Manganese(II) complexes of scorpiand-like azamacrocycles as MnSOD mimics
Garcia-Espana, Enrique; Clares, Ma Paz; Blasco, Salvador; Inclan, Mario; Verdejo, Begona; del Castillo, Lucas; Soriano, Conxa; Domenech, Antonio; Latorre, Julio; Chem.Commun. 47 (2011) 5988–; doi:10.1039/c1cc10526d

data_7106426
_publ_section_title
;
 Manganese(II) complexes of scorpiand-like azamacrocycles as MnSOD mimics
;
_journal_coden_Cambridge         0182
_journal_name_full               Chem.Commun.
_journal_page_first              5988
_journal_paper_doi               10.1039/c1cc10526d
_journal_volume                  47
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C23 H32 Mn N6 O, 2(Cl O4)'
_chemical_formula_sum            'C23 H32 Cl2 Mn N6 O9'
_chemical_formula_weight         662.39
_chemical_name_common            '[Mn(pytren-4Q)](ClO4)2(H2O)'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.030(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7809(4)
_cell_length_b                   15.2321(6)
_cell_length_c                   10.2323(5)
_cell_measurement_reflns_used    1292
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.0457
_cell_measurement_theta_min      3.1629
_cell_volume                     1365.20(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details
;
1 omega -88.00 12.00 1.0000 300.0000
omega____ theta____ kappa____ phi______ frames
- -17.7276 -77.0000 -120.0000 100

2 omega -52.00 48.00 1.0000 300.0000
omega____ theta____ kappa____ phi______ frames
- 18.3526 -77.0000 90.0000 100

;
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.1165
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5548
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.9853
_exptl_absorpt_correction_T_min  0.9321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       leaf
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         4042
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1278
_refine_ls_R_factor_gt           0.0746
_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^)+(0.0633P)^2^+1.6398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1488
_refine_ls_wR_factor_ref         0.1806
_reflns_number_gt                2567
_reflns_number_total             4042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc10526d.txt
_cod_data_source_block           mnpytren4q
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7106426