Nickel(II)-catalyzed asymmetric intramolecular Alder-ene reaction of 1,7-dienes
Liu, Wen; Zhou, Pengfei; Lang, Jiawen; Dong, Shunxi; Liu, Xiaohua; Feng, Xiaoming; Chemical Communications  (2019) –; doi:10.1039/C9CC01521C

data_7123152
_publ_section_title
;
 Nickel(II)-catalyzed asymmetric intramolecular Alder-ene reaction of
 1,7-dienes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01521C
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_sum            'C24 H27 N O6 S'
_chemical_formula_weight         457.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-01-09 deposited with the CCDC.    2019-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.835(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8246(12)
_cell_length_b                   8.6734(6)
_cell_length_c                   18.6689(15)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    171(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.78
_cell_volume                     2330.8(3)
_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-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      171(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
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_diffrn_reflns_limit_k_max       11
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_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53911
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.304
_diffrn_reflns_theta_min         2.742
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6951
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 4288 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         11524
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+0.1537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                10347
_reflns_number_total             11524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01521c2.cif
_cod_data_source_block           mo_20181024_lw_cw_0m_a
_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/RSC/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 
;
_cod_database_code               7123152
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              57229