X-ray and synchrotron diffraction studies of 2-(pyridin-2-yl)-1,10-phenanthroline in the role of ligand for two copper polymorphs or hydrogen bonded with 2,2,6,6-tetramethyl-4-oxopiperidinium hexafluorophosphate
Krause, Jeanette A.; Zhao, Daoli; Chatterjee, Sayandev; Yeung, Bonnie M.; Connick, William B.; Collins, Sibrina N.; Acta Crystallographica Section C 69 (2013) 498–502; doi:10.1107/S0108270113009773

data_2018970
_publ_section_title
;
 X-ray and synchrotron diffraction studies of
 2-(pyridin-2-yl)-1,10-phenanthroline in the role of ligand for two copper
 polymorphs or hydrogen bonded with 2,2,6,6-tetramethyl-4-oxopiperidinium
 hexafluorophosphate
;
_journal_coeditor_code           LG3106
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              498
_journal_page_last               502
_journal_paper_doi               10.1107/S0108270113009773
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C9 H18 N O + , P F6 - , C17 H11 N3'
_chemical_formula_moiety         'C9 H18 N O +, P F6 -, C17 H11 N3'
_chemical_formula_sum            'C26 H29 F6 N4 O P'
_chemical_formula_weight         558.50
_chemical_name_systematic
'2,2,6,6-Tetramethyl-4-oxopiperidinium hexafluorophosphate--2-(pyridin-2-yl)-1,10-phenanthroline'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.337(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1051(10)
_cell_length_b                   21.714(3)
_cell_length_c                   14.4087(19)
_cell_measurement_reflns_used    9159
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      29.04
_cell_measurement_theta_min      2.57
_cell_volume                     2520.4(6)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction
;
SAINT (Bruker, 2003) and SADABS (Sheldrick, 2008<i>a</i>)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008<i>b</i>) and DIAMOND (Brandenburg,
2012)
;
_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      183(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker Platinum 200'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Si-<111> channel-cut crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26509
_diffrn_reflns_theta_full        29.11
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.9886
_exptl_absorpt_correction_T_min  0.9841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008<i>a</i>)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0836P)^2^+0.9747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1511
_reflns_number_gt                4268
_reflns_number_total             5080
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lg3106.cif
_cod_data_source_block           III
_cod_original_cell_volume        2520.3(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2018970
_cod_database_fobs_code          2018970