Structure, magnetism and catecholase activity of the first dicopper(II) complex having a single μ-alkoxo bridge
Das, Debasis; Adhikari, Sangita; Banerjee, Arnab; Nandy, Sandip; Fondo, Matilde; Sanmartin, Jesus; RSC Adv.  (2014) –; doi:10.1039/C4RA14603D

data_7219182
_publ_section_title
;
 Structure, magnetism and catecholase activity of the first dicopper(II)
 complex having a single \m-alkoxo bridge
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA14603D
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C35 H41 Cu3 N5 O10, 2(Cl O4)'
_chemical_formula_sum            'C35 H41 Cl2 Cu3 N5 O18'
_chemical_formula_weight         1081.25
_chemical_name_common            DDJS-48
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-23T13:00:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2014-12-17 deposited with the CCDC.
2014-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.215(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1962(5)
_cell_length_b                   15.1146(7)
_cell_length_c                   11.9446(5)
_cell_measurement_reflns_used    7595
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.81
_cell_measurement_theta_min      2.7
_cell_measurement_wavelength     0.71073
_cell_volume                     2015.87(15)
_computing_cell_refinement       'SAINT V8.32B integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_UB_11      -0.006636
_diffrn_orient_matrix_UB_12      -0.002115
_diffrn_orient_matrix_UB_13      0.08299
_diffrn_orient_matrix_UB_21      -0.023016
_diffrn_orient_matrix_UB_22      0.063934
_diffrn_orient_matrix_UB_23      -0.00059
_diffrn_orient_matrix_UB_31      -0.086295
_diffrn_orient_matrix_UB_32      -0.016889
_diffrn_orient_matrix_UB_33      -0.012627
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.09
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19831
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.99
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.404
_diffrn_reflns_theta_min         1.824
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    1.787
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1102
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details
;
 Flack x determined using 2366 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.034(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     578
_refine_ls_number_reflns         19831
_refine_ls_number_restraints     1497
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0644P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                16358
_reflns_number_total             19831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra14603d2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7219182
_shelx_estimated_absorpt_t_min   0.775
_shelx_estimated_absorpt_t_max   0.9