data_04src1026sq

_exptl_special_details
;
 SQUEEZE was used as there was some highly disordered solvent
 which could not be recognised or modeled.
;

 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. C. Matthews
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C58 H50 Cl4 Mn3 N26 O16'
_chemical_formula_weight          1673.86
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Mn'  'Mn'   0.3368   0.7283
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            tetragonal
_symmetry_space_group_name_H-M    P4(2)/mbc
_symmetry_space_group_name_hall   '-P 4c 2ab '
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, z'
 '-y, x, z+1/2'
 'y, -x, z+1/2'
 '-x+1/2, y+1/2, -z'
 'x+1/2, -y+1/2, -z'
 'y+1/2, x+1/2, -z+1/2'
 '-y+1/2, -x+1/2, -z+1/2'
 '-x, -y, -z'
 'x, y, -z'
 'y, -x, -z-1/2'
 '-y, x, -z-1/2'
 'x-1/2, -y-1/2, z'
 '-x-1/2, y-1/2, z'
 '-y-1/2, -x-1/2, z-1/2'
 'y-1/2, x-1/2, z-1/2'
 
_cell_length_a                    22.060(3)
_cell_length_b                    22.060(3)
_cell_length_c                    19.537(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      9507(2)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     11300
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Block
_exptl_crystal_colour             Orange
_exptl_crystal_size_max           0.22
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.11
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.169
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              3404
_exptl_absorpt_coefficient_mu     0.568
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8852
_exptl_absorpt_correction_T_max   0.9402
_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             61463
_diffrn_reflns_av_R_equivalents   0.0743
_diffrn_reflns_av_sigmaI/netI     0.0544
_diffrn_reflns_limit_h_min        -28
_diffrn_reflns_limit_h_max        28
_diffrn_reflns_limit_k_min        -27
_diffrn_reflns_limit_k_max        28
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        25
_diffrn_reflns_theta_min          2.92
_diffrn_reflns_theta_max          27.48
_reflns_number_total              5614
_reflns_number_gt                 3455
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.1555P)²+7.0254P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          5614
_refine_ls_number_parameters      282
_refine_ls_number_restraints      362
_refine_ls_R_factor_all           0.1472
_refine_ls_R_factor_gt            0.0871
_refine_ls_wR_factor_ref          0.2819
_refine_ls_wR_factor_gt           0.2465
_refine_ls_goodness_of_fit_ref    1.051
_refine_ls_restrained_S_all       1.037
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.1996(4) 0.2499(4) 0.1560(3) 0.123(3) Uani 1 1 d U . .
H1 H 0.2155 0.2833 0.1310 0.148 Uiso 1 1 calc R . .
C2 C 0.2184(5) 0.1950(5) 0.1377(4) 0.171(4) Uani 1 1 d U . .
H2 H 0.2475 0.1892 0.1025 0.206 Uiso 1 1 calc R . .
C3 C 0.1928(6) 0.1457(4) 0.1735(4) 0.178(4) Uani 1 1 d U . .
H3 H 0.2043 0.1056 0.1614 0.214 Uiso 1 1 calc R . .
C4 C 0.1503(5) 0.1544(4) 0.2272(4) 0.149(4) Uani 1 1 d U . .
H4 H 0.1318 0.1218 0.2511 0.179 Uiso 1 1 calc R . .
C5 C 0.1377(4) 0.2165(3) 0.2420(3) 0.104(2) Uani 1 1 d U . .
C6 C 0.0934(3) 0.2320(2) 0.2982(3) 0.0822(17) Uani 1 1 d U . .
C7 C 0.0628(4) 0.1903(3) 0.3372(3) 0.0946(19) Uani 1 1 d U . .
H7 H 0.0678 0.1481 0.3295 0.114 Uiso 1 1 calc R . .
C8 C 0.0246(3) 0.2114(3) 0.3882(3) 0.0837(16) Uani 1 1 d U . .
H8 H 0.0027 0.1837 0.4160 0.100 Uiso 1 1 calc R . .
C9 C 0.0186(2) 0.2718(2) 0.3981(3) 0.0627(12) Uani 1 1 d U . .
