P-C dichotomy: divergent iron(-I)-mediated alkyne and phosphaalkyne cycloligomerisations.
Wolf, Robert; Ghavtadze, Nugzar; Weber, Katharina; Schnöckelborg, Eva-Maria; de Bruin, Bas; Ehlers, Andreas W.; Lammertsma, Koop; Dalton transactions (Cambridge, England : 2003) 39 (2010) 1453–1456; doi:10.1039/b923663p

data_7024977
_publ_section_title
;
 P-C dichotomy: divergent iron(-I)-mediated alkyne and phosphaalkyne
 cycloligomerisations.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1453
_journal_page_last               1456
_journal_paper_doi               10.1039/b923663p
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C82.67 H93.33 Fe K O9.67'
_chemical_formula_weight         1336.52
_chemical_name_systematic
;
?
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_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                81.5020(10)
_cell_angle_beta                 87.1640(10)
_cell_angle_gamma                87.7830(10)
_cell_formula_units_Z            3
_cell_length_a                   10.8712(5)
_cell_length_b                   12.8003(6)
_cell_length_c                   39.1692(19)
_cell_measurement_reflns_used    8784
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      0.53
_cell_volume                     5381.4(4)
_computing_cell_refinement       'APEX2(Bruker AXS, 2007)'
_computing_data_collection       'APEX2(Bruker AXS, 2007)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2007 )'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_solution
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            48105
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         0.53
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  0.9935
_exptl_absorpt_correction_T_min  0.9286
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            dark-orange
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2135
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.381(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2501
_refine_ls_number_reflns         40376
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+2.2410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                29953
_reflns_number_total             40376
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b923663p.txt
_cod_data_source_block           p1fin
_cod_original_sg_symbol_H-M      P1
_cod_database_code               7024977