# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_2016ncs0620_sq
_database_code_depnum_ccdc_archive 'CCDC 1559284'
_audit_update_record             
;
2017-06-29 deposited with the CCDC.
2017-12-15 downloaded from the CCDC.
;
_audit_creation_date             2017-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H23 N6 O16 Sc3'
_chemical_formula_sum            'C36 H23 N6 O16 Sc3'
_chemical_formula_weight         930.48
_chemical_melting_point          ?
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'
Sc Sc 0.2519 0.3716 '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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   17.1503(11)
_cell_length_b                   17.1503(11)
_cell_length_c                   25.6245(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6527.2(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4458
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.1320
_cell_measurement_theta_min      2.1020
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    0.473
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.035
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1721
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34005
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.099
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -107.00  44.00   0.50   90.00    --  -17.00 -18.00 150.00  302
  2  ω    -53.00  53.00   0.50   90.00    --  -17.00  72.00 -60.00  212
  3  ω    -78.00 -50.00   0.50   90.00    --  -17.00  18.00 -30.00   56
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                972
_reflns_number_total             2192
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         2192
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1905
_refine_ls_R_factor_gt           0.1183
_refine_ls_restrained_S_all      1.093
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3236
_refine_ls_wR_factor_ref         0.3783
_refine_special_details          ', SQUEEZE'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2. Shared sites
{N1, C4}
3. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C4)
4. Others
 Fixed Sof: N1(0.5) H1(0.5) H3A(0.5) H3B(0.5) C4(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3A), C3(H3B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Sc1 Sc 0.53051(14) 0.26526(7) 0.250000 0.1363(12) Uani 1 4 d S T P . .
O1 O 0.666667 0.333333 0.250000 0.126(4) Uani 1 12 d S T P . .
O2 O 0.3890(7) 0.1945(4) 0.250000 0.210(4) Uani 1 4 d S T P . .
O3 O 0.5225(3) 0.3458(3) 0.30920(11) 0.1656(18) Uani 1 1 d . . . . .
N1 N 0.5945(5) 0.5484(5) 0.4518(2) 0.234(4) Uani 0.5 1 d . . . A 1
H1 H 0.631755 0.599006 0.467735 0.280 Uiso 0.5 1 calc R . . A 1
C1 C 0.5775(3) 0.4225(3) 0.3293(3) 0.152(3) Uani 1 2 d S T P . .
C2 C 0.5543(3) 0.4457(3) 0.3807(3) 0.166(3) Uani 1 2 d S T P A .
C3 C 0.6142(5) 0.5261(5) 0.4050(2) 0.208(3) Uani 1 1 d . . . . .
H3A H 0.669797 0.565958 0.388471 0.250 Uiso 0.5 1 calc R . . A 1
H3B H 0.669797 0.565958 0.388471 0.250 Uiso 0.5 1 calc R . . A 2
C4 C 0.5945(5) 0.5484(5) 0.4518(2) 0.234(4) Uani 0.5 1 d . . . A 2
C5 C 0.5128(4) 0.4872(4) 0.4728(3) 0.187(4) Uani 1 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
Sc1 Sc1 3.503(4) 3_655 ?
Sc1 Sc1 3.503(4) 14_666 ?
Sc1 O1 2.022(2) . ?
Sc1 O2 2.102(11) . ?
Sc1 O3 2.101(3) . ?
Sc1 O3 2.101(3) 20 ?
Sc1 O3 2.101(3) 12 ?
Sc1 O3 2.101(3) 16_556 ?
O3 C1 1.282(4) . ?
N1 H1 0.8800 . ?
N1 C3 1.352(7) . ?
N1 C5 1.374(7) . ?
C1 C2 1.488(10) . ?
C2 C3 1.388(7) 21_665 ?
C2 C3 1.388(7) . ?
C3 H3A 0.9500 . ?
C3 H3B 0.9500 . ?
C3 C4 1.352(7) . ?
C4 C5 1.374(7) . ?
C5 C5 1.586(15) 13_666 ?

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
Sc1 Sc1 Sc1 60.0 14_666 3_655 ?
O1 Sc1 Sc1 30.000(1) . 3_655 ?
O1 Sc1 Sc1 30.000(1) . 14_666 ?
O1 Sc1 O2 180.00(13) . . ?
