Effect of protic additives in Cu-catalysed asymmetric Diels-Alder cycloadditions of doubly activated dienophiles: towards the synthesis of magellanine-type Lycopodium alkaloids
Lindsay, Vincent; Murphy, Rebecca; Sarpong, Richmond; Chem. Commun.  (2017) –; doi:10.1039/C7CC06367A

data_7120604
_publ_section_title
;
 Effect of protic additives in Cu-catalysed asymmetric Diels-Alder
 cycloadditions of doubly activated dienophiles: towards the synthesis of
 magellanine-type Lycopodium alkaloids
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06367A
_journal_year                    2017
_chemical_formula_sum            'C18 H30 O4 Si'
_chemical_formula_weight         338.51
_chemical_name_common            VLI-005B3
_chemical_name_systematic
; 
 sarpong43 
;
_space_group.centring_type       P
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_audit_update_record
;
2017-08-14 deposited with the CCDC.
2017-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                81.6640(10)
_cell_angle_beta                 80.2810(10)
_cell_angle_gamma                80.8850(10)
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_cell_length_b                   7.0658(7)
_cell_length_c                   20.0779(19)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.94
_cell_volume                     948.40(16)
_computing_cell_refinement       'Bruker SAINT'
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_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_refln_scan_rate          10
_diffrn_refln_scan_width         0.5
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22218
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        25.000
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_diffrn_reflns_theta_min         2.074
_diffrn_source                   'fine-focus sealed source'
_exptl_absorpt_coefficient_mu    0.140
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_exptl_crystal_colour            colorless
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         3493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0368P)^2^+0.4714P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3368
_reflns_number_total             3493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06367a2.cif
_cod_data_source_block           sarpong43
_cod_depositor_comments
;
The following automatic conversions were performed:

'_space_group.centring_type' value 'primitive' was replaced with the
value 'P' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5642 2017-10-24 12:04:52Z antanas 
;
_cod_database_code               7120604
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.972
_shelxl_version_number           2012-9
_shelx_res_checksum              71356