 
data_16
  
_audit_creation_method            'SHELXL-2018/3' 
_shelx_SHELXL_version_number      '2018/3' 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety
 '0.5(C28 H34 Mg N4 O8), 0.5(C24 H30 Mg N4 O10)'
_chemical_formula_sum 
 'C26 H32 Mg N4 O9' 
_chemical_formula_weight          568.86 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 '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' 
 'Mg'  'Mg'   0.1719   0.1771 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_space_group_crystal_system       monoclinic 
_space_group_IT_number            14 
_space_group_name_H-M_alt         'P 21/n' 
_space_group_name_Hall            '-P 2yn' 
  
_shelx_space_group_comment 
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
; 
  
loop_ 
 _space_group_symop_operation_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    7.5519(4) 
_cell_length_b                    8.6190(2) 
_cell_length_c                    22.3086(9) 
_cell_angle_alpha                 90 
_cell_angle_beta                  98.225(4) 
_cell_angle_gamma                 90 
_cell_volume                      1437.13(10) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     1324 
_cell_measurement_theta_min       5.9530 
_cell_measurement_theta_max       72.1130 
  
_exptl_crystal_description        tablets 
_exptl_crystal_colour             Colourless 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     1.315 
_exptl_crystal_F_000              600 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.347 
_exptl_crystal_size_mid           0.075 
_exptl_crystal_size_min           0.051 
_exptl_absorpt_coefficient_mu     1.029 
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    analytical 
_exptl_absorpt_correction_T_min   0.834 
_exptl_absorpt_correction_T_max   0.953 
_exptl_absorpt_process_details     
; 
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
; 
_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      1.54184 
_diffrn_radiation_type            CuK\a 
_diffrn_source                    'Enhance Ultra (Cu) X-ray Source' 
_diffrn_measurement_device_type   'Agilent Xcalibur PX Ultra A' 
_diffrn_measurement_method        'omega scans' 
_diffrn_detector_area_resol_mean  10.4115 
_diffrn_reflns_number             4271 
_diffrn_reflns_av_unetI/netI      0.0551 
_diffrn_reflns_av_R_equivalents   0.0317 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -7 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -27 
_diffrn_reflns_limit_l_max        24 
_diffrn_reflns_theta_min          4.004 
_diffrn_reflns_theta_max          73.608 
_diffrn_reflns_theta_full         67.684 
_diffrn_measured_fraction_theta_max   0.948 
_diffrn_measured_fraction_theta_full  0.983 
_diffrn_reflns_Laue_measured_fraction_max    0.948 
_diffrn_reflns_Laue_measured_fraction_full   0.983 
_diffrn_reflns_point_group_measured_fraction_max   0.948 
_diffrn_reflns_point_group_measured_fraction_full  0.983 
_reflns_number_total              2756 
_reflns_number_gt                 1896 
_reflns_threshold_expression      'I > 2σ(I)' 
_reflns_Friedel_coverage          0.000 
_reflns_Friedel_fraction_max      . 
_reflns_Friedel_fraction_full     . 
  
_reflns_special_details 
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
; 
  
