# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_hk1
_database_code_depnum_ccdc_archive 'CCDC 1842156'
_audit_update_record             
;
2018-05-08 deposited with the CCDC.
2018-06-18 downloaded from the CCDC.
;
_audit_creation_date             2018-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C13 H11 N O, C4 H3 O2'
_chemical_formula_sum            'C17 H14 N O3'
_chemical_formula_weight         280.29
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H20 N" O2'
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'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   7.43953(14)
_cell_length_b                   20.7625(4)
_cell_length_c                   8.87540(15)
_cell_angle_alpha                90
_cell_angle_beta                 102.7663(18)
_cell_angle_gamma                90
_cell_volume                     1337.03(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2604
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.5820
_cell_measurement_theta_min      4.2510
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5234
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.224
_diffrn_reflns_theta_min         4.259
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details      
'#__ type_ start__ end____ width___ exp.time_ 1 omega -39.00 16.00 1.0000 22.5000 omega____ theta____ kappa____ phi______ frames - -41.3359 38.0000 -120.0000 55 #__ type_ start__ end____ width___ exp.time_ 2 omega -111.00 -13.00 1.0000 22.5000 omega____ theta____ kappa____ phi______ frames - -41.3359 -57.0000 -60.0000 98 #__ type_ start__ end____ width___ exp.time_ 3 omega 5.00 82.00 1.0000 22.5000 omega____ theta____ kappa____ phi______ frames - 41.3359 -99.0000 150.0000 77 #__ type_ start__ end____ width___ exp.time_ 4 omega 63.00 151.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 178.0000 -90.0000 88 #__ type_ start__ end____ width___ exp.time_ 5 omega 89.00 177.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 30.0000 150.0000 88 #__ type_ start__ end____ width___ exp.time_ 6 omega 74.00 105.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 -94.0000 90.0000 31 #__ type_ start__ end____ width___ exp.time_ 7 omega 38.00 116.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 -111.0000 60.0000 78 #__ type_ start__ end____ width___ exp.time_ 8 omega 88.00 147.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 30.0000 90.0000 59 #__ type_ start__ end____ width___ exp.time_ 9 omega 41.00 94.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 -45.0000 -120.0000 53 #__ type_ start__ end____ width___ exp.time_ 10 omega 44.00 88.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 -30.0000 -180.0000 44'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.2000319000
_diffrn_orient_matrix_UB_12      0.0115159000
_diffrn_orient_matrix_UB_13      -0.0886998000
_diffrn_orient_matrix_UB_21      -0.0276983000
_diffrn_orient_matrix_UB_22      -0.0731508000
_diffrn_orient_matrix_UB_23      -0.0231984000
_diffrn_orient_matrix_UB_31      -0.0655333000
_diffrn_orient_matrix_UB_32      -0.0044227000
_diffrn_orient_matrix_UB_33      0.1526429000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2433
_reflns_number_total             2775
_reflns_odcompleteness_completeness 99.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.08
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2775
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0423
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0646P)²+0.3462P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1252
_refine_special_details          ?
_olex2_refinement_description    
;
Hydrogen H15 was located on the carboxylate of the terephthalate asymmetric unit but was placed at a 
calculate position for the refinement.
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C18(H18), C19(H19)
2.b Idealised tetrahedral OH refined as rotating group:
 O15(H15)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
C1 C 0.4041(2) 0.40451(7) 0.64371(16) 0.0310(3) Uani 1 1 d . . . . .
H1 H 0.437316 0.440719 0.709409 0.037 Uiso 1 1 calc R . . . .
C2 C 0.46386(19) 0.34453(7) 0.69535(16) 0.0307(3) Uani 1 1 d . . . . .
H2 H 0.537365 0.339430 0.796742 0.037 Uiso 1 1 calc R . . . .
N3 N 0.41932(16) 0.29247(6) 0.60349(14) 0.0294(3) Uani 1 1 d . . . . .
O3 O 0.48058(15) 0.23461(5) 0.65848(12) 0.0366(3) Uani 1 1 d . . . . .
C4 C 0.3153(2) 0.29867(7) 0.45908(16) 0.0315(3) Uani 1 1 d . . . . .
H4 H 0.285497 0.261727 0.395311 0.038 Uiso 1 1 calc R . . . .
C5 C 0.2526(2) 0.35814(7) 0.40403(16) 0.0303(3) Uani 1 1 d . . . . .
H5 H 0.179270 0.361913 0.302196 0.036 Uiso 1 1 calc R . . . .
C6 C 0.29461(19) 0.41322(7) 0.49524(16) 0.0287(3) Uani 1 1 d . . . . .
C7 C 0.2215(2) 0.47540(7) 0.43165(16) 0.0318(3) Uani 1 1 d . . . . .
H7 H 0.146903 0.475247 0.329886 0.038 Uiso 1 1 calc R . . . .
C8 C 0.2497(2) 0.53192(7) 0.50268(16) 0.0317(3) Uani 1 1 d . . . . .
H8 H 0.326290 0.532425 0.603661 0.038 Uiso 1 1 calc R . . . .
C9 C 0.1727(2) 0.59372(7) 0.43875(16) 0.0305(3) Uani 1 1 d . . . . .
C10 C 0.0665(2) 0.60011(7) 0.28779(17) 0.0340(3) Uani 1 1 d . . . . .
H10 H 0.042153 0.563447 0.222432 0.041 Uiso 1 1 calc R . . . .
C11 C -0.0028(2) 0.65964(8) 0.23384(19) 0.0381(3) Uani 1 1 d . . . . .
H11 H -0.072983 0.663612 0.130946 0.046 Uiso 1 1 calc R . . . .
C12 C 0.0288(2) 0.71355(8) 0.3281(2) 0.0405(4) Uani 1 1 d . . . . .
H12 H -0.021996 0.754038 0.291065 0.049 Uiso 1 1 calc R . . . .
C13 C 0.1350(2) 0.70792(8) 0.4770(2) 0.0414(4) Uani 1 1 d . . . . .
H13 H 0.158623 0.744759 0.541815 0.050 Uiso 1 1 calc R . . . .
C14 C 0.2066(2) 0.64883(8) 0.53098(17) 0.0350(3) Uani 1 1 d . . . . .
H14 H 0.280234 0.645585 0.632787 0.042 Uiso 1 1 calc R . . . .
O15 O 0.26925(14) 0.65501(5) 0.92583(12) 0.0324(2) Uani 1 1 d . . . . .
H15 H 0.179161 0.679804 0.896124 0.049 Uiso 1 1 calc GR . . . .
C16 C 0.21021(19) 0.59568(7) 0.92694(14) 0.0271(3) Uani 1 1 d . . . . .
O16 O 0.04867(14) 0.57988(5) 0.90007(12) 0.0330(3) Uani 1 1 d . . . . .
C17 C 0.36218(18) 0.54656(7) 0.96499(14) 0.0262(3) Uani 1 1 d . . . . .
C18 C 0.54129(19) 0.56093(7) 0.95119(15) 0.0288(3) Uani 1 1 d . . . . .
H18 H 0.569083 0.602479 0.917690 0.035 Uiso 1 1 calc R . . . .
C19 C 0.32093(19) 0.48553(7) 1.01354(15) 0.0280(3) Uani 1 1 d . . . . .
H19 H 0.199039 0.475675 1.022524 0.034 Uiso 1 1 calc R . . . .


_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 H1 0.9500 . ?
C1 C2 1.367(2) . ?
C1 C6 1.399(2) . ?
C2 H2 0.9500 . ?
C2 N3 1.3505(18) . ?
N3 O3 1.3381(15) . ?
N3 C4 1.3489(18) . ?
C4 H4 0.9500 . ?
C4 C5 1.371(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.396(2) . ?
C6 C7 1.4646(19) . ?
C7 H7 0.9500 . ?
C7 C8 1.327(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.4671(19) . ?
C9 C10 1.403(2) . ?
C9 C14 1.397(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.383(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.386(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.386(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(2) . ?
C14 H14 0.9500 . ?
O15 H15 0.8400 . ?
O15 C16 1.3086(17) . ?
C16 O16 1.2174(17) . ?
C16 C17 1.5046(19) . ?
