Enantio- and Diastereoselective Organocatalytic Conjugate Additions of Nitroalkanes to Enone Diesters.
Horwitz, Matthew A.; Fulton, Jennifer L.; Johnson, Jeffrey S.; Organic letters 19 (2017) 5783–5785; doi:10.1021/acs.orglett.7b02735

data_1547701
_publ_section_title
;
 Enantio- and Diastereoselective Organocatalytic Conjugate Additions of
 Nitroalkanes to Enone Diesters.
;
_journal_issue                   21
_journal_name_full               'Organic letters'
_journal_page_first              5783
_journal_page_last               5785
_journal_paper_doi               10.1021/acs.orglett.7b02735
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C21 H28 Br N O7'
_chemical_formula_sum            'C21 H28 Br N O7'
_chemical_formula_weight         486.35
_chemical_name_common            166HC
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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   geom
_cell_angle_alpha                89.3430(11)
_cell_angle_beta                 87.7380(12)
_cell_angle_gamma                86.3034(12)
_cell_formula_units_Z            1
_cell_length_a                   5.84650(10)
_cell_length_b                   9.7587(2)
_cell_length_c                   9.8846(2)
_cell_measurement_reflns_used    123
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.0631
_cell_measurement_theta_min      2.0801
_cell_volume                     562.324(19)
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS, VERSION 2013/1'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius X8 Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21897
_diffrn_reflns_theta_full        31.56
_diffrn_reflns_theta_max         31.56
_diffrn_reflns_theta_min         2.06
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.868
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             252
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.468
_refine_ls_abs_structure_details
;

Flack x determined using 3167 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         7421
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.879
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0253
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                7033
_reflns_number_total             7421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b02735_si_001.cif
_cod_data_source_block           rds671
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' 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 1547701.cif.
;
_cod_database_code               1547701
_shelx_res_checksum              33051
_shelx_hkl_checksum              84076