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_2018968
_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          '[Cu Cl2 (C17 H11 N3)]'
_chemical_formula_moiety         'C17 H11 Cl2 Cu N3'
_chemical_formula_sum            'C17 H11 Cl2 Cu N3'
_chemical_formula_weight         391.73
_chemical_name_systematic
;
Dichlorido[2-(pyridin-2-yl)-1,10-phenanthroline]copper(II)
;
_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                103.2630(10)
_cell_angle_beta                 99.0420(10)
_cell_angle_gamma                101.3610(10)
_cell_formula_units_Z            2
_cell_length_a                   7.4523(2)
_cell_length_b                   8.8189(2)
_cell_length_c                   12.1288(3)
_cell_measurement_reflns_used    4986
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.22
_cell_measurement_theta_min      3.83
_cell_volume                     743.36(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_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      150(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker SMART6000 CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6228
_diffrn_reflns_theta_full        67.43
_diffrn_reflns_theta_max         67.43
_diffrn_reflns_theta_min         3.83
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.382
_exptl_absorpt_correction_T_max  0.6151
_exptl_absorpt_correction_T_min  0.3464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008<i>a</i>)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             394
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.351
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0451P)^2^+0.9370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0834
_reflns_number_gt                2401
_reflns_number_total             2545
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lg3106.cif
_cod_data_source_block           I
_cod_database_code               2018968
_cod_database_fobs_code          2018968