C17 C18 1.3970(19) . ?
C17 C19 1.3942(19) . ?
C18 H18 0.9500 . ?
C18 C19 1.392(2) 3_667 ?
C19 H19 0.9500 . ?

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 H1 119.6 . . ?
C2 C1 C6 120.80(13) . . ?
C6 C1 H1 119.6 . . ?
C1 C2 H2 119.7 . . ?
N3 C2 C1 120.57(12) . . ?
N3 C2 H2 119.7 . . ?
O3 N3 C2 118.69(11) . . ?
O3 N3 C4 120.66(12) . . ?
C4 N3 C2 120.66(12) . . ?
N3 C4 H4 119.9 . . ?
N3 C4 C5 120.21(13) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.06(13) . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C7 124.47(13) . . ?
C5 C6 C1 116.70(13) . . ?
C5 C6 C7 118.82(13) . . ?
C6 C7 H7 116.9 . . ?
C8 C7 C6 126.19(13) . . ?
C8 C7 H7 116.9 . . ?
C7 C8 H8 117.2 . . ?
C7 C8 C9 125.64(13) . . ?
C9 C8 H8 117.2 . . ?
C10 C9 C8 122.78(13) . . ?
C14 C9 C8 119.03(13) . . ?
C14 C9 C10 118.19(13) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.22(14) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 H11 119.6 . . ?
C10 C11 C12 120.79(15) . . ?
C12 C11 H11 119.6 . . ?
C11 C12 H12 120.3 . . ?
C13 C12 C11 119.47(14) . . ?
C13 C12 H12 120.3 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.06(15) . . ?
C14 C13 H13 120.0 . . ?
C9 C14 H14 119.4 . . ?
C13 C14 C9 121.24(14) . . ?
C13 C14 H14 119.4 . . ?
C16 O15 H15 109.5 . . ?
O15 C16 C17 113.77(12) . . ?
O16 C16 O15 124.80(13) . . ?
O16 C16 C17 121.44(13) . . ?
C18 C17 C16 121.29(12) . . ?
C19 C17 C16 118.66(12) . . ?
C19 C17 C18 120.04(13) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 120.10(13) 3_667 . ?
C19 C18 H18 120.0 3_667 . ?
C17 C19 H19 120.1 . . ?
C18 C19 C17 119.86(13) 3_667 . ?
C18 C19 H19 120.1 3_667 . ?

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
O15 H15 O3 0.84 1.64 2.4761(14) 173.8 2_556

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_hk3rt
_database_code_depnum_ccdc_archive 'CCDC 1842157'
_audit_update_record             
;
2018-05-08 deposited with the CCDC.
2018-06-18 downloaded from the CCDC.
;
_audit_creation_date             2018-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C108 H76 Co4 N4 O20), 0.5(O)'
_chemical_formula_sum            'C27 H19 Co N O5.50'
_chemical_formula_weight         504.36
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H20 N2 O2 Co'
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'
Co Co -2.3653 3.6143 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   25.1697(4)
_cell_length_b                   7.16550(10)
_cell_length_c                   16.6823(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3008.71(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4185
_cell_measurement_temperature    296(1)
_cell_measurement_theta_max      77.8070
_cell_measurement_theta_min      5.2910
_shelx_estimated_absorpt_T_max   0.764
_shelx_estimated_absorpt_T_min   0.330
_exptl_absorpt_coefficient_mu    4.744
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8486
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.042
_diffrn_reflns_theta_min         5.303
_diffrn_ambient_temperature      296(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1417
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
'#__ type_ start__ end____ width___ exp.time_ 1 omega -83.00 38.00 1.0000 20.5000 omega____ theta____ kappa____ phi______ frames - -41.7109 19.0000 -150.0000 121 #__ type_ start__ end____ width___ exp.time_ 2 omega -4.00 83.00 1.0000 20.5000 omega____ theta____ kappa____ phi______ frames - 41.7109 -99.0000 -30.0000 87 #__ type_ start__ end____ width___ exp.time_ 3 omega 41.00 98.00 1.0000 82.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 -45.0000 30.0000 57 #__ type_ start__ end____ width___ exp.time_ 4 omega 38.00 91.00 1.0000 82.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 -30.0000 -150.0000 53 #__ type_ start__ end____ width___ exp.time_ 5 omega 38.00 91.00 1.0000 82.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 -30.0000 -60.0000 53 #__ type_ start__ end____ width___ exp.time_ 6 omega 38.00 91.00 1.0000 82.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 -30.0000 -90.0000 53 #__ type_ start__ end____ width___ exp.time_ 7 omega 31.00 109.00 1.0000 82.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 -94.0000 -180.0000 78 #__ type_ start__ end____ width___ exp.time_ 8 omega -118.00 -9.00 1.0000 20.5000 omega____ theta____ kappa____ phi______ frames - -41.7109 -77.0000 90.0000 109 #__ type_ start__ end____ width___ exp.time_ 9 omega -116.00 -17.00 1.0000 20.5000 omega____ theta____ kappa____ phi______ frames - -41.7109 -38.0000 -180.0000 99 #__ type_ start__ end____ width___ exp.time_ 10 omega 86.00 178.00 1.0000 82.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 30.0000 30.0000 92 #__ type_ start__ end____ width___ exp.time_ 11 omega 31.00 77.00 1.0000 82.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 -94.0000 -30.0000 46 #__ type_ start__ end____ width___ exp.time_ 12 omega 61.00 178.00 1.0000 82.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 15.0000 -60.0000 117'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0005481000
_diffrn_orient_matrix_UB_12      0.0919393000
_diffrn_orient_matrix_UB_13      -0.0057862000
_diffrn_orient_matrix_UB_21      -0.1616215000
_diffrn_orient_matrix_UB_22      0.0056082000
_diffrn_orient_matrix_UB_23      0.0401883000
_diffrn_orient_matrix_UB_31      0.1417618000
_diffrn_orient_matrix_UB_32      0.0067219000
_diffrn_orient_matrix_UB_33      0.0457986000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1541
_reflns_number_total             1751
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         1751
_refine_ls_number_restraints     159
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0535
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1160P)²+3.4464P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1712
_refine_special_details          ?
_olex2_refinement_description    
;
The asymmetric unit contains a cobalt with a biphenyl_4,4_dicarboxylate and a 4-styrylpyridine N-oxide ligand.
Additionally, there was a very small amount of electron density modeled as a partially occupied water molecule.
There is a lot of disorder and it is a relatively high symmetry space group.
The long axis of the diphenyl dicarboxylate sits on special position 4e with symmetry mm2 (two mirror planes and a 2 fold axis)
The carboxyl carbon (C17), the first carbon of the phenyl group (C18) and the carbon (C21) that links it to the symmetry
related phenyl of the biphenyl-4,4-dicarboxylate still sit on the mirror plane but the other carbons that make up the ring (C19 and C20) 
lie just off the mirror plane so were modeled over two positions either side of the mirror plane. Their occupancies were originally linked 
to a free variable but fixed at 50:50 for the final stages of the refinement.
The 4-styrylpyridine N-oxide also sits on special position 4e with symmetry mm2 (two mirror planes and a 2 fold axis).
Only the N-oxide oxygen (O1) still sits on the special position, the rest of the ligand lies just off the 2 fold axis and mirror planes.
The disorder was modeled by building the complete N-oxide ligand and refining behind a PART -1 instruction. Many DFIX and SIMU restraints
and AFIX 66 constraints were used to give these disordered components reasonable bonds lengths, angles and thermal parameters.
Additionally a small amount of electron density was modeled as a partially occupied water sitting on special position  8i on a mirror plane. 
It should have been refined at 0.5 occupancy to reflect its location on the special position but was refined at 0.125 occupancy 
(to reflect the amount of electron density).  No hydrogens were located for this solvent.

