 
data_2-282K
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C6 Mn N9, C12 N, H O' 
_chemical_formula_sum 
 'C18 H Mn N10 O' 
_chemical_formula_weight          428.23 
 
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' 
 'Mn'  'Mn'   0.3368   0.7283 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            orthorhombic 
_symmetry_space_group_name_H-M    P212121
_symmetry_space_group_name_HALL   P2ac2ab
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-x, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 
_cell_length_a                    11.6357(6) 
_cell_length_b                    12.2736(6) 
_cell_length_c                    16.6608(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      2379.4(2) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     282(2) 
_cell_measurement_reflns_used   5647
_cell_measurement_theta_min     2.4500
_cell_measurement_theta_max     30.1880
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'colorless' 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.195 
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              848 
_exptl_absorpt_coefficient_mu     0.581 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       282(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type    'XtaLAB Synergy R, DW system, HyPix' 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             12559 
_diffrn_reflns_av_R_equivalents   0.0286 
_diffrn_reflns_av_sigmaI/netI     0.0311 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          2.44 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              4128 
_reflns_number_gt                 3145 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_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)+(0.1177P)²+0.5896P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.96(7) 
_refine_ls_number_reflns          4128 
_refine_ls_number_parameters      308 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0804 
_refine_ls_R_factor_gt            0.0623 
_refine_ls_wR_factor_ref          0.1943 
_refine_ls_wR_factor_gt           0.1837 
_refine_ls_goodness_of_fit_ref    1.085 
_refine_ls_restrained_S_all       1.085 
_refine_ls_shift/su_max           0.002 
_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 
C17' C 0.5303(6) 1.1369(6) 0.9418(5) 0.183(3) Uani 0.50 1 d P . . 
Mn1 Mn 0.75167(3) 0.503039(17) 0.245196(11) 0.04959(7) Uani 1 1 d . . . 
C2 C 0.80366(18) 0.59925(14) 0.42748(10) 0.0667(6) Uani 1 1 d . . . 
N2 N 0.77593(17) 0.57801(12) 0.36503(8) 0.0737(5) Uani 1 1 d . . . 
C4 C 0.69874(17) 0.40401(13) 0.06377(9) 0.0582(5) Uani 1 1 d . . . 
N4 N 0.72821(16) 0.42867(12) 0.12510(8) 0.0710(5) Uani 1 1 d . . . 
N5 N 0.85449(16) 0.63745(13) 0.19122(10) 0.0813(5) Uani 1 1 d . . . 
N8 N 0.84471(18) 0.63226(16) 0.49589(9) 0.1033(6) Uani 1 1 d . . . 
N6 N 0.65148(15) 0.36790(13) 0.29661(10) 0.0785(5) Uani 1 1 d . . . 
C3 C 0.52174(19) 0.65081(16) 0.19767(12) 0.0755(6) Uani 1 1 d . . . 
C1 C 0.98386(18) 0.36194(15) 0.29459(13) 0.0829(7) Uani 1 1 d . . . 
N3 N 0.59468(15) 0.59910(12) 0.22033(10) 0.0741(5) Uani 1 1 d . . . 
N1 N 0.91165(15) 0.41082(13) 0.26615(11) 0.0797(5) Uani 1 1 d . . . 
C5 C 0.89479(17) 0.71974(15) 0.18538(12) 0.0750(6) Uani 1 1 d . . . 
C6 C 0.60853(18) 0.28899(17) 0.31043(12) 0.0777(6) Uani 1 1 d . . . 
N7 N 1.0711(2) 0.31615(17) 0.33023(15) 0.1652(9) Uani 1 1 d . . . 
N9 N 0.43665(19) 0.69875(18) 0.16385(14) 0.1602(8) Uani 1 1 d . . . 
N10 N 0.70245(14) 1.01057(11) 0.99860(8) 0.0640(4) Uani 1 1 d . . . 
C12 C 0.6974(4) 0.69155(19) 0.99365(17) 0.1391(13) Uani 1 1 d . . . 
C9 C 0.8709(4) 1.1331(2) 1.1788(2) 0.1786(13) Uani 1 1 d . . . 
C16 C 0.5840(3) 1.0533(3) 0.9979(3) 0.2029(17) Uani 1 1 d . . . 
C8 C 0.8228(4) 1.1169(4) 1.0977(2) 0.2019(17) Uani 1 1 d . . . 
C11' C 0.6787(6) 0.8077(5) 0.9553(3) 0.133(3) Uani 0.50 1 d P . . 
C7 C 0.7330(5) 1.0749(4) 1.0660(3) 0.1108(17) Uani 0.50 1 d P . . 
C10 C 0.7074(3) 0.8908(2) 0.9973(2) 0.1576(15) Uani 1 1 d . . . 
C13 C 0.7603(3) 1.0606(4) 0.92831(16) 0.1730(14) Uani 1 1 d . . . 
C15 C 0.8869(3) 1.1315(3) 0.8267(2) 0.1958(13) Uani 1 1 d . . . 
C14 C 0.7935(7) 1.1279(7) 0.8966(5) 0.237(3) Uani 0.50 1 d P . . 
O1 O 0.5142(4) 1.0430(5) 1.0920(3) 0.365(3) Uani 1 1 d . . . 
H1 H 0.4786 1.0028 1.1224 0.547 Uiso 1 1 calc R . . 
C18 C 0.4855(4) 0.9895(6) 0.9638(5) 0.325(4) Uani 1 1 d . . . 
C17 C 0.5362(6) 1.0374(7) 0.8827(4) 0.170(3) Uani 0.50 1 d P . . 
C7' C 0.7885(3) 1.0173(3) 1.0758(2) 0.0771(11) Uani 0.50 1 d P . . 
C11 C 0.6816(6) 0.8061(3) 1.0323(3) 0.121(2) Uani 0.50 1 d P . . 
C14' C 0.8733(5) 1.0682(5) 0.9066(4) 0.129(2) Uani 0.50 1 d P . . 
 