O1 Sc1 O3 93.23(14) . 20 ?
O1 Sc1 O3 93.23(14) . 16_556 ?
O1 Sc1 O3 93.23(14) . . ?
O1 Sc1 O3 93.23(14) . 12 ?
O2 Sc1 Sc1 150.0 . 14_666 ?
O2 Sc1 Sc1 150.0 . 3_655 ?
O3 Sc1 Sc1 72.78(14) 16_556 14_666 ?
O3 Sc1 Sc1 113.18(13) . 3_655 ?
O3 Sc1 Sc1 113.18(13) 20 14_666 ?
O3 Sc1 Sc1 72.78(14) 20 3_655 ?
O3 Sc1 Sc1 113.18(13) 12 14_666 ?
O3 Sc1 Sc1 72.78(14) 12 3_655 ?
O3 Sc1 Sc1 72.78(14) . 14_666 ?
O3 Sc1 Sc1 113.18(13) 16_556 3_655 ?
O3 Sc1 O2 86.77(14) 16_556 . ?
O3 Sc1 O2 86.77(14) . . ?
O3 Sc1 O2 86.77(14) 20 . ?
O3 Sc1 O2 86.77(14) 12 . ?
O3 Sc1 O3 173.5(3) . 12 ?
O3 Sc1 O3 92.4(2) 16_556 . ?
O3 Sc1 O3 87.2(2) 16_556 12 ?
O3 Sc1 O3 173.5(3) 16_556 20 ?
O3 Sc1 O3 92.4(2) 12 20 ?
O3 Sc1 O3 87.2(2) . 20 ?
Sc1 O1 Sc1 120.000(1) 3_655 14_666 ?
Sc1 O1 Sc1 120.000(1) . 14_666 ?
Sc1 O1 Sc1 120.0 3_655 . ?
C1 O3 Sc1 135.1(5) . . ?
C3 N1 H1 122.1 . . ?
C3 N1 C5 115.9(7) . . ?
C5 N1 H1 122.1 . . ?
O3 C1 O3 123.4(7) . 21_665 ?
O3 C1 C2 118.2(4) . . ?
O3 C1 C2 118.2(4) 21_665 . ?
C3 C2 C1 119.9(4) . . ?
C3 C2 C1 119.9(4) 21_665 . ?
C3 C2 C3 120.2(8) 21_665 . ?
N1 C3 C2 120.8(7) . . ?
N1 C3 H3A 119.6 . . ?
C2 C3 H3A 119.6 . . ?
C2 C3 H3B 119.6 . . ?
C4 C3 C2 120.8(7) . . ?
C4 C3 H3B 119.6 . . ?
C3 C4 C5 115.9(7) . . ?
N1 C5 N1 126.3(7) . 21_665 ?
N1 C5 C5 116.8(4) 21_665 13_666 ?
N1 C5 C5 116.8(4) . 13_666 ?
C4 C5 N1 126.3(7) . 21_665 ?
C4 C5 C5 116.8(4) . 13_666 ?

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
Sc1 O3 C1 O3 11.8(13) . . . 21_665 ?
Sc1 O3 C1 C2 -162.9(5) . . . . ?
O3 C1 C2 C3 176.6(8) . . . . ?
O3 C1 C2 C3 -1.7(13) . . . 21_665 ?
O3 C1 C2 C3 1.7(13) 21_665 . . . ?
O3 C1 C2 C3 -176.6(8) 21_665 . . 21_665 ?
C1 C2 C3 N1 -179.9(8) . . . . ?
C1 C2 C3 C4 -179.9(8) . . . . ?
C2 C3 C4 C5 -0.2(14) . . . . ?
C3 N1 C5 N1 2.2(18) . . . 21_665 ?
C3 N1 C5 C5 -178.8(11) . . . 13_666 ?
C3 C2 C3 N1 -1.6(16) 21_665 . . . ?
C3 C2 C3 C4 -1.6(16) 21_665 . . . ?
C3 C4 C5 C5 -178.8(11) . . . 13_666 ?
C5 N1 C3 C2 -0.2(14) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.438
_oxdiff_exptl_absorpt_empirical_full_min 0.381
####################################################################### 
# 
# 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_2016ncs0620r1_hklf5_sq
_database_code_depnum_ccdc_archive 'CCDC 1559285'
_audit_update_record             
;
2017-10-06 deposited with the CCDC.
