Two centrosymmetric dinuclear phenanthroline–copper(II) complexes with 3,5-dichloro-2-hydroxybenzoic acid and 5-chloro-2-hydroxybenzoic acid
Moncol, Ján; Jomová, Klaudia; Porubská, Mária; Acta Crystallographica Section C 68 (2012) m85–m89; doi:10.1107/S0108270112004532

data_2018461
_publ_section_title
;
 Two centrosymmetric dinuclear phenanthroline--copper(II) complexes with
 3,5-dichloro-2-hydroxybenzoic acid and 5-chloro-2-hydroxybenzoic acid
;
_journal_coeditor_code           SF3164
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m85
_journal_page_last               m89
_journal_paper_doi               10.1107/S0108270112004532
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[Cu2 (C7 H2 Cl2 O3)2 (C12 H8 N2)2 (C7 H4 Cl2 O3)2]'
_chemical_formula_moiety         'C52 H28 Cl8 Cu2 N4 O12'
_chemical_formula_sum            'C52 H28 Cl8 Cu2 N4 O12'
_chemical_formula_weight         1311.48
_chemical_name_systematic
;
bis(\m-3,5-dichloro-2-oxidobenzoato)-
\k^3^<i>O</i>^1^,<i>O</i>^2^:<i>O</i>^2^;
\k^3^<i>O</i>^2^:<i>O</i>^1^,<i>O</i>^2^-
bis[(3,5-dichloro-2-hydroxybenzoic acid-\k<i>O</i>^1^)(1,10-
phenanthroline-\k^2^<i>N</i>,<i>N</i>')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           SHELXL-97
_cell_angle_alpha                102.423(2)
_cell_angle_beta                 99.045(2)
_cell_angle_gamma                106.753(2)
_cell_formula_units_Z            1
_cell_length_a                   9.2295(2)
_cell_length_b                   11.6047(3)
_cell_length_c                   12.9863(3)
_cell_measurement_reflns_used    4563
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      4.17
_cell_volume                     1264.44(6)
_computing_cell_refinement       'CrysAlis RED (Agilent, 2011)'
_computing_data_collection       'CrysAlis CCD (Agilent, 2011)'
_computing_data_reduction        'CrysAlis RED (Agilent, 2011)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4340
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Gemini R CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31426
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED (Agilent, 2011)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.846
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5150
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0989P)^2^+0.1443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1599
_reflns_number_gt                3886
_reflns_number_total             5150
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            sf3164.cif
_cod_data_source_block           I
_cod_original_cell_volume        1264.44(5)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2018461