H9 H -0.0072 0.2869 0.4331 0.075 Uiso 1 1 calc R . .
C10 C 0.0503(2) 0.3110(2) 0.3569(2) 0.0513(10) Uani 1 1 d U . .
C11 C 0.04746(19) 0.37818(19) 0.36134(19) 0.0441(9) Uani 1 1 d U . .
C12 C 0.12696(19) 0.5020(2) 0.3164(2) 0.0482(10) Uani 1 1 d U . .
C13 C 0.12305(18) 0.5620(2) 0.2844(2) 0.0471(10) Uani 1 1 d U . .
C14 C 0.1670(2) 0.6052(3) 0.2865(3) 0.0781(16) Uani 1 1 d U . .
H14 H 0.2029 0.5993 0.3124 0.094 Uiso 1 1 calc R . .
C15 C 0.1579(3) 0.6579(3) 0.2500 0.090(3) Uani 1 2 d SU . .
H15 H 0.1884 0.6884 0.2500 0.108 Uiso 1 2 calc SR . .
N1 N 0.1600(3) 0.2628(2) 0.2071(2) 0.0992(19) Uani 1 1 d U . .
N2 N 0.0877(2) 0.29103(17) 0.30870(18) 0.0640(11) Uani 1 1 d U . .
N3 N 0.00339(16) 0.40371(15) 0.39758(17) 0.0510(9) Uani 1 1 d U . .
H3A H 0.0003 0.4434 0.3993 0.061 Uiso 1 1 calc R . .
H3B H -0.0227 0.3809 0.4199 0.061 Uiso 1 1 calc R . .
N4 N 0.08847(16) 0.40681(15) 0.32650(18) 0.0474(8) Uani 1 1 d U . .
N5 N 0.07753(15) 0.46896(15) 0.31644(15) 0.0411(8) Uani 1 1 d U . .
N6 N 0.18041(16) 0.4813(2) 0.33836(19) 0.0609(11) Uani 1 1 d U . .
H6A H 0.1835 0.4439 0.3538 0.073 Uiso 1 1 calc R . .
H6B H 0.2125 0.5050 0.3374 0.073 Uiso 1 1 calc R . .
N7 N 0.07110(15) 0.57110(15) 0.2500 0.0422(11) Uani 1 2 d SU . .
Mn1 Mn 0.14412(3) 0.35588(3) 0.2500 0.0658(4) Uani 1 2 d SU . .
Mn2 Mn 0.0000 0.5000 0.2500 0.0371(3) Uani 1 4 d SU . .
O21 O 0.1152(2) 0.3095(2) 0.05898(18) 0.0933(13) Uani 1 1 d DU . .
O22 O 0.2042(3) 0.3004(6) 0.0000 0.177(5) Uani 1 2 d SDU . .
O23 O 0.1497(6) 0.3935(4) 0.0000 0.192(5) Uani 1 2 d SDU . .
Cl21 Cl 0.14632(10) 0.32845(11) 0.0000 0.0771(6) Uani 1 2 d SDU . .
O31 O 0.8473(2) 0.3879(3) 0.0595(3) 0.0813(19) Uani 0.720(8) 1 d PDU . 1
O32 O 0.8162(6) 0.3051(4) 0.0000 0.100(4) Uani 0.720(8) 2 d SPDU . 1
O33 O 0.7572(3) 0.3969(3) 0.0000 0.0653(19) Uani 0.720(8) 2 d SPDU . 1
Cl31 Cl 0.81716(17) 0.37046(12) 0.0000 0.0536(9) Uani 0.720(8) 2 d SPDU . 1
O36 O 0.8918(11) 0.3398(11) 0.0558(9) 0.260(16) Uani 0.280(8) 1 d PDU . 2
O37 O 0.8033(12) 0.3188(13) 0.0000 0.155(15) Uani 0.280(8) 2 d SPDU . 2
O38 O 0.8437(11) 0.4198(6) 0.0000 0.109(8) Uani 0.280(8) 2 d SPDU . 2
Cl36 Cl 0.8555(5) 0.3566(3) 0.0000 0.063(2) Uani 0.280(8) 2 d SPDU . 2
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 C2 1.329(10) . ?