2017-12-15 downloaded from the CCDC.
;
_audit_creation_date             2017-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2016/6

# start Validation Reply Form
_vrf_PLAT213_2016ncs0620r1_hklf5_sq 
;
PROBLEM: Atom N2              has ADP max/min Ratio .....        5.5 prolat
RESPONSE: The atomic displacement parameters of all the atoms of the linkers are 
elongated perpendicular to the plane of the rings, including the potential 
pivot atoms (C2/C6, C89/C12 and C14/C18) suggesting a bowing of the linker
rather than twisting. 
;
_vrf_PLAT241_2016ncs0620r1_hklf5_sq 
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O1 Check 
RESPONSE: The atomic displacement parameters of all the atoms of the linkers are 
elongated perpendicular to the plane of the rings, including the potential 
pivot atoms (C2/C6, C89/C12 and C14/C18) suggesting a bowing of the linker
rather than twisting. 
;
_vrf_PLAT242_2016ncs0620r1_hklf5_sq 
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Sc1 Check 
RESPONSE: As well as being lighter atoms than the Sc, the linker atoms coordinated
all show a high degree of vibration.
;
_vrf_PLAT250_2016ncs0620r1_hklf5_sq 
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        5.4 Note  
RESPONSE: The atomic displacement parameters of all the atoms of the linkers are 
elongated perpendicular to the plane of the rings, including the potential 
pivot atoms (C2/C6, C89/C12 and C14/C18) suggesting a bowing of the linker
rather than twisting. 
;
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H9 N3 O6 Sc'
_chemical_formula_sum            'C18 H9 N3 O6 Sc'
_chemical_formula_weight         408.24
_chemical_melting_point          ?
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'
Sc Sc 0.2519 0.3716 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_symmetry_space_group_name_H-M_alt 'C 1 2/c 1'
_cell_length_a                   8.8618(4)
_cell_length_b                   48.6247(16)
_cell_length_c                   14.5573(6)
_cell_angle_alpha                90.0
_cell_angle_beta                 102.581(4)
_cell_angle_gamma                90.0
_cell_volume                     6122.1(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    16426
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5590
_cell_measurement_theta_min      2.1940
_cell_oxdiff_angle_alpha         89.963(2)
_cell_oxdiff_angle_beta          102.566(3)
_cell_oxdiff_angle_gamma         89.988(3)
_cell_oxdiff_length_a            8.8579(4)
_cell_oxdiff_length_b            48.6325(12)
_cell_oxdiff_length_c            14.5605(4)
_cell_oxdiff_measurement_reflns_used 15738
_cell_oxdiff_volume              6122.1(3)
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    0.886
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       62
_diffrn_reflns_limit_k_min       -62
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54506
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         1.660
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00  73.00   0.50   25.00    --  -17.00  72.00 150.00  200
  2  ω    -69.00  22.00   0.50   25.00    --  -17.00 -72.00  30.00  182
  3  ω    -69.00  22.00   0.50   25.00    --  -17.00 -72.00-150.00  182
  4  ω    -84.00 -21.00   0.50   25.00    --  -17.00   0.00  30.00  126
  5  ω    -32.00 -12.00   0.50   25.00    --  -17.00  54.00   0.00   40
  6  ω    -35.00  73.00   0.50   25.00    --  -17.00  72.00-150.00  216
  7  ω    -77.00  22.00   0.50   25.00    --  -17.00 -72.00  90.00  198
  8  ω    -68.00  22.00   0.50   25.00    --  -17.00 -72.00 -90.00  180
  9  ω    -90.00  -4.00   0.50   25.00    --  -17.00   0.00  90.00  172
 10  ω    -27.00  -7.00   0.50   25.00    --  -17.00  72.00  30.00   40
 11  ω    -35.00  23.00   0.50   25.00    --  -17.00  72.00 120.00  116
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  
;
Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC10 goniometer and HG Saturn 724+ detector
;
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0170620500
_diffrn_orient_matrix_UB_12      -0.0134753500
_diffrn_orient_matrix_UB_13      -0.0133641000
_diffrn_orient_matrix_UB_21      -0.0778227000
_diffrn_orient_matrix_UB_22      -0.0039432000
_diffrn_orient_matrix_UB_23      -0.0022943000
_diffrn_orient_matrix_UB_31      -0.0195935500
_diffrn_orient_matrix_UB_32      0.0039535500
_diffrn_orient_matrix_UB_33      -0.0480291000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11018
_reflns_number_total             13433
_reflns_special_details          
;
 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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         13433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0899
_refine_ls_restrained_S_all      1.023
_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)+(0.1601P)²+8.8352P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2508
_refine_ls_wR_factor_ref         0.2704
_refine_special_details          
;
 Refined as a 2-component twin. Data processed as a 2 component twin with the second component
 rotated by 180° around [0.90 0.00 -0.45] (reciprocal) or [1.00 -0.00 -0.06] (direct). The 
twin component scales were refined to 0.5057(18) and 0.4943(18. Large solvent accessible voids 
were calculated and the electron density within the voids accounted for using SQUEEZE, volume
per cell 3349 cubic angstroms containing 1401 electrons.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5057(18)
 0.4943(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16),
 C17(H17)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Sc1 Sc 0.500000 0.37170(2) 0.250000 0.0296(2) Uani 1 2 d S T P . .
