Diene-Transmissive Enantioselective Diels-Alder Reactions and Sequences Involving Substituted Dendralenes.
George, Josemon; Sherburn, Michael S.; The Journal of organic chemistry  (2019) –; doi:10.1021/acs.joc.9b02296

data_4033657
_publ_section_title
;
 Diene-Transmissive Enantioselective Diels-Alder Reactions and Sequences
 Involving Substituted Dendralenes.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b02296
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_compound_source        local
_chemical_formula_moiety         'C18 H24 O4'
_chemical_formula_sum            'C18 H24 O4'
_chemical_formula_weight         304.39
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             16-02-08
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2016-02-09 - Report on C18 H24 O4
             by Anthony C. Willis
             for Josemon George and Mick Sherburn

2016-02-09 - details of refinement in _refine_special_details below

2016-02-09 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 103.8053(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.1640(1)
_cell_length_b                   10.8451(1)
_cell_length_c                   10.6270(1)
_cell_measurement_reflns_used    10060
_cell_measurement_temperature    150
_cell_measurement_theta_max      72
_cell_measurement_theta_min      4
_cell_volume                     801.806(16)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2015)'
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
;
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2015)'
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Supernova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.018
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12636
_diffrn_reflns_theta_full        71.129
_diffrn_reflns_theta_max         72.581
_diffrn_reflns_theta_min         4.284
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.11
_refine_diff_density_min         -0.14
_refine_ls_abs_structure_details 'Flack (1983), 1183 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.08(12)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0046
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         2850
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.0044360
_refine_ls_shift/su_mean         0.0006100
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.10P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0629
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0629
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              11
_reflns_limit_k_min              -13
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                2819
_reflns_number_total             2850
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.96
_oxford_diffrn_Wilson_scale      0.01
_oxford_refine_ls_r_factor_ref   0.0245
_oxford_refine_ls_scale          9.5(3)
_oxford_reflns_number_all        2850
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'Z:\she1604SN\Tony_she1604SN_data At 17:30 on'
_cod_data_source_file            jo9b02296_si_002.cif
_cod_data_source_block           she1604SN
_cod_original_sg_symbol_Hall     'P 2yb '
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               4033657
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT O    (    1 ,X'S,U'S)  UNTIL C    (   18 ) 
CONT H    (    1 ,X'S)  UNTIL H    (  183 ) 
CONT ENANTIO 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;