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C5-C8 = C9-C10
 1.4 with sigma of 0.0004
 C8-C9
 1.3 with sigma of 0.0004
3. Uiso/Uaniso restraints and constraints
N2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9: within 1.7A
with sigma of 0.002 and sigma for terminal atoms of 0.004
C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15: within 1.7A with sigma
of 0.001 and sigma for terminal atoms of 0.002
C18 \\sim C19A \\sim C20A \\sim C21 \\sim C19 \\sim C21: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: N2(0.25) C3(0.25) H3(0.25) C4(0.25) H4(0.25) C5(0.25) C6(0.25)
 H6(0.25) C7(0.25) H7(0.25) C8(0.25) H8(0.25) C9(0.25) H9(0.25) C10(0.25)
 C11(0.25) H11(0.25) C12(0.25) H12(0.25) C13(0.25) H13(0.25) C14(0.25)
 H14(0.25) C15(0.25) H15(0.25) C19(0.5) H19(0.5) C20(0.5) H20(0.5) C19A(0.5)
 H19A(0.5) C20A(0.5) H20A(0.5) O100(0.125)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C19(H19), C20(H20), C19A(H19A), C20A(H20A)
5.b Fitted hexagon refined as free rotating group:
 N2(C3,C4,C5,C6,C7), C10(C11,C12,C13,C14,C15)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Co1 Co 0.500000 0.500000 1.000000 0.0255(3) Uani 1 4 d S T P A .
O1 O 0.500000 0.750000 0.93692(18) 0.0381(7) Uani 1 4 d S T P . .
N2 N 0.5014(5) 0.747(3) 0.85732(16) 0.0506(11) Uani 0.25 1 d . U . A -1
C3 C 0.4576(4) 0.719(2) 0.8080(4) 0.0537(14) Uani 0.25 1 d G U . A -1
H3 H 0.424227 0.699568 0.830389 0.064 Uiso 0.25 1 calc R . . A -1
C4 C 0.4638(2) 0.7185(18) 0.7252(4) 0.0567(14) Uani 0.25 1 d G U . A -1
H4 H 0.434513 0.699300 0.692189 0.068 Uiso 0.25 1 calc R . . A -1
C5 C 0.5137(2) 0.747(2) 0.69172(16) 0.0600(13) Uani 0.25 1 d DG U . A -1
C6 C 0.5575(3) 0.7756(18) 0.7410(4) 0.0566(14) Uani 0.25 1 d G U . A -1
H6 H 0.590855 0.794713 0.718642 0.068 Uiso 0.25 1 calc R . . A -1
C7 C 0.5513(4) 0.776(2) 0.8238(3) 0.0526(13) Uani 0.25 1 d G U . A -1
H7 H 0.580570 0.794982 0.856842 0.063 Uiso 0.25 1 calc R . . A -1
C8 C 0.5172(3) 0.737(3) 0.60805(16) 0.0657(16) Uani 0.25 1 d D U . A -1
H8 H 0.551156 0.706390 0.590419 0.079 Uiso 0.25 1 calc R . . A -1
C9 C 0.4840(4) 0.762(4) 0.5494(2) 0.0682(18) Uani 0.25 1 d D U . A -1
H9 H 0.450132 0.791594 0.567770 0.082 Uiso 0.25 1 calc R . . A -1
C10 C 0.4860(4) 0.755(4) 0.4656(2) 0.0822(19) Uani 0.25 1 d D U . A -1
C11 C 0.4384(3) 0.781(3) 0.4250(4) 0.0826(19) Uani 0.25 1 d G U . A -1
H11 H 0.407115 0.799758 0.453656 0.099 Uiso 0.25 1 calc R . . A -1
C12 C 0.4374(3) 0.780(3) 0.3417(4) 0.0827(19) Uani 0.25 1 d G U . A -1
H12 H 0.405540 0.797410 0.314611 0.099 Uiso 0.25 1 calc R . . A -1
C13 C 0.4842(3) 0.752(4) 0.2989(2) 0.0826(19) Uani 0.25 1 d G U . A -1
H13 H 0.483523 0.751002 0.243199 0.099 Uiso 0.25 1 calc R . . A -1
C14 C 0.5318(3) 0.726(3) 0.3395(4) 0.0827(19) Uani 0.25 1 d G U . A -1
H14 H 0.563080 0.706940 0.310832 0.099 Uiso 0.25 1 calc R . . A -1
C15 C 0.5328(3) 0.727(3) 0.4228(4) 0.0826(19) Uani 0.25 1 d G U . A -1
H15 H 0.564655 0.709288 0.449877 0.099 Uiso 0.25 1 calc R . . A -1
O16 O 0.44068(8) 0.4045(3) 0.92467(13) 0.0606(6) Uani 1 1 d . . . . .
C17 C 0.42189(13) 0.250000 0.9085(2) 0.0388(8) Uani 1 2 d S T P A .
C18 C 0.37000(16) 0.250000 0.8620(3) 0.0515(9) Uani 1 2 d S TU P . .
C19 C 0.3387(3) 0.0911(11) 0.8587(5) 0.0594(13) Uani 0.5 1 d . U . A 1
H19 H 0.349506 -0.015593 0.885890 0.071 Uiso 0.5 1 calc R . . A 1
C20 C 0.2915(3) 0.0877(12) 0.8154(5) 0.070(2) Uani 0.5 1 d . . . A 1
H20 H 0.270770 -0.019775 0.813959 0.084 Uiso 0.5 1 calc R . . A 1
C19A C 0.3535(3) 0.0930(11) 0.8209(5) 0.0626(13) Uani 0.5 1 d . U . A 2
H19A H 0.373763 -0.015435 0.822249 0.075 Uiso 0.5 1 calc R . . A 2
C20A C 0.3066(3) 0.0981(13) 0.7776(5) 0.0655(14) Uani 0.5 1 d . U . A 2
H20A H 0.296271 -0.008543 0.749925 0.079 Uiso 0.5 1 calc R . . A 2
C21 C 0.27528(17) 0.250000 0.7737(3) 0.0636(12) Uani 1 2 d S TU P . .
O100 O 0.6743(19) 0.750000 0.619(3) 0.226(17) Uiso 0.25 2 d S T 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
Co1 O1 2.0776(15) . ?
Co1 O1 2.0776(15) 9_667 ?
Co1 O16 2.0680(17) 12_655 ?
Co1 O16 2.0680(17) 9_667 ?
Co1 O16 2.0680(17) 4_567 ?
Co1 O16 2.0680(17) . ?
O1 N2 1.329(4) . ?
N2 C3 1.3900 . ?
N2 C7 1.3900 . ?
C3 H3 0.9300 . ?
C3 C4 1.3900 . ?
C4 H4 0.9300 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C5 C8 1.4002 . ?
C6 H6 0.9300 . ?
C6 C7 1.3900 . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C8 C9 1.3001(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.4001 . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 H11 0.9300 . ?
C11 C12 1.3900 . ?
C12 H12 0.9300 . ?
C12 C13 1.3900 . ?
C13 H13 0.9300 . ?
C13 C14 1.3900 . ?
C14 H14 0.9300 . ?
C14 C15 1.3900 . ?
C15 H15 0.9300 . ?
O16 C17 1.234(2) . ?
C17 C18 1.519(4) . ?
C18 C19 1.386(8) 11_565 ?
C18 C19 1.386(8) . ?
C18 C19A 1.382(8) 11_565 ?
C18 C19A 1.382(8) . ?
C19 H19 0.9300 . ?
C19 C20 1.391(8) . ?
C20 H20 0.9300 . ?
C20 C21 1.415(8) . ?
C19A H19A 0.9300 . ?
C19A C20A 1.383(9) . ?
C20A H20A 0.9300 . ?
C20A C21 1.346(9) . ?
C21 C21 1.499(7) 13_556 ?

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
O1 Co1 O1 180.0 . 9_667 ?
O16 Co1 O1 88.72(8) 4_567 9_667 ?
O16 Co1 O1 88.72(8) 9_667 9_667 ?
O16 Co1 O1 91.28(8) 12_655 9_667 ?
O16 Co1 O1 91.28(8) . 9_667 ?
O16 Co1 O1 91.28(8) 9_667 . ?
O16 Co1 O1 88.72(8) . . ?
O16 Co1 O1 88.72(8) 12_655 . ?
O16 Co1 O1 91.28(8) 4_567 . ?
O16 Co1 O16 180.0 9_667 . ?
O16 Co1 O16 92.43(14) 9_667 4_567 ?
