Stereocontrol of intramolecular Diels–Alder reactions by an allylic diphenylcyclopropyl group
Tripoli, Regis; Cayzer, Tory N.; Willis, Anthony C.; Sherburn, Michael S.; Paddon-Row, Michael N.; Organic & Biomolecular Chemistry 5 (2007) 2606–; doi:10.1039/b708324f

data_7151152
_publ_section_title
;
 Stereocontrol of intramolecular Diels--Alder reactions by an allylic
 diphenylcyclopropyl group
;
_journal_issue                   16
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              2606
_journal_paper_doi               10.1039/b708324f
_journal_volume                  5
_journal_year                    2007
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C25 H24 O4 '
_chemical_formula_sum            'C25 H24 O4'
_chemical_formula_weight         388.46
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             04-01-11
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2004-11-01 - Report on C25 H24 O4
by Anthony C. Willis
for Regis Tripoli and Mick Sherburn
2004-11-01 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 96.0142(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9345(2)
_cell_length_b                   8.7920(2)
_cell_length_c                   16.3108(3)
_cell_measurement_reflns_used    24969
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     1987.27(6)
_computing_cell_refinement
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
COLLECT (Nonius BV, 1997)
;
_computing_data_reduction
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material
;
CRYSTALS (Watkin et al 2003)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2003)
;
_computing_structure_solution
;
SIR92 (Altomare et al, 1994)
;
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Nonius Kappa CCD
;
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41962
_diffrn_reflns_theta_full        27.477
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         2.635
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.968
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.17
_refine_diff_density_min         -0.15
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1283
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         3260
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.001518
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.857 0.561 0.698 0.187 0.178
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0427
_refine_ls_wR_factor_gt          0.0351
_refine_ls_wR_factor_ref         0.0351
_reflns_limit_h_max              17
_reflns_limit_h_min              -18
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                3260
_reflns_number_total             4543
_reflns_threshold_expression     I>2.00u(I)
_cod_data_source_file            b708324f.txt
_cod_data_source_block           mss048
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value ' not measured ' was changed to
'?' - the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 21/a 1 '
_cod_original_formula_sum        ' C25 H24 O4 '
_cod_database_code               7151152