Cross-coupling for cross-conjugation: practical synthesis and Diels-Alder reactions of [3]dendralenes.
Bradford, Tanya A.; Payne, Alan D.; Willis, Anthony C.; Paddon-Row, Michael N; Sherburn, Michael S.; Organic letters 9 (2007) 4861–4864; doi:10.1021/ol7021998

data_1505606
_publ_section_title
;
 Cross-coupling for cross-conjugation: practical synthesis and Diels-Alder
 reactions of [3]dendralenes.
;
_journal_issue                   23
_journal_name_full               'Organic letters'
_journal_page_first              4861
_journal_page_last               4864
_journal_paper_doi               10.1021/ol7021998
_journal_volume                  9
_journal_year                    2007
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C16 H17 Cl N2 O4, 0.5(C2 H4 Cl2) '
_chemical_formula_sum            'C17 H19 Cl2 N2 O4'
_chemical_formula_weight         386.23
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-22-02
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2005-02-22 - Report on  C34 H38 Cl4 N4 O8 - (TB08)
             by Anthony C. Willis
             for Tanya Bradford and Mick Sherburn
2005-02-22 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 110.4753(16)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.3354(7)
_cell_length_b                   8.4373(2)
_cell_length_c                   17.0270(4)
_cell_measurement_reflns_used    72160
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     3544.37(16)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.04
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39719
_diffrn_reflns_theta_full        27.492
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.551
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.894
_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    1.448
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.58
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0811
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         2420
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.002324
_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: 
 1.78 0.797 1.21 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0654
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0605
_reflns_limit_h_max              32
_reflns_limit_h_min              -34
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                2420
_reflns_number_total             4054
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ol7021998-file003.cif
_cod_data_source_block           she0506
_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_values 1715 2011-07-08 13:25:40Z adriana 

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      'C 1 2/c 1 '
_cod_original_formula_sum        ' C17 H19 Cl2 N2 O4 '
_cod_database_code               1505606