Nickel-catalyzed [3+1+1] cycloaddition reactions of alkenyl Fischer carbene complexes with methylenecyclopropanes.
Kamikawa, Ken; Shimizu, Yasunori; Takemoto, Shin; Matsuzaka, Hiroyuki; Organic letters 8 (2006) 4011–4014; doi:10.1021/ol061559s

data_1506164
_publ_section_title
;
 Nickel-catalyzed [3+1+1] cycloaddition reactions of alkenyl Fischer
 carbene complexes with methylenecyclopropanes.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4011
_journal_page_last               4014
_journal_paper_doi               10.1021/ol061559s
_journal_volume                  8
_journal_year                    2006
_chemical_formula_sum            'C56 H50 Cl6 N4 O4 S2'
_chemical_formula_weight         1119.82
_chemical_name_systematic        ?
_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                 110.11(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.894(7)
_cell_length_b                   25.242(13)
_cell_length_c                   19.300(8)
_cell_measurement_temperature    296(2)
_cell_volume                     6814(6)
_computing_cell_refinement       'RIGAKU PROCESS AUTO'
_computing_data_collection       'RIGAKU PROCESS AUTO'
_computing_data_reduction        'RIGAKU PROCESS AUTO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'RIGAKU RAXIS RAPID'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1757
_diffrn_reflns_av_sigmaI/netI    0.1909
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            54486
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.9015
_exptl_absorpt_correction_T_min  0.7901
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   ABSCOR
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.097
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.293
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         15238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.293
_refine_ls_R_factor_all          0.3993
_refine_ls_R_factor_gt           0.2166
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4660
_refine_ls_wR_factor_ref         0.5352
_reflns_number_gt                4683
_reflns_number_total             15238
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol061559ssi20060625_105543.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               1506164