O16 Co1 O16 87.57(14) 4_567 . ?
O16 Co1 O16 87.57(14) 9_667 12_655 ?
O16 Co1 O16 92.43(14) 12_655 . ?
O16 Co1 O16 180.0 12_655 4_567 ?
Co1 O1 Co1 119.14(14) 2_665 . ?
N2 O1 Co1 119.6(10) . . ?
N2 O1 Co1 121.3(10) . 2_665 ?
O1 N2 C3 125.0(8) . . ?
O1 N2 C7 115.0(8) . . ?
C3 N2 C7 120.0 . . ?
N2 C3 H3 120.0 . . ?
N2 C3 C4 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 C8 116.8(7) . . ?
C6 C5 C8 123.2(6) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
N2 C7 H7 120.0 . . ?
C6 C7 N2 120.0 . . ?
C6 C7 H7 120.0 . . ?
C5 C8 H8 112.7 . . ?
C9 C8 C5 134.7(6) . . ?
C9 C8 H8 112.7 . . ?
C8 C9 H9 111.8 . . ?
C8 C9 C10 136.3(6) . . ?
C10 C9 H9 111.8 . . ?
C11 C10 C9 116.7(6) . . ?
C11 C10 C15 120.0 . . ?
C15 C10 C9 123.3(6) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
C10 C15 H15 120.0 . . ?
C14 C15 C10 120.0 . . ?
C14 C15 H15 120.0 . . ?
C17 O16 Co1 134.95(18) . . ?
O16 C17 O16 127.6(3) . 11_565 ?
O16 C17 C18 116.18(15) . . ?
O16 C17 C18 116.18(15) 11_565 . ?
C19 C18 C17 120.6(3) 11_565 . ?
C19 C18 C17 120.6(3) . . ?
C19 C18 C19 110.5(7) 11_565 . ?
C19A C18 C17 120.8(3) 11_565 . ?
C19A C18 C17 120.8(3) . . ?
C18 C19 H19 119.3 . . ?
C18 C19 C20 121.4(6) . . ?
C20 C19 H19 119.3 . . ?
C19 C20 H20 120.4 . . ?
C19 C20 C21 119.1(6) . . ?
C21 C20 H20 120.4 . . ?
C18 C19A H19A 120.2 . . ?
C18 C19A C20A 119.6(7) . . ?
C20A C19A H19A 120.2 . . ?
C19A C20A H20A 118.5 . . ?
C21 C20A C19A 123.1(7) . . ?
C21 C20A H20A 118.5 . . ?
C20 C21 C20 110.6(7) . 11_565 ?
C20 C21 C21 120.3(3) 11_565 13_556 ?
C20 C21 C21 120.3(4) . 13_556 ?
C20A C21 C20A 108.0(8) 11_565 . ?
C20A C21 C21 121.5(4) 11_565 13_556 ?
C20A C21 C21 121.5(4) . 13_556 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O1 N2 C3 -100.7(11) 2_665 . . . ?
Co1 O1 N2 C3 81.1(12) . . . . ?
Co1 O1 N2 C7 -98.9(8) . . . . ?
Co1 O1 N2 C7 79.4(10) 2_665 . . . ?
Co1 O16 C17 O16 -14.0(7) . . . 11_565 ?
Co1 O16 C17 C18 167.2(3) . . . . ?
O1 N2 C3 C4 -180(2) . . . . ?
O1 N2 C7 C6 179.9(18) . . . . ?
N2 C3 C4 C5 0.0 . . . . ?
C3 N2 C7 C6 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C3 C4 C5 C8 177.5(18) . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C8 C9 25(4) . . . . ?
C5 C6 C7 N2 0.0 . . . . ?
C5 C8 C9 C10 179(3) . . . . ?
C6 C5 C8 C9 -158(3) . . . . ?
C7 N2 C3 C4 0.0 . . . . ?
C8 C5 C6 C7 -177.3(19) . . . . ?
C8 C9 C10 C11 176(3) . . . . ?
C8 C9 C10 C15 -5(5) . . . . ?
C9 C10 C11 C12 179(3) . . . . ?
C9 C10 C15 C14 -179(3) . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C10 C15 C14 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C13 C14 C15 C10 0.0 . . . . ?
C15 C10 C11 C12 0.0 . . . . ?
O16 C17 C18 C19 -17.8(7) . . . 11_565 ?
O16 C17 C18 C19 17.8(7) 11_565 . . . ?
O16 C17 C18 C19 163.2(5) 11_565 . . 11_565 ?
O16 C17 C18 C19 -163.2(5) . . . . ?
O16 C17 C18 C19A 160.9(5) . . . . ?
O16 C17 C18 C19A 18.0(7) . . . 11_565 ?
O16 C17 C18 C19A -160.9(5) 11_565 . . 11_565 ?
O16 C17 C18 C19A -18.0(7) 11_565 . . . ?
C17 C18 C19 C20 -179.1(7) . . . . ?
C17 C18 C19A C20A -178.7(7) . . . . ?
C18 C19 C20 C21 0.3(14) . . . . ?
C18 C19A C20A C21 -0.6(15) . . . . ?
C19 C18 C19 C20 32.3(13) 11_565 . . . ?
C19 C20 C21 C20 -33.0(14) . . . 11_565 ?
C19 C20 C21 C21 179.6(8) . . . 13_556 ?
C19A C18 C19A C20A -31.9(13) 11_565 . . . ?
C19A C20A C21 C20A 32.5(15) . . . 11_565 ?
C19A C20A C21 C21 -180.0(8) . . . 13_556 ?

_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_hk4southamptonp_sq
_database_code_depnum_ccdc_archive 'CCDC 1842158'
_audit_update_record             
;
2018-05-08 deposited with the CCDC.
2018-06-18 downloaded from the CCDC.
;
_audit_creation_date             2018-03-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C216 H152 Mg8 N8 O40)'
_chemical_formula_sum            'C54 H38 Mg2 N2 O10'
_chemical_formula_weight         923.48
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C27 H28 Mg N O5'
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_H-M_alt        'P b c m'
_space_group_name_Hall           '-P 2c 2b'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.59874(19)
_cell_length_b                   7.14697(12)
_cell_length_c                   50.2201(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5957.64(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17368
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.2720
_cell_measurement_theta_min      5.3110
_shelx_estimated_absorpt_T_max   0.955
_shelx_estimated_absorpt_T_min   0.831
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.030
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            44127
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.402
_diffrn_reflns_theta_max         67.402
_diffrn_reflns_theta_min         2.662
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
'#__ type_ start__ end____ width___ exp.time_ 1 omega -107.00 73.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - -17.0000 40.0000 0.0000 360 #__ type_ start__ end____ width___ exp.time_ 2 omega -179.00 0.00 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 30.0000 120.0000 358 #__ type_ start__ end____ width___ exp.time_ 3 omega -162.00 -0.50 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 30.0000 -120.0000 323 #__ type_ start__ end____ width___ exp.time_ 4 omega -155.50 -18.00 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 60.0000 -60.0000 275 #__ type_ start__ end____ width___ exp.time_ 5 omega -122.00 -57.00 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 0.0000 30.0000 130 #__ type_ start__ end____ width___ exp.time_ 6 omega -156.00 -78.00 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 60.0000 30.0000 156 #__ type_ start__ end____ width___ exp.time_ 7 omega -115.00 -4.50 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 60.0000 90.0000 221 #__ type_ start__ end____ width___ exp.time_ 8 omega -142.50 -118.00 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 50.0000 60.0000 49 #__ type_ start__ end____ width___ exp.time_ 9 omega -179.00 -95.00 0.5000 28.0000 omega____ theta____ kappa____ phi______ frames - -90.0000 60.0000 -90.0000 168'
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0057083000
_diffrn_orient_matrix_UB_12      0.1548636000
_diffrn_orient_matrix_UB_13      -0.0212621000
_diffrn_orient_matrix_UB_21      0.0919363000
_diffrn_orient_matrix_UB_22      -0.0087926000
_diffrn_orient_matrix_UB_23      -0.0040237000
_diffrn_orient_matrix_UB_31      -0.0113924000
_diffrn_orient_matrix_UB_32      -0.1497014000
_diffrn_orient_matrix_UB_33      -0.0217390000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4772
_reflns_number_total             5431
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.29
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         5431
_refine_ls_number_restraints     248
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0772
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1390P)²+5.9147P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2424
_refine_ls_wR_factor_ref         0.2474
_refine_special_details          ?
