Total synthesis of diazonamide A.
Knowles, Robert R.; Carpenter, Joseph; Blakey, Simon B.; Kayano, Akio; Mangion, Ian K.; Sinz, Christopher J.; Macmillan, David W. C.; Chemical science (Royal Society of Chemistry : 2010) 2011 (2011) 308–311; doi:10.1039/C0SC00577K

data_1515413
_publ_section_title
;
 Total synthesis of diazonamide A.
;
_journal_issue                   2
_journal_name_full
'Chemical science (Royal Society of Chemistry : 2010)'
_journal_page_first              308
_journal_page_last               311
_journal_paper_doi               10.1039/C0SC00577K
_journal_volume                  2011
_journal_year                    2011
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C47 H59 Cl3 N4 O8 Si, CH Cl3'
_chemical_formula_sum            'C47 H59 Cl3 N4 O8 Si'
_chemical_formula_weight         942.42
_chemical_name_systematic
;
?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 105.63(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.546(4)
_cell_length_b                   17.360(4)
_cell_length_c                   19.889(4)
_cell_measurement_reflns_used    8612
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      24.4
_cell_measurement_theta_min      2.6
_cell_volume                     6499(3)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0832
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8612
_diffrn_reflns_theta_full        24.38
_diffrn_reflns_theta_max         24.38
_diffrn_reflns_theta_min         2.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.963
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         5228
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1515
_refine_ls_R_factor_gt           0.1136
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2908
_refine_ls_wR_factor_ref         0.3174
_reflns_number_gt                3121
_reflns_number_total             5228
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c0sc00577k.txt
_cod_data_source_block           k08308
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        6499(2)
_cod_original_sg_symbol_Hall     C2y
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               1515413