Synthesis and Diels-Alder Reactivity of Substituted [4]Dendralenes.
Saglam, Mehmet F.; Alborzi, Ali R.; Payne, Alan D.; Willis, Anthony C.; Paddon-Row, Michael N; Sherburn, Michael S.; The Journal of organic chemistry 81 (2016) 1461–1475; doi:10.1021/acs.joc.5b02583

data_4031883
_publ_section_title
;
 Synthesis and Diels-Alder Reactivity of Substituted [4]Dendralenes.
;
_journal_issue                   4
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1461
_journal_page_last               1475
_journal_paper_doi               10.1021/acs.joc.5b02583
_journal_volume                  81
_journal_year                    2016
_chemical_compound_source        local
_chemical_formula_moiety         'C24 H27 N3 O6 , C H2 Cl2'
_chemical_formula_sum            'C25 H29 Cl2 N3 O6'
_chemical_formula_weight         538.43
_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             08-03-13
_audit_creation_method           CRYSTALS_ver_12.18
_audit_update_record
;
2008-02-17 - Report on C25 H29 Cl2 N3 O6
             by Anthony C. Willis
             for Ali Reza Alborzi and Mick Sherburn
2008-02-17 - passes checkcif tests with minor warnings
2015-09-01 - CCDC version
;
_cell_angle_alpha                90
_cell_angle_beta                 94.2880(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.8137(1)
_cell_length_b                   20.3565(2)
_cell_length_c                   19.3212(2)
_cell_measurement_reflns_used    70139
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     5025.67(8)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_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 KappaCCD'
_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  0.056
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            106256
_diffrn_reflns_theta_full        27.508
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         2.558
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.889
_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    1.423
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.10
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_refine_diff_density_min         -0.52
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8210
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     834
_refine_ls_number_reflns         11508
_refine_ls_number_restraints     209
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.049
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0934
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0934
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                7015
_reflns_number_total             11540
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.19
_oxford_diffrn_Wilson_scale      11.52
_oxford_refine_ls_scale          0.3437(2)
_oxford_structure_analysis_title '3071212 she0805'
_cod_data_source_file            jo5b02583_si_001.cif
_cod_data_source_block           compound_58
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_Hall     '-p 2yab'
_cod_original_sg_symbol_H-M      'P 1 21/a 1 '
_cod_database_code               4031883