_computing_data_collection        'CrysAlisPro, Rigaku OD' 
_computing_cell_refinement        'CrysAlisPro, Rigaku OD' 
_computing_data_reduction         'CrysAlisPro, Rigaku OD' 
_computing_structure_solution     'SHELXS-2014 (Sheldrick, 2017)' 
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'CIFTAB-2014 (Sheldrick, 2017)' 
_refine_special_details           ? 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.1222P)²+0.1504P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      ? 
_atom_sites_solution_secondary    ? 
_atom_sites_solution_hydrogens    mixed 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        . 
_refine_ls_number_reflns          2756 
_refine_ls_number_parameters      212 
_refine_ls_number_restraints      17 
_refine_ls_R_factor_all           0.0922 
_refine_ls_R_factor_gt            0.0673 
_refine_ls_wR_factor_ref          0.2249 
_refine_ls_wR_factor_gt           0.1834 
_refine_ls_goodness_of_fit_ref    1.055 
_refine_ls_restrained_S_all       1.065 
_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_site_symmetry_order 
 _atom_site_calc_flag 
 _atom_site_refinement_flags_posn 
 _atom_site_refinement_flags_adp 
 _atom_site_refinement_flags_occupancy 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Mg1 Mg 0.500000 0.500000 0.500000 0.0704(5) Uani 1 2 d S . P B . 
N1 N 0.2474(3) 1.0574(2) 0.48295(12) 0.0541(6) Uani 1 1 d . . . . . 
N2 N 0.2820(3) 0.9443(2) 0.52715(12) 0.0532(6) Uani 1 1 d . . . . . 
C3 C 0.3362(4) 0.8068(3) 0.50278(15) 0.0535(7) Uani 1 1 d . . . . . 
O3 O 0.3762(4) 0.6851(2) 0.53380(11) 0.0696(7) Uani 1 1 d . . . . . 
C4 C 0.3335(4) 0.8355(3) 0.44092(15) 0.0557(7) Uani 1 1 d . . . . . 
C5 C 0.2768(4) 0.9912(3) 0.43177(15) 0.0570(7) Uani 1 1 d . . . . . 
H5A H 0.261683 1.042056 0.393587 0.068 Uiso 1 1 calc R U . . . 
C6 C 0.2602(4) 0.9788(3) 0.58711(14) 0.0537(7) Uani 1 1 d . . . . . 
C7 C 0.1517(5) 1.1028(4) 0.59846(16) 0.0637(8) Uani 1 1 d . . . . . 
H7A H 0.092559 1.162636 0.565824 0.076 Uiso 1 1 calc R U . . . 
C8 C 0.1304(6) 1.1386(5) 0.65739(19) 0.0782(10) Uani 1 1 d . . . . . 
H8A H 0.058305 1.224889 0.664803 0.094 Uiso 1 1 calc R U . . . 
C9 C 0.2106(7) 1.0529(4) 0.70525(19) 0.0818(11) Uani 1 1 d . . . . . 
H9A H 0.192338 1.077514 0.745417 0.098 Uiso 1 1 calc R U . . . 
C10 C 0.3194(8) 0.9289(4) 0.69422(19) 0.0880(13) Uani 1 1 d . . . . . 
H10A H 0.377092 0.869429 0.727200 0.106 Uiso 1 1 calc R U . . . 
C11 C 0.3445(6) 0.8912(3) 0.63541(17) 0.0730(10) Uani 1 1 d . . . . . 
H11A H 0.418733 0.806144 0.628221 0.088 Uiso 1 1 calc R U . . . 
C12 C 0.3845(5) 0.7248(3) 0.39918(15) 0.0613(8) Uani 1 1 d D . . . . 
O12 O 0.4462(4) 0.5958(2) 0.41398(13) 0.0787(8) Uani 1 1 d . . . . . 
O13 O 0.3580(4) 0.7701(3) 0.34174(12) 0.0750(7) Uani 1 1 d D . . . . 
C14 C 0.4097(17) 0.6602(13) 0.2973(4) 0.089(4) Uani 0.646(14) 1 d D U P A 1 
H14A H 0.541244 0.646853 0.303191 0.107 Uiso 0.646(14) 1 calc R U P A 1 
H14B H 0.353721 0.557903 0.301996 0.107 Uiso 0.646(14) 1 calc R U P A 1 
C15 C 0.3485(13) 0.7236(11) 0.2377(3) 0.103(3) Uani 0.646(14) 1 d D . P A 1 
H15A H 0.218280 0.736605 0.232499 0.154 Uiso 0.646(14) 1 calc R U P A 1 
H15B H 0.380516 0.652456 0.206671 0.154 Uiso 0.646(14) 1 calc R U P A 1 
H15C H 0.405368 0.824489 0.233548 0.154 Uiso 0.646(14) 1 calc R U P A 1 
C14' C 0.425(3) 0.672(3) 0.2972(7) 0.096(7) Uiso 0.354(14) 1 d D U P A 2 
H14C H 0.486037 0.580073 0.317106 0.116 Uiso 0.354(14) 1 calc R U P A 2 
H14D H 0.510624 0.729814 0.276158 0.116 Uiso 0.354(14) 1 calc R U P A 2 
C15' C 0.270(2) 0.623(2) 0.2539(7) 0.103(5) Uiso 0.354(14) 1 d D . P A 2 
H15D H 0.189761 0.560388 0.274808 0.155 Uiso 0.354(14) 1 calc R U P A 2 
H15E H 0.310978 0.562266 0.221550 0.155 Uiso 0.354(14) 1 calc R U P A 2 
H15F H 0.205826 0.715461 0.236502 0.155 Uiso 0.354(14) 1 calc R U P A 2 
O20 O 0.2550(4) 0.3792(2) 0.48579(19) 0.0958(11) Uani 1 1 d D . . . . 
H20 H 0.248(5) 0.2755(4) 0.4892(14) 0.14(2) Uiso 1 1 d D . . . . 
C21 C 0.0823(15) 0.4255(10) 0.4480(7) 0.116(4) Uani 0.5 1 d . . P B 1 
H21A H 0.076328 0.540199 0.449292 0.139 Uiso 0.5 1 calc R U P B 1 
H21B H -0.015352 0.386405 0.469175 0.139 Uiso 0.5 1 calc R U P B 1 
C22 C 0.036(3) 0.3785(18) 0.3817(9) 0.158(6) Uani 0.5 1 d . U P B 1 
H22A H -0.082087 0.420141 0.365414 0.238 Uiso 0.5 1 calc R U P B 1 
H22B H 0.125957 0.420114 0.358531 0.238 Uiso 0.5 1 calc R U P B 1 
H22C H 0.033553 0.265104 0.378571 0.238 Uiso 0.5 1 calc R U P B 1 
O30' O -0.0638(17) 0.4684(15) 0.4036(7) 0.176(5) Uani 0.5 1 d . U P C 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 
Mg1 O3 2.0473(19) . ? 
Mg1 O3 2.0473(19) 3_666 ? 
Mg1 O12 2.075(3) . ? 
Mg1 O12 2.075(3) 3_666 ? 
Mg1 O20 2.107(3) . ? 
Mg1 O20 2.107(3) 3_666 ? 
N1 C5 1.323(4) . ? 
N1 N2 1.384(3) . ? 
N2 C3 1.390(3) . ? 
N2 C6 1.403(4) . ? 
C3 O3 1.268(4) . ? 
C3 C4 1.399(5) . ? 
C4 C5 1.415(4) . ? 
C4 C12 1.424(4) . ? 
C6 C7 1.392(4) . ? 
C6 C11 1.393(5) . ? 
C7 C8 1.382(5) . ? 
C8 C9 1.367(6) . ? 
C9 C10 1.391(6) . ? 
C10 C11 1.391(5) . ? 
C12 O12 1.233(4) . ? 
C12 O13 1.327(4) . ? 
O13 C14' 1.449(14) . ? 
O13 C14 1.463(5) . ? 
C14 C15 1.452(12) . ? 
C14' C15' 1.465(18) . ? 
O20 C21 1.502(12) . ? 
C21 C22 1.53(2) . ? 
  