_olex2_refinement_description    
;
The Squeeze routine was used to model the contribution form disordered solvent

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C8A-C9A = C5B-C8B = C8B-C9B = C9B-C10B
 1.35 with sigma of 0.02
 C9-C10C = C6-C5C = C12-C11C = C14C-C13C
 1.395 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1B \\sim N2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B \\sim
C9B \\sim C10B \\sim C11B \\sim C12B \\sim C13B \\sim C14B \\sim C15B: within
1.7A with sigma of 0.003 and sigma for terminal atoms of 0.006
O1A \\sim N2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim
C9A \\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A: within
1.7A with sigma of 0.003 and sigma for terminal atoms of 0.006
C10C \\sim C11C \\sim C12 \\sim C13C \\sim C14C: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
C3 \\sim C4C \\sim C5C \\sim C7C \\sim C8C: within 1.7A with sigma of 0.002 and
sigma for terminal atoms of 0.004
4. Others
 Sof(C4C)=Sof(H4C)=Sof(C5C)=Sof(H5C)=Sof(C8C)=Sof(H8C)=Sof(C7C)=Sof(H7C)=
 Sof(C10C)=Sof(H10C)=Sof(C13C)=Sof(H13C)=Sof(C11C)=Sof(H11C)=Sof(C14C)=
 Sof(H14C)=1-FVAR(1)
 Sof(C7)=Sof(H7)=Sof(C10)=Sof(H10)=Sof(C8)=Sof(H8)=Sof(C11)=Sof(H11)=Sof(C5)=
 Sof(H5)=Sof(C4)=Sof(H4)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=FVAR(1)
 Fixed Sof: N2B(0.5) C3B(0.5) H3B(0.5) C4B(0.5) H4B(0.5) C5B(0.5) C6B(0.5)
 H6B(0.5) C7B(0.5) H7B(0.5) C8B(0.5) H8B(0.5) C9B(0.5) H9B(0.5) C10B(0.5)
 C11B(0.5) H11B(0.5) C12B(0.5) H12B(0.5) C13B(0.5) H13B(0.5) C14B(0.5)
 H14B(0.5) C15B(0.5) H15B(0.5) N2A(0.5) C3A(0.5) H3A(0.5) C4A(0.5) H4A(0.5)
 C5A(0.5) C6A(0.5) H6A(0.5) C7A(0.5) H7A(0.5) C8A(0.5) H8A(0.5) C9A(0.5)
 H9A(0.5) C10A(0.5) C11A(0.5) H11A(0.5) C12A(0.5) H12A(0.5) C13A(0.5) H13A(0.5)
 C14A(0.5) H14A(0.5) C15A(0.5) H15A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3B(H3B), C4B(H4B), C6B(H6B), C7B(H7B), C8B(H8B), C9B(H9B), C11B(H11B),
 C12B(H12B), C13B(H13B), C14B(H14B), C15B(H15B), C3A(H3A), C4A(H4A), C6A(H6A),
 C7A(H7A), C8A(H8A), C9A(H9A), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A),
 C15A(H15A), C7(H7), C10(H10), C8(H8), C11(H11), C5(H5), C4(H4), C13(H13),
 C14(H14), C4C(H4C), C5C(H5C), C8C(H8C), C7C(H7C), C10C(H10C), C13C(H13C),
 C11C(H11C), C14C(H14C)
5.b Fitted hexagon refined as free rotating group:
 N2B(C3B,C4B,C5B,C6B,C7B), C10B(C11B,C12B,C13B,C14B,C15B), N2A(C3A,C4A,C5A,C6A,
 C7A), C10A(C11A,C12A,C13A,C14A,C15A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 1.00319(5) 1.05567(15) 0.250000 0.0221(3) Uani 1 2 d S T P B .
Mg2 Mg 0.500000 1.500000 0.500000 0.0237(3) Uani 1 2 d S T P A .
O1A O 0.93630(11) 0.8097(3) 0.250000 0.0291(5) Uani 1 2 d S TU P . .
O1B O 0.56445(12) 1.750000 0.500000 0.0313(5) Uani 1 2 d S TU P . .
N2B N 0.64363(12) 1.747(2) 0.50081(19) 0.0407(7) Uani 0.5 1 d . U . A -1
C3B C 0.6933(3) 1.7767(16) 0.47892(14) 0.0495(11) Uani 0.5 1 d G U . A -1
H3B H 0.670355 1.797902 0.461851 0.059 Uiso 0.5 1 calc R . . A -1
C4B C 0.7765(3) 1.7750(9) 0.48200(8) 0.0546(13) Uani 0.5 1 d G U . A -1
H4B H 0.810447 1.795083 0.467038 0.066 Uiso 0.5 1 calc R . . A -1
C5B C 0.81006(11) 1.7439(10) 0.50697(8) 0.0578(12) Uani 0.5 1 d DG U . A -1
C6B C 0.7604(3) 1.7145(9) 0.52886(9) 0.0543(12) Uani 0.5 1 d G U . A -1
H6B H 0.783335 1.693214 0.545922 0.065 Uiso 0.5 1 calc R . . A -1
C7B C 0.6772(2) 1.7161(16) 0.52578(15) 0.0484(11) Uani 0.5 1 d G U . A -1
H7B H 0.643242 1.696032 0.540736 0.058 Uiso 0.5 1 calc R . . A -1
C8B C 0.8978(3) 1.7419(11) 0.50987(14) 0.0677(14) Uani 0.5 1 d D U . A -1
H8B H 0.918165 1.730726 0.527469 0.081 Uiso 0.5 1 calc R . . A -1
C9B C 0.9522(3) 1.7543(12) 0.49028(15) 0.0751(14) Uani 0.5 1 d D U . A -1
H9B H 0.930495 1.764847 0.472848 0.090 Uiso 0.5 1 calc R . . A -1
C10B C 1.03993(19) 1.7539(13) 0.49174(12) 0.0815(15) Uani 0.5 1 d D U . A -1
C11B C 1.0800(3) 1.7731(11) 0.46759(10) 0.0896(17) Uani 0.5 1 d G U . A -1
H11B H 1.050215 1.783421 0.451512 0.108 Uiso 0.5 1 calc R . . A -1
C12B C 1.1637(3) 1.7773(11) 0.46698(9) 0.0916(18) Uani 0.5 1 d G U . A -1
H12B H 1.191123 1.790404 0.450478 0.110 Uiso 0.5 1 calc R . . A -1
C13B C 1.20733(19) 1.7622(12) 0.49051(11) 0.0888(18) Uani 0.5 1 d G U . A -1
H13B H 1.264538 1.765018 0.490091 0.107 Uiso 0.5 1 calc R . . A -1
C14B C 1.1672(3) 1.7430(10) 0.51466(10) 0.0891(18) Uani 0.5 1 d G U . A -1
H14B H 1.197047 1.732649 0.530739 0.107 Uiso 0.5 1 calc R . . A -1
C15B C 1.0835(3) 1.7388(11) 0.51527(10) 0.0869(17) Uani 0.5 1 d G U . A -1
H15B H 1.056139 1.725666 0.531774 0.104 Uiso 0.5 1 calc R . . A -1
O2 O 0.92146(11) 1.4603(2) 0.27938(3) 0.0423(5) Uani 1 1 d . . . . .
O1 O 0.92937(11) 1.1500(3) 0.27966(4) 0.0436(5) Uani 1 1 d . . . . .
O15 O 0.56455(10) 1.0882(2) 0.46759(3) 0.0399(5) Uani 1 1 d . . . . .
O16 O 0.58290(10) 1.3959(2) 0.47364(3) 0.0379(4) Uani 1 1 d . . . . .
