Synthesis of Hexacyclic Parnafungin A and C Models
Quan Zhou; Barry B. Snider; Journal of Organic Chemistry 75 (2010) 8224–8233; doi:10.1021/jo101826p

data_4025856
_publ_section_title
;
 Synthesis of Hexacyclic Parnafungin A and C Models
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8224
_journal_page_last               8233
_journal_paper_doi               10.1021/jo101826p
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C14 H9 I1 O4'
_chemical_formula_sum            'C14 H9 I O4'
_chemical_formula_weight         368.13
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-12-12
_audit_creation_method           CRYSTALS_ver_12.87
_cell_angle_alpha                90
_cell_angle_beta                 96.533(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7699(4)
_cell_length_b                   4.7912(3)
_cell_length_c                   32.4130(18)
_cell_measurement_reflns_used    5788
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1198.81(12)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            18655
_diffrn_reflns_theta_full        30.003
_diffrn_reflns_theta_max         30.003
_diffrn_reflns_theta_min         1.265
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.678
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.040
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'acicular fragment'
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.118
_refine_diff_density_max         2.79
_refine_diff_density_min         -3.23
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3488
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.0017247
_refine_ls_shift/su_mean         2.3034749
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.00P)^2^ +17.43P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1234
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1234
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              6
_reflns_limit_k_min              0
_reflns_limit_l_max              45
_reflns_limit_l_min              0
_reflns_number_gt                3102
_reflns_number_total             3488
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.40
_oxford_diffrn_Wilson_scale      4.95
_oxford_refine_ls_r_factor_ref   0.0677
_oxford_refine_ls_scale          0.3532(5)
_oxford_reflns_number_all        3488
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'Quan6_33_1_01 in P2(1)/c'
_cod_data_source_file            jo101826p_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C14 H9 I1 O4'
_cod_database_code               4025856