Exploitation of cyclopropane ring-cleavage reactions for the rapid assembly of tetracyclic frameworks related to gibberellins.
Banwell, Martin G.; Phillis, Andrew T.; Willis, Anthony C.; Organic letters 8 (2006) 5341–5344; doi:10.1021/ol062224d

data_1506279
_publ_section_title
;
 Exploitation of cyclopropane ring-cleavage reactions for the rapid
 assembly of tetracyclic frameworks related to gibberellins.
;
_journal_issue                   23
_journal_name_full               'Organic letters'
_journal_page_first              5341
_journal_page_last               5344
_journal_paper_doi               10.1021/ol062224d
_journal_volume                  8
_journal_year                    2006
_chemical_compound_source
;
local
;
_chemical_formula_moiety         ' C17 H21 Cl3 O '
_chemical_formula_sum            'C17 H21 Cl3 O'
_chemical_formula_weight         347.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-03-11
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2005-11-04 - Report on C17 H21 Cl3 O
              by Anthony C. Willis
              for  Andrew Phillis and Martin Banwell

2005-11-04 - passes checkcif tests with no warnings

;
_cell_angle_alpha                90
_cell_angle_beta                 99.0435(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7868(3)
_cell_length_b                   6.4660(1)
_cell_length_c                   16.3562(3)
_cell_measurement_reflns_used    25149
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     1648.84(5)
_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       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32449
_diffrn_reflns_theta_full        27.497
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.613
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.839
_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    1.401
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
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_refine_diff_density_min         -0.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0654
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         2709
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.000755
_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:
  0.770 0.275 0.468
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0382
_refine_ls_wR_factor_gt          0.0316
_refine_ls_wR_factor_ref         0.0316
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                2709
_reflns_number_total             3781
_reflns_threshold_expression     I>3u(I)
_cod_data_source_file            ol062224dsi20060907_092214.cif
_cod_data_source_block           ban0519
_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      'P 1 21/n 1 '
_cod_original_formula_sum        ' C17 H21 Cl3 O '
_cod_database_code               1506279