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 
O3 Mg1 O3 180.0 . 3_666 ? 
O3 Mg1 O12 89.49(9) . . ? 
O3 Mg1 O12 90.51(9) 3_666 . ? 
O3 Mg1 O12 90.51(9) . 3_666 ? 
O3 Mg1 O12 89.49(9) 3_666 3_666 ? 
O12 Mg1 O12 180.0 . 3_666 ? 
O3 Mg1 O20 90.17(10) . . ? 
O3 Mg1 O20 89.83(10) 3_666 . ? 
O12 Mg1 O20 90.34(14) . . ? 
O12 Mg1 O20 89.65(14) 3_666 . ? 
O3 Mg1 O20 89.83(10) . 3_666 ? 
O3 Mg1 O20 90.17(10) 3_666 3_666 ? 
O12 Mg1 O20 89.66(14) . 3_666 ? 
O12 Mg1 O20 90.35(14) 3_666 3_666 ? 
O20 Mg1 O20 180.0 . 3_666 ? 
C5 N1 N2 105.9(2) . . ? 
N1 N2 C3 111.0(2) . . ? 
N1 N2 C6 119.6(2) . . ? 
C3 N2 C6 129.4(2) . . ? 
O3 C3 N2 123.5(3) . . ? 
O3 C3 C4 130.8(2) . . ? 
N2 C3 C4 105.7(2) . . ? 
C3 O3 Mg1 121.93(19) . . ? 
C3 C4 C5 105.7(2) . . ? 
C3 C4 C12 124.0(3) . . ? 
C5 C4 C12 130.2(3) . . ? 
N1 C5 C4 111.7(3) . . ? 
C7 C6 C11 119.4(3) . . ? 
C7 C6 N2 119.3(3) . . ? 
C11 C6 N2 121.3(3) . . ? 
C8 C7 C6 119.8(4) . . ? 
C9 C8 C7 121.6(3) . . ? 
C8 C9 C10 119.0(4) . . ? 
C9 C10 C11 120.7(4) . . ? 
C10 C11 C6 119.6(3) . . ? 
O12 C12 O13 121.5(3) . . ? 
O12 C12 C4 123.8(3) . . ? 
O13 C12 C4 114.6(3) . . ? 
C12 O12 Mg1 128.6(2) . . ? 
C12 O13 C14' 118.1(10) . . ? 
C12 O13 C14 116.4(5) . . ? 
C15 C14 O13 107.2(7) . . ? 
O13 C14' C15' 107.2(13) . . ? 
C21 O20 Mg1 128.8(4) . . ? 
O20 C21 C22 122.3(11) . . ? 
  
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
 _geom_hbond_publ_flag 
O20 H20 N1  0.9000(2) 1.885(5) 2.775(3) 170(3) 1_545 yes 
  
_refine_diff_density_max    0.676 
_refine_diff_density_min   -0.225 
_refine_diff_density_rms    0.064 
  
  
  
#===END