C1 N1 1.356(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.411(16) . ?
C2 H2 0.9500 . ?
C3 C4 1.420(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.427(9) . ?
C4 H4 0.9500 . ?
C5 N1 1.324(9) . ?
C5 C6 1.508(9) . ?
C6 N2 1.325(6) . ?
C6 C7 1.371(9) . ?
C7 C8 1.386(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.352(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.374(6) . ?
C9 H9 0.9500 . ?
C10 N2 1.326(6) . ?
C10 C11 1.485(6) . ?
C11 N4 1.296(5) . ?
C11 N3 1.328(5) . ?
C12 N5 1.311(5) . ?
C12 N6 1.336(6) . ?
C12 C13 1.467(6) . ?
C13 N7 1.343(5) . ?
C13 C14 1.360(7) . ?
C14 C15 1.378(7) . ?
C14 H14 0.9500 . ?
C15 C14 1.378(7) 7_455 ?
C15 H15 0.9500 . ?
N1 Mn1 2.246(5) . ?
N2 Mn1 2.217(4) . ?
N3 H3A 0.8800 . ?
N3 H3B 0.8800 . ?
N4 N5 1.406(5) . ?
N4 Mn1 2.237(3) . ?
N5 Mn2 2.254(3) . ?
N6 H6A 0.8800 . ?
N6 H6B 0.8800 . ?
N7 C13 1.343(5) 7_455 ?
N7 Mn2 2.218(5) . ?
Mn1 N2 2.217(4) 8 ?
Mn1 N4 2.237(3) 8 ?
Mn1 N1 2.246(5) 8 ?
Mn2 N7 2.218(5) 2_565 ?
Mn2 N5 2.254(3) 7_455 ?
Mn2 N5 2.254(3) 2_565 ?
Mn2 N5 2.254(3) 8 ?
O21 Cl21 1.405(4) . ?
O22 Cl21 1.419(7) . ?
O23 Cl21 1.436(8) . ?
Cl21 O21 1.405(4) 10 ?
O31 Cl31 1.394(5) . ?
O32 Cl31 1.442(9) . ?
O33 Cl31 1.446(7) . ?
Cl31 O31 1.394(5) 10 ?
O36 Cl36 1.402(11) . ?
O37 Cl36 1.421(13) . ?
O38 Cl36 1.420(12) . ?
Cl36 O36 1.402(11) 10 ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C2 C1 N1 126.1(9) . . ?
C2 C1 H1 116.9 . . ?
N1 C1 H1 116.9 . . ?
C1 C2 C3 116.4(8) . . ?
C1 C2 H2 121.8 . . ?
C3 C2 H2 121.8 . . ?
C2 C3 C4 121.7(7) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C5 114.1(9) . . ?
C3 C4 H4 122.9 . . ?
C5 C4 H4 122.9 . . ?
N1 C5 C4 124.3(7) . . ?
N1 C5 C6 116.2(5) . . ?
C4 C5 C6 119.4(8) . . ?
N2 C6 C7 121.7(5) . . ?
N2 C6 C5 113.4(6) . . ?
C7 C6 C5 124.9(5) . . ?
C6 C7 C8 118.3(5) . . ?
C6 C7 H7 120.9 . . ?
C8 C7 H7 120.9 . . ?
C9 C8 C7 119.5(6) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C10 119.2(5) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N2 C10 C9 121.5(4) . . ?
N2 C10 C11 113.6(4) . . ?
C9 C10 C11 124.9(4) . . ?
N4 C11 N3 125.8(4) . . ?
N4 C11 C10 115.2(4) . . ?
N3 C11 C10 119.0(4) . . ?
N5 C12 N6 122.9(4) . . ?
N5 C12 C13 117.0(4) . . ?
N6 C12 C13 119.9(4) . . ?
N7 C13 C14 121.2(4) . . ?
N7 C13 C12 113.4(4) . . ?
C14 C13 C12 125.3(4) . . ?
C13 C14 C15 118.2(5) . . ?
C13 C14 H14 120.9 . . ?
C15 C14 H14 120.9 . . ?