N2A N 0.85715(11) 0.8158(4) 0.25103(16) 0.0368(7) Uani 0.5 1 d . U . B -1
C3A C 0.8074(3) 0.8085(8) 0.22878(12) 0.0460(11) Uani 0.5 1 d G U . B -1
H3A H 0.830328 0.800775 0.211479 0.055 Uiso 0.5 1 calc R . . B -1
C4A C 0.7242(2) 0.8125(8) 0.23185(7) 0.0507(12) Uani 0.5 1 d G U . B -1
H4A H 0.690252 0.807488 0.216643 0.061 Uiso 0.5 1 calc R . . B -1
C5A C 0.69073(11) 0.8238(5) 0.25717(7) 0.0538(11) Uani 0.5 1 d G U . B -1
C6A C 0.7404(2) 0.8311(8) 0.27941(8) 0.0510(12) Uani 0.5 1 d G U . B -1
H6A H 0.717552 0.838867 0.296717 0.061 Uiso 0.5 1 calc R . . B -1
C7A C 0.8237(2) 0.8271(8) 0.27635(13) 0.0450(11) Uani 0.5 1 d G U . B -1
H7A H 0.857628 0.832155 0.291554 0.054 Uiso 0.5 1 calc R . . B -1
C8A C 0.6033(3) 0.8244(9) 0.26045(13) 0.0614(12) Uani 0.5 1 d D U . B -1
H8A H 0.583183 0.829938 0.278144 0.074 Uiso 0.5 1 calc R . . B -1
C9A C 0.5488(3) 0.8178(9) 0.24071(14) 0.0666(13) Uani 0.5 1 d D U . B -1
H9A H 0.570222 0.811767 0.223199 0.080 Uiso 0.5 1 calc R . . B -1
C10A C 0.46077(18) 0.8186(6) 0.24252(11) 0.0728(14) Uani 0.5 1 d . U . B -1
C11A C 0.4203(2) 0.8098(9) 0.21833(9) 0.0803(16) Uani 0.5 1 d G U . B -1
H11A H 0.449822 0.803902 0.202148 0.096 Uiso 0.5 1 calc R . . B -1
C12A C 0.3366(3) 0.8096(9) 0.21781(9) 0.0825(16) Uani 0.5 1 d G U . B -1
H12A H 0.308873 0.803610 0.201271 0.099 Uiso 0.5 1 calc R . . B -1
C13A C 0.29332(18) 0.8183(7) 0.24148(11) 0.0795(16) Uani 0.5 1 d G U . B -1
H13A H 0.236098 0.818151 0.241124 0.095 Uiso 0.5 1 calc R . . B -1
C14A C 0.3338(3) 0.8271(9) 0.26567(9) 0.0796(16) Uani 0.5 1 d G U . B -1
H14A H 0.304271 0.832984 0.281853 0.096 Uiso 0.5 1 calc R . . B -1
C15A C 0.4175(3) 0.8273(9) 0.26620(9) 0.0775(16) Uani 0.5 1 d G U . B -1
H15A H 0.445220 0.833276 0.282731 0.093 Uiso 0.5 1 calc R . . B -1
C3 C 0.86222(17) 1.2985(4) 0.31508(5) 0.0435(7) Uani 1 1 d . U . . .
C2 C 0.90837(14) 1.3034(3) 0.28925(5) 0.0330(5) Uani 1 1 d . . . . .
C12 C 0.63643(17) 1.2558(4) 0.43489(5) 0.0448(7) Uani 1 1 d D U . . .
C6 C 0.7728(2) 1.2827(5) 0.36239(6) 0.0605(9) Uani 1 1 d D . . . .
C15 C 0.59062(14) 1.2463(4) 0.46085(5) 0.0353(6) Uani 1 1 d . . . . .
C9 C 0.7257(2) 1.2731(5) 0.38759(6) 0.0614(9) Uani 1 1 d D . . . .
C7 C 0.7771(4) 1.4435(7) 0.34784(11) 0.0721(17) Uani 0.826(8) 1 d . . . C 1
H7 H 0.749468 1.551948 0.353823 0.087 Uiso 0.826(8) 1 calc R . . C 1
C10 C 0.6854(4) 1.1069(8) 0.39475(11) 0.0720(18) Uani 0.826(8) 1 d . . . C 1
H10 H 0.688134 1.000563 0.383425 0.086 Uiso 0.826(8) 1 calc R . . C 1
C8 C 0.8215(4) 1.4510(6) 0.32434(11) 0.0656(16) Uani 0.826(8) 1 d . . . C 1
H8 H 0.823435 1.564682 0.314557 0.079 Uiso 0.826(8) 1 calc R . . C 1
C11 C 0.6415(4) 1.0980(7) 0.41842(9) 0.0624(14) Uani 0.826(8) 1 d . . . C 1
H11 H 0.615130 0.985186 0.423354 0.075 Uiso 0.826(8) 1 calc R . . C 1
C5 C 0.8168(4) 1.1242(6) 0.35352(10) 0.0744(18) Uani 0.826(8) 1 d . . . C 1
H5 H 0.816314 1.012229 0.363719 0.089 Uiso 0.826(8) 1 calc R . . C 1
C4 C 0.8603(4) 1.1322(6) 0.33001(9) 0.0666(16) Uani 0.826(8) 1 d . . . C 1
H4 H 0.888868 1.025199 0.323965 0.080 Uiso 0.826(8) 1 calc R . . C 1
C13 C 0.6754(4) 1.4160(9) 0.42755(12) 0.072(2) Uani 0.826(8) 1 d . . . C 1
H13 H 0.672142 1.523339 0.438651 0.086 Uiso 0.826(8) 1 calc R . . C 1
C14 C 0.7198(5) 1.4246(10) 0.40413(12) 0.081(2) Uani 0.826(8) 1 d . . . C 1
H14 H 0.746621 1.537578 0.399529 0.097 Uiso 0.826(8) 1 calc R . . C 1
C4C C 0.8169(13) 1.151(3) 0.3222(4) 0.0441(13) Uani 0.174(8) 1 d . U . C 2
H4C H 0.815557 1.046750 0.310571 0.053 Uiso 0.174(8) 1 calc R . . C 2
C5C C 0.7729(13) 1.141(2) 0.3450(3) 0.0443(17) Uani 0.174(8) 1 d D U . C 2
H5C H 0.741819 1.032459 0.348644 0.053 Uiso 0.174(8) 1 calc R . . C 2
C8C C 0.8588(13) 1.457(3) 0.3312(4) 0.0448(13) Uani 0.174(8) 1 d . U . C 2
H8C H 0.884234 1.570565 0.326207 0.054 Uiso 0.174(8) 1 calc R . . C 2
C7C C 0.8164(13) 1.439(3) 0.3548(4) 0.0457(17) Uani 0.174(8) 1 d . U . C 2
H7C H 0.817234 1.542235 0.366707 0.055 Uiso 0.174(8) 1 calc R . . C 2
C10C C 0.7215(15) 1.118(3) 0.4026(4) 0.052(5) Uani 0.174(8) 1 d D U . C 2
H10C H 0.749291 1.008780 0.396769 0.063 Uiso 0.174(8) 1 calc R . . C 2
C13C C 0.6424(14) 1.420(4) 0.4211(5) 0.046(4) Uani 0.174(8) 1 d D U . C 2
H13C H 0.617629 1.530150 0.427650 0.055 Uiso 0.174(8) 1 calc R . . C 2
C11C C 0.6799(14) 1.110(3) 0.4253(4) 0.048(4) Uani 0.174(8) 1 d D U . C 2
H11C H 0.680837 0.996650 0.435297 0.058 Uiso 0.174(8) 1 calc R . . C 2
C14C C 0.6847(16) 1.423(4) 0.3975(5) 0.053(5) Uani 0.174(8) 1 d D U . C 2
H14C H 0.685418 1.536573 0.387609 0.063 Uiso 0.174(8) 1 calc R . . 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 Mg1 3.57505(9) 4_755 ?
Mg1 Mg1 3.57504(8) 7_755 ?
Mg1 O1A 2.075(2) 7_765 ?
Mg1 O1A 2.079(2) . ?
Mg1 O2 2.0508(17) 4_745 ?
Mg1 O2 2.0508(17) 7_755 ?
Mg1 O1 2.0434(17) . ?
Mg1 O1 2.0435(17) 6_556 ?
Mg2 Mg2 3.57348(6) 3_576 ?