Sc2 Sc 0.000000 0.38168(2) 0.250000 0.0271(2) Uani 1 2 d S T P . .
O1 O 0.6243(4) 0.40107(8) 0.2002(4) 0.116(2) Uani 1 1 d . . . . .
O2 O 0.8543(3) 0.41269(7) 0.1828(3) 0.0984(15) Uani 1 1 d . . . . .
O3 O 0.3781(4) 0.34181(7) 0.2996(3) 0.0895(13) Uani 1 1 d . . . . .
O4 O 0.1407(4) 0.35169(9) 0.3168(4) 0.127(2) Uani 1 1 d . . . . .
O5 O -0.1108(4) 0.38172(12) 0.3566(2) 0.1105(18) Uani 1 1 d . . . . .
O6 O -0.3478(4) 0.37256(10) 0.3797(2) 0.1008(18) Uani 1 1 d . . . . .
N1 N 0.4331(5) 0.47033(15) 0.0564(7) 0.188(5) Uani 1 1 d . . . . .
N2 N 0.3799(7) 0.26998(17) 0.4441(9) 0.264(7) Uani 1 1 d . . . . .
N3 N -0.1837(7) 0.3772(2) 0.6654(3) 0.202(6) Uani 1 1 d . . . . .
C1 C 0.7135(5) 0.41646(11) 0.1717(5) 0.100(2) Uani 1 1 d . . . . .
C2 C 0.6472(6) 0.44178(12) 0.1201(6) 0.121(3) Uani 1 1 d . . . . .
C3 C 0.4938(6) 0.44779(15) 0.1071(8) 0.168(5) Uani 1 1 d . . . . .
H3 H 0.429781 0.436403 0.133083 0.201 Uiso 1 1 calc R . . . .
C4 C 0.7386(7) 0.45895(16) 0.0825(8) 0.184(6) Uani 1 1 d . . . . .
H4 H 0.842907 0.454821 0.089072 0.221 Uiso 1 1 calc R . . . .
C5 C 0.6803(6) 0.48203(15) 0.0354(8) 0.179(5) Uani 1 1 d . . . . .
H5 H 0.744161 0.493990 0.011588 0.215 Uiso 1 1 calc R . . . .
C6 C 0.5308(6) 0.48720(16) 0.0241(8) 0.164(5) Uani 1 1 d . . . . .
C7 C 0.2597(6) 0.33696(11) 0.3291(5) 0.093(2) Uani 1 1 d . . . . .
C8 C 0.2541(6) 0.31087(13) 0.3801(6) 0.127(3) Uani 1 1 d . . . . .
C9 C 0.3777(7) 0.29354(15) 0.3951(8) 0.179(5) Uani 1 1 d . . . . .
H9 H 0.463287 0.298100 0.370898 0.215 Uiso 1 1 calc R . . . .
C10 C 0.1274(8) 0.30370(17) 0.4130(9) 0.204(6) Uani 1 1 d . . . . .
H10 H 0.041854 0.315284 0.402190 0.244 Uiso 1 1 calc R . . . .
C11 C 0.1233(8) 0.27959(17) 0.4623(9) 0.212(7) Uani 1 1 d . . . . .
