Ensemble of Pinanones from the Permanganate Oxidation of Myrtenal.
Clay, Julia M.; Hesek, Dusan; Oliver, Allen G.; Lee, Mijoon; Fisher, Jed F.; The Journal of organic chemistry 81 (2016) 5705–5709; doi:10.1021/acs.joc.6b00756

data_4032020
_publ_section_title
;
 Ensemble of Pinanones from the Permanganate Oxidation of Myrtenal.
;
_journal_issue                   13
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5705
_journal_page_last               5709
_journal_paper_doi               10.1021/acs.joc.6b00756
_journal_volume                  81
_journal_year                    2016
_chemical_absolute_configuration syn
_chemical_compound_source        'Julia M. Clay, SIP student in Jed Fisher lab'
_chemical_formula_sum            'C10 H14 O4'
_chemical_formula_weight         198.21
_chemical_name_common            'PNU-143663  29580-jff-20B'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             8/1998
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.968(5)
_cell_length_b                   8.073(5)
_cell_length_c                   17.744(10)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      5.18
_cell_volume                     998.1(11)
_computing_cell_refinement       Denzo
_computing_data_collection       Mar/ADSC
_computing_data_reduction        Denzo
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.94
_diffrn_measurement_device_type  'Mar Imaging Plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5737
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         5.18
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1.84(275)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.089
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          -0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+0.5829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1515
_reflns_number_gt                999
_reflns_number_total             1140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo6b00756_si_002.cif
_cod_data_source_block           compound4
_cod_database_code               4032020
_database_code_name              JMC1
_refine_ls_restrained_s_ref      1.104