In-house and synchrotron X-ray diffraction studies of 2-phenyl-1,10-phenanthroline, protonated salts, complexes with gold(III) and copper(II), and an orthometallation product with palladium(II)
Krause, Jeanette A.; Zhao, Daoli; Chatterjee, Sayandev; Falcon, Roland; Stoltz, Kristen; Warren, John C.; Wiswell, Sara E.; Connick, William B.; Collins, Sibrina N.; Acta Crystallographica Section C 70 (2014) 260–266; doi:10.1107/S2053229614001843

data_2019473
_publ_section_title
;
 In-house and synchrotron X-ray diffraction studies of
 2-phenyl-1,10-phenanthroline, protonated salts, complexes with gold(III)
 and copper(II), and an orthometallation product with palladium(II)
;
_journal_coeditor_code           GZ3246
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              260
_journal_page_last               266
_journal_paper_doi               10.1107/S2053229614001843
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C18 H13 N2 +, C F3 S O3 -'
_chemical_formula_moiety         'C18 H13 N2 +, C F3 S O3 -'
_chemical_formula_sum            'C19 H13 F3 N2 O3 S'
_chemical_formula_weight         406.37
_chemical_name_systematic
;
2-Phenyl-1,10-phenanthrolin-1-ium trifluoromethanesulfonate
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.848(2)
_cell_angle_beta                 95.687(2)
_cell_angle_gamma                100.439(2)
_cell_formula_units_Z            2
_cell_length_a                   7.6682(2)
_cell_length_b                   10.7446(4)
_cell_length_c                   11.1174(4)
_cell_measurement_reflns_used    4788
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.65
_cell_measurement_theta_min      4.16
_cell_volume                     860.48(5)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008<i>b</i>)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008<i>b</i>)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008<i>b</i>)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008<i>b</i>)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker SMART6000 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7396
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.87
_diffrn_reflns_theta_min         4.16
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.194
_exptl_absorpt_correction_T_max  0.8982
_exptl_absorpt_correction_T_min  0.7944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008<i>a</i>)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         2976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0628P)^2^+0.2088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                2658
_reflns_number_total             2976
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            gz3246sup1.cif
_cod_data_source_block           III
_cod_database_code               2019473
_cod_database_fobs_code          2019473