Synthesis, Structure, and Catalase-Like Activity of Dimanganese(III) Complexes of 1,5-Bis[(2-hydroxy-5-X-benzyl)(2-pyridylmethyl)amino]pentan-3-ol (X = H, Br, OCH3)
Hernán Biava; Claudia Palopoli; Carine Duhayon; Jean-Pierre Tuchagues; Sandra Signorella; Inorganic Chemistry 48 (2009) 3205–3214; doi:10.1021/ic8019793

data_4301786
_publ_contact_author_address
; 
Instituto de Quimica Rosario, CONICET, 
Universidad Nacional de Rosario, 
Suipacha 531, S2002LRK Rosario, Argentina
;
_publ_contact_author_email       signorel@infovia.com.ar
_publ_contact_author_name        'Sandra Signorella'
_publ_section_title
;
Synthesis, Structure, and Catalase-Like Activity of Dimanganese(III)
Complexes of
1,5-Bis[(2-hydroxy-5-X-benzyl)(2-pyridylmethyl)amino]pentan-3-ol (X = H,
Br, OCH3)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3205
_journal_page_last               3214
_journal_paper_doi               10.1021/ic8019793
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
(C35H39Br2Mn2N4O6),(C24H20B),0.75(CHCl3),1.5(H2O)
_chemical_formula_sum            'C59.75 H62.75 B Br2 Cl2.25 Mn2 N4 O7.5'
_chemical_formula_weight         1317.17
_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
_audit_creation_date             07-05-15
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                75.590(10)
_cell_angle_beta                 78.68(2)
_cell_angle_gamma                76.840(10)
_cell_formula_units_Z            4
_cell_length_a                   10.971(2)
_cell_length_b                   23.169(4)
_cell_length_c                   25.272(4)
_cell_measurement_reflns_used    6253
_cell_measurement_temperature    180
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     5991.6(18)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            55542
_diffrn_reflns_theta_full        26.745
_diffrn_reflns_theta_max         29.070
_diffrn_reflns_theta_min         2.720
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.91
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis RED, Oxford Diffraction Ltd.'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.46
_exptl_crystal_description       needle
_exptl_crystal_F_000             2678
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.31
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     None
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         3667
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          0.000142
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 6.52 1.66 4.88 2.16 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              31
_reflns_limit_k_min              -30
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                3667
_reflns_number_total             31298
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            ic8019793_si_001.cif
_cod_data_source_block           complex_4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C59.75 H62.75 B1 Br2 Cl2.25 Mn2 N4 O7.50'
_cod_database_code               4301786