4,15-Dimethyl-7,12-diazoniatricyclo[10.4.0.0^2,7^]hexadeca-1(12),2,4,6,13,15-hexaene dibromide monohydrate
Behrman, Edward J.; Hansen, Alexandar L.; Yuan, Chunhua; Parkin, Sean; Acta Crystallographica Section E 76 (2020) 1467–1471; doi:10.1107/S2056989020011147

data_2243548
_publ_section_title
;
 4,15-Dimethyl-7,12-diazoniatricyclo[10.4.0.0^2,7^]hexadeca-1(12),2,4,6,13,15-hexaene
 dibromide monohydrate
;
_journal_coeditor_code           EX2036
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1467
_journal_page_last               1471
_journal_paper_doi               10.1107/S2056989020011147
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C16 H20 N2 2+, 2(Br -), H2 O'
_chemical_formula_moiety         'C16 H20 N2 2+, 2(Br -), H2 O'
_chemical_formula_sum            'C16 H22 Br2 N2 O'
_chemical_formula_weight         418.17
_chemical_name_systematic
'4,15-Dimethyl-7,12-diazoniatricyclo[10.4.0.0^2,7^]hexadeca-1(12),2,4,6,13,15-hexaene dibromide monohydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 101.1620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6402(2)
_cell_length_b                   13.7578(3)
_cell_length_c                   16.7691(3)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.76
_cell_volume                     1729.30(7)
_computing_cell_refinement
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>XP</i> in <i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_publication_material
;
<i>SHELX</i> (Sheldrick, 2008), <i>CIFFIX</i> (Parkin, 2013),
and
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26025
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.529
_diffrn_reflns_theta_min         2.476
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    4.688
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       'irregular shard'
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.381
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3959
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0121P)^2^+1.4994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0431
_reflns_number_gt                3527
_reflns_number_total             3959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ex2036sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243548
_cod_database_fobs_code          2243548
_shelx_estimated_absorpt_t_min   0.521
_shelx_estimated_absorpt_t_max   0.735
_shelx_hkl_checksum              22470
_shelx_res_checksum              96264