Structures of 1-hydrophenanthroimidazoles: building blocks in the synthesis of expanded-ring bis(imidazoles)
Stibrany, Robert T.; Potenza, Joseph A.; Acta Crystallographica Section C 65 (2009) o406–o409; doi:10.1107/S0108270109025165

data_2017228
_publ_section_title
;
 Structures of 1-hydrophenanthroimidazoles: building blocks in the
 synthesis of expanded-ring bis(imidazoles)
;
_journal_coeditor_code           FG3095
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o406
_journal_page_last               o409
_journal_paper_doi               10.1107/S0108270109025165
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C15 H8 Br2 N2 , 0.5H2 O'
_chemical_formula_moiety         'C15 H8 Br2 N2 , 0.5H2 O'
_chemical_formula_sum            'C15 H9 Br2 N2 O0.5'
_chemical_formula_weight         385.04
_chemical_melting_point          583
_chemical_name_systematic
;
3,6-dibromo-1-<i>H</i>-phenanthro[9,10-<i>d</i>]imidazole hemihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                101.683(4)
_cell_angle_beta                 101.398(5)
_cell_angle_gamma                104.109(5)
_cell_formula_units_Z            4
_cell_length_a                   8.415(2)
_cell_length_b                   10.139(2)
_cell_length_c                   17.227(4)
_cell_measurement_reflns_used    824
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.909
_cell_measurement_theta_min      2.182
_cell_volume                     1347.9(5)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and ORTEP32 (Farrugia, 1997)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12857
_diffrn_reflns_theta_full        26.10
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         2.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.004
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Blessing, 1995)'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.294
_refine_diff_density_min         -0.770
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5330
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0728P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1278
_reflns_number_gt                3658
_reflns_number_total             5330
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3095.cif
_cod_data_source_block           II
_cod_database_code               2017228
_cod_database_fobs_code          2017228