Crystal structures of two triazola-dioxola-benzenacyclononaphanes
Viswanathan, Vijayan; Rao, Naga Siva; Raghunathan, Raghavachary; Velmurugan, Devadasan; Acta Crystallographica Section E 71 (2015) 827–831; doi:10.1107/S205698901501141X

data_2240861
_publ_section_title
;
 Crystal structures of two triazola-dioxola-benzenacyclononaphanes
;
_journal_coeditor_code           SU5103
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              827
_journal_page_last               831
_journal_paper_doi               10.1107/S205698901501141X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C25 H29 Br N5 O7'
_chemical_formula_moiety         'C25 H29 Br N5 O7'
_chemical_formula_sum            'C25 H29 Br N5 O7'
_chemical_formula_weight         591.44
_chemical_name_systematic
(<i>Z</i>)-1^5^-Bromo-3^2^,3^2^-dimethyl-2^1^-nitro-2^2^,2^3^,2^5^,2^6^,2^7^,2^7a^,3^3a^,3^5^,3^6^,3^6a^-decahydro-2^1^<i>H</i>,6^1^<i>H</i>-4,9-dioxa-2(3,2)-pyrrolizina-6(4,1)-triazola-3(5,6)-furo[2,3-<i>d</i>][1,3]dioxola-1(1,2)-benzenacyclononaphane
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 99.903(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.913(5)
_cell_length_b                   11.414(5)
_cell_length_c                   12.144(5)
_cell_measurement_reflns_used    6278
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      1.70
_cell_volume                     1353.6(11)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEXII area-detector'
_diffrn_measurement_method       '\w and \f scans'
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0922
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12444
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.378
_diffrn_reflns_theta_min         1.702
_exptl_absorpt_coefficient_mu    1.571
_exptl_absorpt_correction_T_max  0.8587
_exptl_absorpt_correction_T_min  0.7441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       block
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.458
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.007(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         6278
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0281P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.1051
_reflns_number_gt                3587
_reflns_number_total             6278
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           I
_cod_database_code               2240861
_shelx_hkl_checksum              10043
_shelx_res_checksum              48888
_shelxl_version_number           2014/6
_cod_database_fobs_code 2240861