 
_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 
C17' C16 1.521(8) . ? 
C17' C17 1.570(10) . ? 
Mn1 N6 2.2009(16) . ? 
Mn1 N1 2.2064(17) . ? 
Mn1 N3 2.2133(17) . ? 
Mn1 N4 2.2162(14) . ? 
Mn1 N2 2.2164(14) . ? 
Mn1 N5 2.2275(17) . ? 
C2 N2 1.120(2) . ? 
C2 N8 1.300(2) . ? 
C4 N4 1.119(2) . ? 
C4 N8 1.316(2) 2_664 ? 
N5 C5 1.118(2) . ? 
N8 C4 1.316(2) 2_665 ? 
N6 C6 1.114(3) . ? 
C3 N3 1.125(3) . ? 
C3 N9 1.282(3) . ? 
C1 N1 1.136(3) . ? 
C1 N7 1.304(3) . ? 
C5 N7 1.275(3) 3_755 ? 
C6 N9 1.299(3) 3_645 ? 
N7 C5 1.275(3) 3_745 ? 
N9 C6 1.299(3) 3_655 ? 
N10 C7 1.418(5) . ? 
N10 C10 1.471(3) . ? 
N10 C16 1.475(3) . ? 
N10 C13 1.484(3) . ? 
N10 C7' 1.632(4) . ? 
C12 C11 1.557(5) . ? 
C12 C11' 1.577(7) . ? 
C9 C8 1.476(5) . ? 
C16 C18 1.500(7) . ? 
C16 C17 2.008(7) . ? 
C8 C7 1.280(7) . ? 
C8 C7' 1.337(6) . ? 
C11' C10 1.282(7) . ? 
C10 C11 1.230(5) . ? 
C13 C14 1.054(9) . ? 
C13 C14' 1.367(6) . ? 
C15 C14' 1.549(7) . ? 
C15 C14 1.593(9) . ? 
C14 C14' 1.194(10) . ? 
O1 C18 2.260(9) . ? 
 
