Approaches to the quaternary stereocentre and to the heterocyclic core in diazonamide A using the Heck reaction and related coupling reactions
Booker, James E. M.; Boto, Alicia; Churchill, Gwydion H.; Green, Clive P.; Ling, Matthew; Meek, Graham; Prabhakaran, Jaya; Sinclair, David; Blake, Alexander J.; Pattenden, Gerald; Organic & Biomolecular Chemistry 4 (2006) 4193–; doi:10.1039/b609604b

data_7151298
_publ_section_title
;
 Approaches to the quaternary stereocentre and to the heterocyclic core
 in diazonamide A using the Heck reaction and related coupling
 reactions
;
_journal_issue                   22
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              4193
_journal_paper_doi               10.1039/b609604b
_journal_volume                  4
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C23 H20 Br N O2'
_chemical_formula_sum            'C23 H20 Br N O2'
_chemical_formula_weight         422.31
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens
'introduced at calculated positions, except for amide H (not found)'
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-96
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.865(11)
_cell_length_b                   15.761(11)
_cell_length_c                   19.557(11)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      12.3
_cell_measurement_theta_min      11.0
_cell_volume                     3965(5)
_computing_cell_refinement       'STADI4 (Stoe & Cie, 1995a)'
_computing_data_collection       'STADI4 (Stoe & Cie, 1995a)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1995b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measurement_device       'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       omega/2-theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1430
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3102
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        'random variation +/-10'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.090
_exptl_absorpt_correction_T_max  0.725
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 1995b)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       column
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.64
_refine_diff_density_rms         0.13
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.33
_refine_ls_goodness_of_fit_obs   1.37
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         3102
_refine_ls_number_restraints     511
_refine_ls_restrained_S_all      1.24
_refine_ls_restrained_S_obs      1.19
_refine_ls_R_factor_all          0.218
_refine_ls_R_factor_obs          0.111
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.00P)^2^+48.3P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.240
_refine_ls_wR_factor_obs         0.175
_reflns_number_observed          1755
_reflns_number_total             3102
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            b609604b.txt
_cod_data_source_block           BZFUAM
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.00P)^2^+48.3P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.00P)^2^+48.3P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3966(5)
_cod_database_code               7151298