Unprecedented cubane-type silver cluster with a novel phosphinite functionalized N-heterocyclic carbene ligand
Raynal, Matthieu; Liu, Xianghao; Pattacini, Roberto; Vallée, Christophe; Olivier-Bourbigou, Hélène; Braunstein, Pierre; Dalton Transactions  (2009) 7288–; doi:10.1039/b911439d

data_7001951
_publ_section_title
;
 Unprecedented cubane-type silver cluster with a novel phosphinite
 functionalized N-heterocyclic carbene ligand
;
_journal_issue                   35
_journal_name_full               'Dalton Transactions'
_journal_page_first              7288
_journal_paper_doi               10.1039/b911439d
_journal_year                    2009
_chemical_formula_moiety         'C21 H34 N2 O P, C4 H8 O, I'
_chemical_formula_sum            'C25 H42 I N2 O2 P'
_chemical_formula_weight         560.48
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 112.949(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.511(2)
_cell_length_b                   12.0084(10)
_cell_length_c                   16.9043(7)
_cell_measurement_reflns_used    9255
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     5703.3(7)
_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_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_av_sigmaI/netI    0.1047
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17320
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.45
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.200
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULscanABS in PLATON (Spek, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         5606
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1629
_reflns_number_gt                2800
_reflns_number_total             5606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b911439d.txt
_cod_data_source_block           Compound3_THF
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7001951