Stereospecific Intramolecular Reductive Cross-Electrophile Coupling Reactions for Cyclopropane Synthesis.
Tollefson, Emily J.; Erickson, Lucas W.; Jarvo, Elizabeth R.; Journal of the American Chemical Society 137 (2015) 9760–9763; doi:10.1021/jacs.5b03870

data_4124202
_publ_section_title
;
 Stereospecific Intramolecular Reductive Cross-Electrophile Coupling
 Reactions for Cyclopropane Synthesis.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9760
_journal_page_last               9763
_journal_paper_doi               10.1021/jacs.5b03870
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C22 H19 N O4'
_chemical_formula_weight         361.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90
_cell_angle_beta                 93.6709(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4673(7)
_cell_length_b                   8.7330(4)
_cell_length_c                   12.2472(5)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      2.48
_cell_volume                     1757.64(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
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_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20431
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.842
_diffrn_reflns_theta_min         2.479
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.8109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
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_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.343
_exptl_crystal_size_min          0.256
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    refall
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_refine_ls_number_reflns         4355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.8896P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1290
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3714
_reflns_number_total             4355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b03870_si_002.cif
_cod_data_source_block           erj12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4124202.cif.
;
_cod_database_code               4124202
_shelx_estimated_absorpt_t_min   0.966
_shelx_estimated_absorpt_t_max   0.976
_shelxl_version_number           2013-2
_shelx_res_checksum              359
_shelx_hkl_checksum              209