Novel 1,4-Homofragmentation via an α-Lactone
Jollie D. Godfrey, Jr.; Rita T. Fox; Frederic G. Buono; Jack Z. Gougoutas; Mary F. Malley; Journal of Organic Chemistry 71 (2006) 8647–8650; doi:10.1021/jo0613380

data_4022038
_publ_contact_author_address
;Bristol Myers Squibb
P.O. Box 4000
Princeton NJ 08543-4000 USA
;
_publ_contact_author_email       jollie.godfrey@bms.com
_publ_contact_author_fax         609-252-7668
_publ_contact_author_name        'Jollie Godfrey'
_publ_contact_author_phone       609-252-4654
_publ_section_title
;
 Novel 1,4-Homofragmentation via an \a-Lactone
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8647
_journal_page_last               8650
_journal_paper_doi               10.1021/jo0613380
_journal_volume                  71
_journal_year                    2006
_chemical_absolute_configuration unk
_chemical_formula_moiety         C12H15ClO3
_chemical_formula_sum            'C12 H15 Cl O3'
_chemical_formula_weight         242.69
_chemical_melting_point          215-25deg.C
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.90(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.4818(13)
_cell_length_b                   9.5780(19)
_cell_length_c                   8.9682(18)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      28.87
_cell_measurement_theta_min      9.3
_cell_volume                     556.47(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      243
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       diffractometer
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1677
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1827
_diffrn_reflns_theta_full        64.82
_diffrn_reflns_theta_max         64.82
_diffrn_reflns_theta_min         4.93
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Rigaku RU200'
_diffrn_standards_decay_%        5.5
_diffrn_standards_interval_time  2400s
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.962
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             256
_exptl_crystal_recrystallization_method aq.MeOH
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .05
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.456
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1824
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.456
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0904
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2235
_refine_ls_wR_factor_ref         0.2430
_reflns_number_gt                1439
_reflns_number_total             1824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0613380si20060628_023829.cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'None' changed to 'none' 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 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4022038