Intramolecular Phosphorus-Phosphorus Bond Formation within a Co2P4 Core
Tianshu Li; Nicholas Arleth; Michael T. Gamer; Ralf Köppe; Timo Augenstein; Fabian Dielmann; Manfred Scheer; Sergey N. Konchenko; Peter W. Roesky; Inorganic Chemistry 52 (2013) 14231–14236; doi:10.1021/ic402159y

data_4337008
_publ_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT)
      Institut fuer Anorganische Chemie
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_publ_contact_author_email       roesky@kit.edu
_publ_contact_author_fax         '+49 721 6084854'
_publ_contact_author_phone       '+49 721 6086117'
_publ_section_title
;
 Intramolecular Phosphorus-Phosphorus Bond Formation within a Co2P4 Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              14231
_journal_page_last               14236
_journal_paper_doi               10.1021/ic402159y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C58 H96 Co2 P4 Sm'
_chemical_formula_sum            'C58 H96 Co2 P4 Sm'
_chemical_formula_weight         1185.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.202(8)
_cell_angle_beta                 84.017(9)
_cell_angle_gamma                63.168(7)
_cell_formula_units_Z            2
_cell_length_a                   13.0764(14)
_cell_length_b                   14.5320(14)
_cell_length_c                   17.9246(19)
_cell_measurement_reflns_used    10643
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.21
_cell_measurement_theta_min      1.62
_cell_volume                     2938.4(6)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'area detector'
_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  0.0969
_diffrn_reflns_av_sigmaI/netI    0.1649
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22333
_diffrn_reflns_theta_full        25.64
_diffrn_reflns_theta_max         25.64
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    1.687
_exptl_absorpt_correction_T_max  0.9052
_exptl_absorpt_correction_T_min  0.7328
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.037
_refine_diff_density_max         2.040
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.0138(6)
_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   0.861
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         10881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.861
_refine_ls_R_factor_all          0.1485
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1746
_reflns_number_gt                4683
_reflns_number_total             10881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402159y_si_002_3.cif
_cod_data_source_block           1b
_cod_original_cell_volume        2938.4(5)
_cod_database_code               4337008