C14 C15 C14 120.8(7) 7_455 . ?
C14 C15 H15 119.6 7_455 . ?
C14 C15 H15 119.6 . . ?
C5 N1 C1 117.2(6) . . ?
C5 N1 Mn1 117.0(3) . . ?
C1 N1 Mn1 124.6(6) . . ?
C6 N2 C10 119.8(5) . . ?
C6 N2 Mn1 120.0(4) . . ?
C10 N2 Mn1 120.1(3) . . ?
C11 N3 H3A 120.0 . . ?
C11 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C11 N4 N5 115.4(3) . . ?
C11 N4 Mn1 119.3(3) . . ?
N5 N4 Mn1 119.4(2) . . ?
C12 N5 N4 113.5(3) . . ?
C12 N5 Mn2 117.5(3) . . ?
N4 N5 Mn2 120.5(2) . . ?
C12 N6 H6A 120.0 . . ?
C12 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
C13 N7 C13 120.3(5) . 7_455 ?
C13 N7 Mn2 119.8(2) . . ?
C13 N7 Mn2 119.8(2) 7_455 . ?
N2 Mn1 N2 173.2(2) 8 . ?
N2 Mn1 N4 70.74(13) 8 8 ?
N2 Mn1 N4 114.69(14) . 8 ?
N2 Mn1 N4 114.69(14) 8 . ?
N2 Mn1 N4 70.74(13) . . ?
N4 Mn1 N4 83.98(17) 8 . ?
N2 Mn1 N1 102.69(19) 8 . ?
N2 Mn1 N1 72.00(18) . . ?
N4 Mn1 N1 109.31(14) 8 . ?
N4 Mn1 N1 142.63(18) . . ?
N2 Mn1 N1 72.00(18) 8 8 ?
N2 Mn1 N1 102.69(19) . 8 ?
N4 Mn1 N1 142.63(18) 8 8 ?
N4 Mn1 N1 109.31(14) . 8 ?
N1 Mn1 N1 81.6(3) . 8 ?
N7 Mn2 N7 180.0 . 2_565 ?
N7 Mn2 N5 71.23(8) . 7_455 ?
N7 Mn2 N5 108.77(8) 2_565 7_455 ?
N7 Mn2 N5 71.23(8) . . ?
N7 Mn2 N5 108.77(8) 2_565 . ?
N5 Mn2 N5 142.45(17) 7_455 . ?
N7 Mn2 N5 108.77(8) . 2_565 ?
N7 Mn2 N5 71.23(8) 2_565 2_565 ?
N5 Mn2 N5 82.56(16) 7_455 2_565 ?
N5 Mn2 N5 109.67(15) . 2_565 ?
N7 Mn2 N5 108.77(8) . 8 ?
N7 Mn2 N5 71.23(8) 2_565 8 ?
N5 Mn2 N5 109.67(15) 7_455 8 ?
N5 Mn2 N5 82.56(16) . 8 ?
N5 Mn2 N5 142.45(17) 2_565 8 ?
O21 Cl21 O21 110.2(4) 10 . ?
O21 Cl21 O22 108.1(3) 10 . ?
O21 Cl21 O22 108.1(3) . . ?
O21 Cl21 O23 108.8(3) 10 . ?
O21 Cl21 O23 108.8(3) . . ?
O22 Cl21 O23 112.9(7) . . ?
O31 Cl31 O31 113.1(5) . 10 ?
O31 Cl31 O32 106.5(4) . . ?
O31 Cl31 O32 106.5(4) 10 . ?
O31 Cl31 O33 108.9(3) . . ?
O31 Cl31 O33 108.9(3) 10 . ?
O32 Cl31 O33 113.0(6) . . ?
O36 Cl36 O36 102(2) . 10 ?
O36 Cl36 O38 111.3(11) . . ?
O36 Cl36 O38 111.3(11) 10 . ?
O36 Cl36 O37 108.0(12) . . ?
O36 Cl36 O37 108.0(12) 10 . ?
O38 Cl36 O37 115.4(17) . . ?
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    0.663
_refine_diff_density_min   -0.552
_refine_diff_density_rms    0.093
