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   1
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              64
_journal_page_last               66
_journal_paper_doi               10.1039/b713540h
_journal_year                    2008
_chemical_formula_moiety
'C146 H106 Cl4 Co12 N4 O28 P8 S4, 3(C H2 Cl2), 2(C6 H14)'
_chemical_formula_sum            'C161 H140 Cl10 Co12 N4 O28 P8 S4'
_chemical_formula_weight         4016.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 111.493(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.034(5)
_cell_length_b                   19.519(5)
_cell_length_c                   23.247(7)
_cell_measurement_reflns_used    21809
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.131
_cell_measurement_theta_min      0.998
_cell_volume                     8881(4)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p 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  0.0720
_diffrn_reflns_av_sigmaI/netI    0.1131
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            43501
_diffrn_reflns_theta_full        29.14
_diffrn_reflns_theta_max         29.14
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    1.424
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4072
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.293
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1035
_refine_ls_number_reflns         23877
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.1655
_refine_ls_R_factor_gt           0.0968
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.2051
_reflns_number_gt                14910
_reflns_number_total             23877
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7102766
_cod_data_source_file            b713540h.txt
_cod_data_source_block           spider_Co12
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7113165