Mg2 Mg2 3.57348(6) 3_586 ?
Mg2 O1B 2.0825(10) 5_686 ?
Mg2 O1B 2.0825(10) . ?
Mg2 O15 2.0482(15) 7_665 ?
Mg2 O15 2.0482(15) 3_576 ?
Mg2 O16 2.0494(15) 5_686 ?
Mg2 O16 2.0494(15) . ?
O1A N2A 1.316(3) . ?
O1B N2B 1.315(3) . ?
N2B C3B 1.3900 . ?
N2B C7B 1.3900 . ?
C3B H3B 0.9500 . ?
C3B C4B 1.3900 . ?
C4B H4B 0.9500 . ?
C4B C5B 1.3900 . ?
C5B C6B 1.3900 . ?
C5B C8B 1.463(6) . ?
C6B H6B 0.9500 . ?
C6B C7B 1.3900 . ?
C7B H7B 0.9500 . ?
C8B H8B 0.9500 . ?
C8B C9B 1.339(8) . ?
C9B H9B 0.9500 . ?
C9B C10B 1.457(6) . ?
C10B C11B 1.3900 . ?
C10B C15B 1.3900 . ?
C11B H11B 0.9500 . ?
C11B C12B 1.3900 . ?
C12B H12B 0.9500 . ?
C12B C13B 1.3900 . ?
C13B H13B 0.9500 . ?
C13B C14B 1.3900 . ?
C14B H14B 0.9500 . ?
C14B C15B 1.3900 . ?
C15B H15B 0.9500 . ?
O2 C2 1.245(3) . ?
O1 C2 1.247(3) . ?
O15 C15 1.256(3) . ?
O16 C15 1.253(3) . ?
N2A C3A 1.3900 . ?
N2A C7A 1.3900 . ?
C3A H3A 0.9500 . ?
C3A C4A 1.3900 . ?
C4A H4A 0.9500 . ?
C4A C5A 1.3900 . ?
C5A C6A 1.3900 . ?
C5A C8A 1.461(6) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.3900 . ?
C7A H7A 0.9500 . ?
C8A H8A 0.9500 . ?
C8A C9A 1.343(8) . ?
C9A H9A 0.9500 . ?
C9A C10A 1.463(6) . ?
C10A C11A 1.3900 . ?
C10A C15A 1.3900 . ?
C11A H11A 0.9500 . ?
C11A C12A 1.3900 . ?
C12A H12A 0.9500 . ?
C12A C13A 1.3900 . ?
C13A H13A 0.9500 . ?
C13A C14A 1.3900 . ?
C14A H14A 0.9500 . ?
C14A C15A 1.3900 . ?
C15A H15A 0.9500 . ?
C3 C2 1.507(3) . ?
C3 C8 1.365(5) . ?
C3 C4 1.405(5) . ?
C3 C4C 1.342(18) . ?
C3 C8C 1.39(2) . ?
C12 C15 1.511(3) . ?
C12 C11 1.402(5) . ?
C12 C13 1.366(6) . ?
C12 C13C 1.36(3) . ?
C12 C11C 1.357(15) . ?
C6 C9 1.489(4) . ?
C6 C7 1.364(5) . ?
C6 C5 1.419(6) . ?
C6 C5C 1.335(14) . ?
C6 C7C 1.38(2) . ?
C9 C10 1.410(6) . ?
C9 C14 1.368(7) . ?
C9 C10C 1.345(17) . ?
C9 C14C 1.36(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.392(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.396(6) . ?
C8 H8 0.9500 . ?
C11 H11 0.9500 . ?
C5 H5 0.9500 . ?
C5 C4 1.385(5) . ?
C4 H4 0.9500 . ?
C13 H13 0.9500 . ?
C13 C14 1.390(5) . ?
C14 H14 0.9500 . ?
C4C H4C 0.9500 . ?
C4C C5C 1.36(2) . ?
C5C H5C 0.9500 . ?
C8C H8C 0.9500 . ?
C8C C7C 1.39(3) . ?
C7C H7C 0.9500 . ?
C10C H10C 0.9500 . ?
C10C C11C 1.34(3) . ?
C13C H13C 0.9500 . ?
C13C C14C 1.376(18) . ?
C11C H11C 0.9500 . ?
C14C H14C 0.9500 . ?

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
Mg1 Mg1 Mg1 176.60(6) 7_755 4_755 ?
O1A Mg1 Mg1 30.58(6) . 7_755 ?
O1A Mg1 Mg1 146.02(7) . 4_755 ?
O1A Mg1 Mg1 30.64(6) 7_765 4_755 ?
O1A Mg1 Mg1 152.75(7) 7_765 7_755 ?
O1A Mg1 O1A 176.67(8) 7_765 . ?
O2 Mg1 Mg1 110.50(6) 7_755 4_755 ?
O2 Mg1 Mg1 71.69(6) 4_745 7_755 ?
O2 Mg1 Mg1 71.69(6) 7_755 7_755 ?
O2 Mg1 Mg1 110.50(6) 4_745 4_755 ?
O2 Mg1 O1A 89.75(7) 4_745 7_765 ?
O2 Mg1 O1A 92.56(7) 7_755 . ?
O2 Mg1 O1A 89.75(7) 7_755 7_765 ?
O2 Mg1 O1A 92.56(7) 4_745 . ?
O2 Mg1 O2 92.02(11) 7_755 4_745 ?
O1 Mg1 Mg1 69.65(6) . 4_755 ?
O1 Mg1 Mg1 69.66(6) 6_556 4_755 ?
O1 Mg1 Mg1 108.19(6) . 7_755 ?
O1 Mg1 Mg1 108.19(6) 6_556 7_755 ?
O1 Mg1 O1A 90.08(7) 6_556 7_765 ?
O1 Mg1 O1A 87.64(7) 6_556 . ?
O1 Mg1 O1A 87.64(7) . . ?
O1 Mg1 O1A 90.08(7) . 7_765 ?
O1 Mg1 O2 87.19(8) . 7_755 ?
O1 Mg1 O2 87.18(8) 6_556 4_745 ?
O1 Mg1 O2 179.19(9) . 4_745 ?
O1 Mg1 O2 179.19(9) 6_556 7_755 ?
O1 Mg1 O1 93.61(12) . 6_556 ?
Mg2 Mg2 Mg2 180.0 3_586 3_576 ?
O1B Mg2 Mg2 149.09(5) . 3_576 ?
O1B Mg2 Mg2 149.09(5) 5_686 3_586 ?
O1B Mg2 Mg2 30.91(5) 5_686 3_576 ?
O1B Mg2 Mg2 30.91(5) . 3_586 ?
O1B Mg2 O1B 180.0 . 5_686 ?
O15 Mg2 Mg2 72.07(5) 3_576 3_576 ?
O15 Mg2 Mg2 107.93(5) 7_665 3_576 ?
O15 Mg2 Mg2 72.07(5) 7_665 3_586 ?
O15 Mg2 Mg2 107.93(5) 3_576 3_586 ?
O15 Mg2 O1B 89.74(6) 7_665 5_686 ?
O15 Mg2 O1B 90.26(6) 3_576 5_686 ?
O15 Mg2 O1B 90.26(6) 7_665 . ?
O15 Mg2 O1B 89.74(6) 3_576 . ?
O15 Mg2 O15 180.00(6) 7_665 3_576 ?
O15 Mg2 O16 92.88(7) 7_665 5_686 ?
O15 Mg2 O16 92.88(7) 3_576 . ?
O15 Mg2 O16 87.12(7) 7_665 . ?
O15 Mg2 O16 87.12(7) 3_576 5_686 ?
O16 Mg2 Mg2 68.70(5) 5_686 3_586 ?
O16 Mg2 Mg2 68.70(5) . 3_576 ?
O16 Mg2 Mg2 111.30(5) 5_686 3_576 ?
O16 Mg2 Mg2 111.30(5) . 3_586 ?
O16 Mg2 O1B 88.09(6) . . ?
O16 Mg2 O1B 88.09(6) 5_686 5_686 ?
O16 Mg2 O1B 91.91(6) . 5_686 ?
O16 Mg2 O1B 91.91(6) 5_686 . ?
