Base-promoted reactions of dichlorocarbene adducts of cyclic enamines: a new route to annulated pyrroles.
Bissember, Alex C.; Phillis, Andrew T.; Banwell, Martin G.; Willis, Anthony C.; Organic letters 9 (2007) 5421–5424; doi:10.1021/ol7021774

data_1505597
_publ_section_title
;
 Base-promoted reactions of dichlorocarbene adducts of cyclic enamines: a
 new route to annulated pyrroles.
;
_journal_issue                   26
_journal_name_full               'Organic letters'
_journal_page_first              5421
_journal_page_last               5424
_journal_paper_doi               10.1021/ol7021774
_journal_volume                  9
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_compound_source        local
_chemical_formula_moiety         'C15 H17 Cl2 N O'
_chemical_formula_sum            'C15 H17 Cl2 N O'
_chemical_formula_weight         298.21
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-02-02
_audit_creation_method           CRYSTALS_ver_12.18
_audit_update_record
;
2006-02-03 - Report on C15 H17 Cl2 N O
              by Anthony C. Willis
              for Andrew Phillis and Martin Banwell

2006-02-03 - passes checkcif tests with no warnings

;
_cell_angle_alpha                90
_cell_angle_beta                 91.9718(14)
_cell_angle_gamma                90
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_cell_length_a                   15.5984(3)
_cell_length_b                   13.5175(3)
_cell_length_c                   6.6823(1)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     1408.14(5)
_computing_cell_refinement       'Denzo/Scalepack '
_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 '
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_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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'
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_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13930
_diffrn_reflns_theta_full        26.662
_diffrn_reflns_theta_max         27.5
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_diffrn_standards_number         0
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;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            yellow
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_exptl_crystal_description       block
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_refine_ls_abs_structure_details
;
Flack (1983), 1619 Friedel-pairs
The crystal is inversion twinned.
;
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_extinction_method     None
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_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
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_refine_ls_shift/su_max          0.002654
_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:
  0.707 -0.0217 0.367
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0241
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_reflns_limit_h_max              20
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_reflns_limit_k_max              17
_reflns_limit_k_min              0
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_reflns_limit_l_min              -8
_reflns_number_gt                2999
_reflns_number_total             3155
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.45
_oxford_diffrn_Wilson_scale      1.10
_oxford_refine_ls_scale          1.0692(10)
_oxford_structure_analysis_title '2021723 ban0605'
_cod_data_source_file            ol7021774-file003.cif
_cod_data_source_block           ban0605
_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 c 1 '
_cod_database_code               1505597