Observation of a Tricyclic[4.1.0.02,4]heptane During a Michael Addition-Ring Closure Reaction and a Computational Study on Its Mechanism of Formation.
Farren-Dai, Marco; Thompson, John R.; Bernardi, Anna; Colombo, Cinzia; Bennet, Andrew J.; The Journal of organic chemistry 82 (2017) 12511–12519; doi:10.1021/acs.joc.7b02218

data_4033134
_publ_section_title
;
 Observation of a Tricyclic[4.1.0.02,4]heptane During a Michael
 Addition-Ring Closure Reaction and a Computational Study on Its Mechanism
 of Formation.
;
_journal_issue                   23
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12511
_journal_page_last               12519
_journal_paper_doi               10.1021/acs.joc.7b02218
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C15 H19 N O6'
_chemical_formula_sum            'C15 H19 N O6'
_chemical_formula_weight         309.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                93.180(4)
_cell_angle_beta                 100.480(4)
_cell_angle_gamma                98.749(4)
_cell_formula_units_Z            4
_cell_length_a                   11.1968(9)
_cell_length_b                   11.2580(10)
_cell_length_c                   12.7572(11)
_cell_measurement_reflns_used    9736
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      2.35
_cell_volume                     1557.1(2)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2013)'
_computing_structure_refinement
'SHELXL-2014/7 (Sheldrick, 2015),Shelxle (H\"ubschle et al., 2011)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            52158
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.536
_diffrn_reflns_theta_min         1.629
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9376
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Sheldrick , 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.960
_exptl_crystal_size_mid          0.510
_exptl_crystal_size_min          0.186
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.187
_refine_ls_extinction_coef       0.0064(14)
_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   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         5794
_refine_ls_number_restraints     361
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0677P)^2^+1.0824P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4850
_reflns_number_total             5794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b02218_si_002.cif
_cod_data_source_block           CC_295
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 4033134.cif.
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_cod_database_code               4033134
_shelx_res_checksum              16129
_shelx_hkl_checksum              92497