Synthesis, structural analysis and magnetic properties of two novel doubly oxygen bridged binuclear manganese(III) and copper(II) complexes with ONO tridentate ligands
Yasemin Yahsi; Hulya Kara; Inorganica Chimica Acta 397 (2013) 110–116; doi:10.1016/j.ica.2012.11.029

data_1513178
_publ_section_title
;
 Synthesis, structural analysis and magnetic properties of two novel
 doubly oxygen bridged binuclear manganese(III) and copper(II) complexes
 with ONO tridentate ligands
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              110
_journal_page_last               116
_journal_paper_doi               10.1016/j.ica.2012.11.029
_journal_volume                  397
_journal_year                    2013
_chemical_formula_sum            'C13 H7 Cl2 Cu N O2'
_chemical_formula_weight         343.65
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 106.717(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.2082(3)
_cell_length_b                   15.8065(12)
_cell_length_c                   15.2221(12)
_cell_measurement_reflns_used    2107
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6217
_cell_measurement_theta_min      3.8885
_cell_volume                     1200.17(15)
_computing_cell_refinement
;
 CrysAlis RED, Oxford Diffraction Ltd.,
 Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
 (compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
 CrysAlis CCD, Oxford Diffraction Ltd.,
 Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
 (compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
 CrysAlis RED, Oxford Diffraction Ltd.,
 Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
 (compiled Jun 10 2008,16:49:55)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.876
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_details
;
  1 omega  -48.00    4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.0487   45.0000  240.0000    0.0000    0.0000 52

  2 omega  -11.00   44.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.1424   77.0000    0.0000    0.0000    0.0000 55

  3 omega  -50.00    2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.1424  -45.0000  240.0000    0.0000    0.0000 52

  4 omega  -35.00    3.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.1424  120.0000  134.0000    0.0000    0.0000 38

  5 omega    1.00   47.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.1424  -77.0000   60.0000    0.0000    0.0000 46

  6 omega   20.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.1424    0.0000  270.0000    0.0000    0.0000 68

;
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur3'
_diffrn_measurement_method       'omega scan'
_diffrn_orient_matrix_UB_11      0.0221030015
_diffrn_orient_matrix_UB_12      0.0019640640
_diffrn_orient_matrix_UB_13      -0.0475479354
_diffrn_orient_matrix_UB_21      0.0160110235
_diffrn_orient_matrix_UB_22      0.0444364867
_diffrn_orient_matrix_UB_23      0.0034018222
_diffrn_orient_matrix_UB_31      0.1336310413
_diffrn_orient_matrix_UB_32      -0.0056863173
_diffrn_orient_matrix_UB_33      0.0101973843
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0907
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6611
_diffrn_reflns_theta_full        28.67
_diffrn_reflns_theta_max         28.67
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    2.258
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.817
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.817
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0336P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                1567
_reflns_number_total             2703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-397-110-116-2.cif
_cod_data_source_block           yc-1
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1513178