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 
C16 C17' C17 81.0(4) . . ? 
N6 Mn1 N1 89.92(6) . . ? 
N6 Mn1 N3 92.13(6) . . ? 
N1 Mn1 N3 177.74(7) . . ? 
N6 Mn1 N4 88.61(6) . . ? 
N1 Mn1 N4 92.03(7) . . ? 
N3 Mn1 N4 87.06(6) . . ? 
N6 Mn1 N2 91.70(6) . . ? 
N1 Mn1 N2 87.88(7) . . ? 
N3 Mn1 N2 93.02(6) . . ? 
N4 Mn1 N2 179.67(7) . . ? 
N6 Mn1 N5 178.81(6) . . ? 
N1 Mn1 N5 89.47(6) . . ? 
N3 Mn1 N5 88.47(6) . . ? 
N4 Mn1 N5 90.39(6) . . ? 
N2 Mn1 N5 89.30(6) . . ? 
N2 C2 N8 172.9(2) . . ? 
C2 N2 Mn1 165.95(16) . . ? 
N4 C4 N8 173.3(2) . 2_664 ? 
C4 N4 Mn1 166.70(16) . . ? 
C5 N5 Mn1 158.39(17) . . ? 
C2 N8 C4 120.43(19) . 2_665 ? 
C6 N6 Mn1 166.74(17) . . ? 
N3 C3 N9 171.5(2) . . ? 
N1 C1 N7 173.6(2) . . ? 
C3 N3 Mn1 170.39(17) . . ? 
C1 N1 Mn1 163.94(18) . . ? 
N5 C5 N7 170.8(2) . 3_755 ? 
N6 C6 N9 172.4(2) . 3_645 ? 
C5 N7 C1 123.3(2) 3_745 . ? 
C3 N9 C6 124.0(2) . 3_655 ? 
C7 N10 C10 123.9(3) . . ? 
C7 N10 C16 92.4(3) . . ? 
C10 N10 C16 113.1(2) . . ? 
C7 N10 C13 106.3(3) . . ? 
C10 N10 C13 112.6(2) . . ? 
C16 N10 C13 105.7(2) . . ? 
C7 N10 C7' 36.3(2) . . ? 
C10 N10 C7' 92.2(2) . . ? 
C16 N10 C7' 124.2(2) . . ? 
C13 N10 C7' 108.8(2) . . ? 
C11 C12 C11' 48.3(3) . . ? 
N10 C16 C18 122.1(4) . . ? 
N10 C16 C17' 128.9(4) . . ? 
C18 C16 C17' 78.8(4) . . ? 
N10 C16 C17 103.4(3) . . ? 
C18 C16 C17 51.4(4) . . ? 
C17' C16 C17 50.6(4) . . ? 
C7 C8 C7' 43.5(3) . . ? 
C7 C8 C9 137.8(4) . . ? 
C7' C8 C9 119.1(4) . . ? 
C10 C11' C12 117.5(5) . . ? 
C8 C7 N10 139.1(5) . . ? 
C11 C10 C11' 61.4(4) . . ? 
C11 C10 N10 146.0(4) . . ? 
C11' C10 N10 142.5(4) . . ? 
C14 C13 C14' 57.4(5) . . ? 
C14 C13 N10 152.4(6) . . ? 
C14' C13 N10 132.4(4) . . ? 
C14' C15 C14 44.6(4) . . ? 
C13 C14 C14' 74.6(6) . . ? 
C13 C14 C15 129.7(8) . . ? 
C14' C14 C15 65.7(5) . . ? 
C16 C18 O1 51.5(3) . . ? 
C17' C17 C16 48.5(3) . . ? 
C8 C7' N10 116.4(3) . . ? 
C10 C11 C12 122.6(4) . . ? 
C14 C14' C13 48.0(5) . . ? 
C14 C14' C15 69.6(5) . . ? 
C13 C14' C15 111.1(4) . . ? 
 
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    0.413 
_refine_diff_density_min   -0.376 
_refine_diff_density_rms    0.076 

# start Validation Reply Form
_vrf_PLAT241_2-282K
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         C8 Check 
RESPONSE: This atom has relatively high atomic displacement parameters
 compared with the connected atoms.
;
_vrf_PLAT242_2-282K
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        N10 Check 
RESPONSE: This atom has relatively low atomic displacement parameters 
 compared with the Connected atoms.
;
_vrf_PLAT260_2-282K
;
PROBLEM: Large Average Ueq of Residue Including        O1      0.365 Check 
RESPONSE: Because of disorder, the data quality is not good.
;
_vrf_PLAT315_2-282K
;
PROBLEM: Singly Bonded Carbon Detected (H-atoms Missing).         C9 Check 
RESPONSE: Some hydrogen atoms are not added.
;
# end Validation Reply Form

