NHC-Mediated Aggregation of P4: Isolation of a P12 Cluster
Jason D. Masuda; Wolfgang W. Schoeller; Bruno Donnadieu; Guy Bertrand; Journal of the American Chemical Society 129 (2007) 14180–14181; doi:10.1021/ja077296u

data_4110197
_publ_contact_author             'Prof G. Bertrand'
_publ_contact_author_address
;
University of California
UCR-CNRS Joint Research Lab
(UMR 2282) 
Department of Chemistry
Riverside, CA 92521 USA 
;
_publ_contact_author_email       ' guy.bertrand@ucr.edu '
_publ_contact_author_fax         951-827-4713
_publ_section_title
;
 NHC-Mediated Aggregation of P4: Isolation of a P12 Cluster
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14180
_journal_page_last               14181
_journal_paper_doi               10.1021/ja077296u
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C54 H75 N4 P12'
_chemical_formula_sum            'C54 H75 N4 P12'
_chemical_formula_weight         1151.82
_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                 96.5960(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6657(11)
_cell_length_b                   15.3695(17)
_cell_length_c                   38.351(4)
_cell_measurement_reflns_used    5694
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.76
_cell_measurement_theta_min      2.30
_cell_volume                     6245.1(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep 3'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Sir92
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0777
_diffrn_reflns_av_sigmaI/netI    0.0844
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            44549
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.9646
_exptl_absorpt_correction_T_min  0.8927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, version 2004/1'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             2428
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.00019(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         12736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0503P)^2^+1.9090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                8466
_reflns_number_total             12736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja077296usi20071017_014618_1.cif
_cod_data_source_block           3
_cod_original_cell_volume        6245.1(12)
_cod_database_code               4110197