O16 Mg2 O16 180.00(7) 5_686 . ?
Mg1 O1A Mg1 118.77(9) 7_755 . ?
N2A O1A Mg1 120.35(17) . . ?
N2A O1A Mg1 120.82(17) . 7_755 ?
Mg2 O1B Mg2 118.18(9) . 3_586 ?
N2B O1B Mg2 120.0(7) . . ?
N2B O1B Mg2 121.8(7) . 3_586 ?
O1B N2B C3B 124.5(6) . . ?
O1B N2B C7B 115.5(6) . . ?
C3B N2B C7B 120.0 . . ?
N2B C3B H3B 120.0 . . ?
N2B C3B C4B 120.0 . . ?
C4B C3B H3B 120.0 . . ?
C3B C4B H4B 120.0 . . ?
C5B C4B C3B 120.0 . . ?
C5B C4B H4B 120.0 . . ?
C4B C5B C8B 119.3(4) . . ?
C6B C5B C4B 120.0 . . ?
C6B C5B C8B 120.7(4) . . ?
C5B C6B H6B 120.0 . . ?
C5B C6B C7B 120.0 . . ?
C7B C6B H6B 120.0 . . ?
N2B C7B H7B 120.0 . . ?
C6B C7B N2B 120.0 . . ?
C6B C7B H7B 120.0 . . ?
C5B C8B H8B 116.6 . . ?
C9B C8B C5B 126.7(6) . . ?
C9B C8B H8B 116.6 . . ?
C8B C9B H9B 115.2 . . ?
C8B C9B C10B 129.6(7) . . ?
C10B C9B H9B 115.2 . . ?
C11B C10B C9B 115.7(5) . . ?
C11B C10B C15B 120.0 . . ?
C15B C10B C9B 124.3(5) . . ?
C10B C11B H11B 120.0 . . ?
C10B C11B C12B 120.0 . . ?
C12B C11B H11B 120.0 . . ?
C11B C12B H12B 120.0 . . ?
C13B C12B C11B 120.0 . . ?
C13B C12B H12B 120.0 . . ?
C12B C13B H13B 120.0 . . ?
C12B C13B C14B 120.0 . . ?
C14B C13B H13B 120.0 . . ?
C13B C14B H14B 120.0 . . ?
C13B C14B C15B 120.0 . . ?
C15B C14B H14B 120.0 . . ?
C10B C15B H15B 120.0 . . ?
C14B C15B C10B 120.0 . . ?
C14B C15B H15B 120.0 . . ?
C2 O2 Mg1 133.80(15) . 4_755 ?
C2 O1 Mg1 137.67(16) . . ?
C15 O15 Mg2 132.15(16) . 3_576 ?
C15 O16 Mg2 135.19(15) . . ?
O1A N2A C3A 124.1(5) . . ?
O1A N2A C7A 115.9(5) . . ?
C3A N2A C7A 120.0 . . ?
N2A C3A H3A 120.0 . . ?
C4A C3A N2A 120.0 . . ?
C4A C3A H3A 120.0 . . ?
C3A C4A H4A 120.0 . . ?
C3A C4A C5A 120.0 . . ?
C5A C4A H4A 120.0 . . ?
C4A C5A C6A 120.0 . . ?
C4A C5A C8A 120.1(4) . . ?
C6A C5A C8A 119.9(4) . . ?
C5A C6A H6A 120.0 . . ?
C7A C6A C5A 120.0 . . ?
C7A C6A H6A 120.0 . . ?
N2A C7A H7A 120.0 . . ?
C6A C7A N2A 120.0 . . ?
C6A C7A H7A 120.0 . . ?
C5A C8A H8A 117.1 . . ?
C9A C8A C5A 125.9(6) . . ?
C9A C8A H8A 117.1 . . ?
C8A C9A H9A 115.6 . . ?
C8A C9A C10A 128.8(6) . . ?
C10A C9A H9A 115.6 . . ?
C11A C10A C9A 115.4(4) . . ?
C11A C10A C15A 120.0 . . ?
C15A C10A C9A 124.6(4) . . ?
C10A C11A H11A 120.0 . . ?
C12A C11A C10A 120.0 . . ?
C12A C11A H11A 120.0 . . ?
C11A C12A H12A 120.0 . . ?
C11A C12A C13A 120.0 . . ?
C13A C12A H12A 120.0 . . ?
C12A C13A H13A 120.0 . . ?
C14A C13A C12A 120.0 . . ?
C14A C13A H13A 120.0 . . ?
C13A C14A H14A 120.0 . . ?
C15A C14A C13A 120.0 . . ?
C15A C14A H14A 120.0 . . ?
C10A C15A H15A 120.0 . . ?
C14A C15A C10A 120.0 . . ?
C14A C15A H15A 120.0 . . ?
C8 C3 C2 121.8(3) . . ?
C8 C3 C4 118.8(3) . . ?
C4 C3 C2 119.4(3) . . ?
C4C C3 C2 122.3(8) . . ?
C4C C3 C8C 117.3(11) . . ?
C8C C3 C2 120.1(9) . . ?
O2 C2 O1 126.1(2) . . ?
O2 C2 C3 116.9(2) . . ?
O1 C2 C3 117.0(2) . . ?
C11 C12 C15 120.2(3) . . ?
C13 C12 C15 120.6(3) . . ?
C13 C12 C11 119.1(3) . . ?
C13C C12 C15 120.9(10) . . ?
C11C C12 C15 122.5(9) . . ?
C11C C12 C13C 116.2(13) . . ?
C7 C6 C9 121.5(3) . . ?
C7 C6 C5 118.5(3) . . ?
C5 C6 C9 120.0(3) . . ?
C5C C6 C9 121.3(8) . . ?
C5C C6 C7C 115.5(11) . . ?
C7C C6 C9 123.1(9) . . ?
O15 C15 C12 116.5(2) . . ?
O16 C15 O15 126.4(2) . . ?
O16 C15 C12 117.1(2) . . ?
C10 C9 C6 120.3(3) . . ?
C14 C9 C6 121.1(4) . . ?
C14 C9 C10 118.6(4) . . ?
C10C C9 C6 122.7(10) . . ?
C10C C9 C14C 114.8(14) . . ?
C14C C9 C6 122.4(11) . . ?
C6 C7 H7 119.5 . . ?
C6 C7 C8 121.0(4) . . ?
C8 C7 H7 119.5 . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.2(4) . . ?
C11 C10 H10 119.9 . . ?
C3 C8 C7 121.3(4) . . ?
C3 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C12 C11 H11 120.1 . . ?
C10 C11 C12 119.8(4) . . ?
C10 C11 H11 120.1 . . ?
C6 C5 H5 119.9 . . ?
C4 C5 C6 120.2(4) . . ?
C4 C5 H5 119.9 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 H4 119.9 . . ?
C12 C13 H13 119.4 . . ?
C12 C13 C14 121.1(5) . . ?
C14 C13 H13 119.4 . . ?
C9 C14 C13 121.1(5) . . ?
C9 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C3 C4C H4C 117.7 . . ?
C3 C4C C5C 124.6(15) . . ?
C5C C4C H4C 117.7 . . ?
C6 C5C C4C 120.6(15) . . ?
C6 C5C H5C 119.7 . . ?
C4C C5C H5C 119.7 . . ?
C3 C8C H8C 121.8 . . ?
C7C C8C C3 116.4(18) . . ?
C7C C8C H8C 121.8 . . ?
C6 C7C C8C 125.1(18) . . ?
C6 C7C H7C 117.5 . . ?
C8C C7C H7C 117.5 . . ?
C9 C10C H10C 118.6 . . ?
C11C C10C C9 122.7(17) . . ?
C11C C10C H10C 118.6 . . ?
C12 C13C H13C 120.3 . . ?
C12 C13C C14C 119(2) . . ?
C14C C13C H13C 120.3 . . ?
C12 C11C H11C 118.5 . . ?
C10C C11C C12 123.0(16) . . ?
C10C C11C H11C 118.5 . . ?
C9 C14C C13C 124(2) . . ?
C9 C14C H14C 118.2 . . ?
C13C C14C H14C 118.2 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
