4b,5,7,7a-Tetrahydro-4b,7a-epiminomethanoimino-6<i>H</i>-imidazo[4,5-<i>f</i>][1,10]phenanthroline-6,13-dione monohydrate
Rillema, D. Paul; Kirgan, Robert A.; Moore, Curtis; Koshy, Seena; Acta Crystallographica Section E 63 (2007) o3526–o3526; doi:10.1107/S1600536807034198

data_2214646
_publ_section_title
;4b,5,7,7a-Tetrahydro-4b,7a-epiminomethanoimino-6<i>H</i>-imidazo[4,5-<i>f</i>][1,10]phenanthroline-6,13-dione
 monohydrate
;
_journal_coeditor_code           FL2142
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3526
_journal_page_last               o3526
_journal_paper_doi               10.1107/S1600536807034198
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C14 H10 N6 O2, H2 O'
_chemical_formula_moiety         'C14 H10 N6 O2, H2 O'
_chemical_formula_sum            'C14 H12 N6 O3'
_chemical_formula_weight         312.30
_chemical_name_systematic
;
4b,5,7,7a-Tetrahydro-4b,7a-epiminomethanoimino-6H-
imidazo[4,5-f][1,10]phenanthroline-6,13-dione monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 108.528(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.5164(18)
_cell_length_b                   12.3920(12)
_cell_length_c                   12.6929(13)
_cell_measurement_reflns_used    9312
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.91
_cell_volume                     2761.5(5)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'SMART (Bruker, 2006)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2006)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 2006)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            68322
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.9728
_exptl_absorpt_correction_T_min  0.9376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'lusterous grey'
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+1.7397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                4600
_reflns_number_total             5422
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl2142.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2214646
_cod_database_fobs_code          2214646