3,4,7,8-Tetramethyl-1,10-phenanthrolin-1-ium nitrate monohydrate
Zhang, Ke-Jie; Zhang, Yan-Fang; Acta Crystallographica Section E 68 (2012) o1931–o1932; doi:10.1107/S1600536812023318

data_2235310
_publ_section_title
;
 3,4,7,8-Tetramethyl-1,10-phenanthrolin-1-ium nitrate monohydrate
;
_journal_coeditor_code           XU5537
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1931
_journal_page_last               o1932
_journal_paper_doi               10.1107/S1600536812023318
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C16 H17 N2 +, N O3 -, H2 O'
_chemical_formula_moiety         'C16 H17 N2 +, N O3 -, H2 O'
_chemical_formula_sum            'C16 H19 N3 O4'
_chemical_formula_weight         317.34
_chemical_name_systematic
;
3,4,7,8-Tetramethyl-1,10-phenanthrolin-1-ium nitrate monohydrate
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   6.7401(8)
_cell_length_b                   24.090(3)
_cell_length_c                   19.254(2)
_cell_measurement_reflns_used    2972
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.95
_cell_measurement_theta_min      2.71
_cell_volume                     3126.3(6)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_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 1000 CCD area-detector'
_diffrn_measurement_method       '\f and \w 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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11308
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.271
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         1585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0707P)^2^+2.7655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                1149
_reflns_number_total             1585
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5537.cif
_cod_data_source_block           I
_cod_original_cell_volume        3126.1(6)
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               2235310
_cod_database_fobs_code          2235310