Guiding the nitrogen nucleophile to the middle: palladium-catalyzed decarboxylative cyclopropanation of 2-alkylidenetrimethylene carbonates with isocyanates
Shintani, Ryo; Moriya, Kohei; Hayashi, Tamio; Chemical Communications (Cambridge, United Kingdom) 47 (2011) 3057–3059; doi:10.1039/c0cc05308b

data_7112688
_publ_section_title
;
 Guiding the nitrogen nucleophile to the middle: palladium-catalyzed
 decarboxylative cyclopropanation of 2-alkylidenetrimethylene carbonates
 with isocyanates
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   11
_journal_name_full
'Chemical Communications (Cambridge, United Kingdom)'
_journal_page_first              3057
_journal_page_last               3059
_journal_paper_doi               10.1039/c0cc05308b
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C18 H16 Cl N O2 '
_chemical_formula_sum            'C18 H16 Cl N O2'
_chemical_formula_weight         313.78
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 102.76(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.369(5)
_cell_length_b                   16.869(9)
_cell_length_c                   9.901(7)
_cell_measurement_reflns_used    9110
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     1526.2(16)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      123(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.080
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14573
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

Higashi, T. (1995). Program for Absorption Correction.

Rigaku Corporation, Tokyo, Japan.

;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             656.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.95
_refine_diff_density_min         -1.63
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     215
_refine_ls_number_reflns         8816
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                8724
_reflns_number_total             3483
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c0cc05308b.txt
_cod_data_source_block           '_100610yuki'
_cod_original_cell_volume        1526.2(15)
_cod_original_formula_sum        'C18 H16 Cl N O2 '
_cod_database_code               7112688