(1α,2β,3α,6α,7β,8α,9β,13β)-9,13-Dibromo-11-methyl-14,15-dioxa-11-azapentacyclo[6.5.1.1^3,6^.0^2,7^.0^9,13^]pentadec-4-ene-10,12-dione
Warrener, Ronald N.; Maksimovic, L.; Kennard, Colin H. L.; Acta Crystallographica Section C 53 (1997) 1501–1502; doi:10.1107/S0108270197006616

data_2006627
_publ_section_title
(1\a,2\b,3\a,6\a,7\b,8\a,9\b,13\b)-9,13-Dibromo-11-methyl-14,15-dioxa-11-azapentacyclo[6.5.1.1^3,6^.0^2,7^.0^9,13^]pentadec-4-ene-10,12-dione
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1501
_journal_page_last               1502
_journal_paper_doi               10.1107/S0108270197006616
_journal_volume                  53
_journal_year                    1997
_chemical_formula_structural     'C13 H11 Br2 N O4'
_chemical_formula_sum            'C13 H11 Br2 N O4'
_chemical_formula_weight         405.05
_chemical_melting_point          519(3)
_chemical_name_systematic
;
(1\a,2\b,3\a,6\a,7\b,8\a,9\b,13\b)-9,13-dibromo-11-methyl-11-aza-
14,15-dioxa-11-pentacyclo [6.5.1.1^3,6^.0^2,7^.0^9,13^]
pentadec-4-en-10,12-dione
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.314(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3770(10)
_cell_length_b                   18.664(3)
_cell_length_c                   9.897(2)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      6
_cell_volume                     1356.8(4)
_computing_cell_refinement       SDP-Plus
_computing_data_collection       'SDP-Plus (Frenz, 1985)'
_computing_data_reduction        'Xtal3.2 DIFDAT (Hall, Flack & Stewart, 1992)'
_computing_molecular_graphics    'PLATON96 (Spek, 1996)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'CAD4 MicroVAX-controlled'
_diffrn_measurement_method       2\q/\w
_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    0.0511
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3412
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  '2 hours'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.986
_exptl_absorpt_correction_T_max  0.52
_exptl_absorpt_correction_T_min  0.21
_exptl_absorpt_correction_type
;
empirical \y scan (North, Phillips & Mathews, 1968)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.958
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.098
_refine_ls_hydrogen_treatment
;
hydrogen atoms in calculated positions, but not refined
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_restrained_S_obs      1.098
_refine_ls_R_factor_all          0.116
_refine_ls_R_factor_obs          .047
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0697P)^2^+1.0814P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.139
_refine_ls_wR_factor_obs         .110
_reflns_number_observed          1913
_reflns_number_total             3412
_reflns_observed_criterion       '>2 sigma(I)'
_cod_data_source_file            ta1163.cif
_cod_data_source_block           571rw3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '243-248\%C' was changed to '519(3)'
- it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '243-248\%C' was changed to '519(3)'
- it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0697P)^2^+1.0814P] 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^)+(0.0697P)^2^+1.0814P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               2006627