H11 H 0.038040 0.274876 0.486566 0.255 Uiso 1 1 calc R . . . .
C12 C 0.2489(8) 0.26312(18) 0.4737(10) 0.218(7) Uani 1 1 d . . . . .
C13 C -0.2063(6) 0.37721(15) 0.4073(3) 0.091(2) Uani 1 1 d . . . . .
C14 C -0.1423(7) 0.3782(2) 0.5098(3) 0.126(4) Uani 1 1 d . . . . .
C15 C -0.2388(8) 0.3763(2) 0.5708(4) 0.179(6) Uani 1 1 d . . . . .
H15 H -0.344552 0.374315 0.547188 0.215 Uiso 1 1 calc R . . . .
C16 C 0.0134(7) 0.3816(2) 0.5465(4) 0.160(5) Uani 1 1 d . . . . .
H16 H 0.080638 0.384142 0.506318 0.192 Uiso 1 1 calc R . . . .
C17 C 0.0695(7) 0.3812(2) 0.6412(3) 0.174(5) Uani 1 1 d . . . . .
H17 H 0.175049 0.382888 0.666179 0.208 Uiso 1 1 calc R . . . .
C18 C -0.0294(7) 0.3783(3) 0.6976(4) 0.208(7) Uani 1 1 d . . . . .


_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
Sc1 O1 2.032(3) 2_655 ?
Sc1 O1 2.032(3) . ?
Sc1 O3 2.034(3) 2_655 ?
Sc1 O3 2.034(3) . ?
Sc1 O6 2.068(3) 1_655 ?
Sc1 O6 2.068(3) 2 ?
Sc2 O2 2.085(3) 1_455 ?
Sc2 O2 2.085(3) 2_655 ?
Sc2 O4 2.024(3) 2 ?
Sc2 O4 2.024(3) . ?
Sc2 O5 2.009(3) . ?
Sc2 O5 2.009(3) 2 ?
O1 C1 1.224(5) . ?
O2 C1 1.237(6) . ?
O3 C7 1.241(6) . ?
O4 C7 1.255(6) . ?
O5 C13 1.257(6) . ?
O6 C13 1.252(6) . ?
N1 C3 1.365(6) . ?
N1 C6 1.350(7) . ?
N2 C9 1.347(6) . ?
N2 C12 1.364(7) . ?
N3 C15 1.358(7) . ?
N3 C18 1.346(8) . ?
C1 C2 1.494(5) . ?
C2 C3 1.363(8) . ?
C2 C4 1.359(8) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C4 C5 1.357(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.322(7) . ?
C6 C6 1.474(9) 5_665 ?
C7 C8 1.475(5) . ?
C8 C9 1.362(7) . ?
C8 C10 1.359(7) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.379(6) . ?
C11 H11 0.9300 . ?
C11 C12 1.352(8) . ?
C12 C12 1.486(9) 7_556 ?
C13 C14 1.478(6) . ?
C14 C15 1.364(8) . ?
C14 C16 1.377(8) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C16 C17 1.360(7) . ?
C17 H17 0.9300 . ?
C17 C18 1.332(8) . ?
C18 C18 1.501(10) 2_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 Sc1 O1 90.7(3) 2_655 . ?
O1 Sc1 O3 179.03(16) . . ?
O1 Sc1 O3 90.2(2) 2_655 . ?
O1 Sc1 O3 90.2(2) . 2_655 ?
O1 Sc1 O3 179.03(16) 2_655 2_655 ?
O1 Sc1 O6 90.88(19) . 1_655 ?
O1 Sc1 O6 87.50(17) 2_655 1_655 ?
O1 Sc1 O6 90.88(19) 2_655 2 ?
O1 Sc1 O6 87.50(17) . 2 ?
O3 Sc1 O3 88.8(2) 2_655 . ?
O3 Sc1 O6 88.94(18) 2_655 2 ?
O3 Sc1 O6 88.94(18) . 1_655 ?
O3 Sc1 O6 92.71(17) 2_655 1_655 ?
O3 Sc1 O6 92.71(17) . 2 ?
O6 Sc1 O6 177.7(3) 1_655 2 ?
O2 Sc2 O2 87.4(2) 2_655 1_455 ?
O4 Sc2 O2 179.3(2) 2 2_655 ?
O4 Sc2 O2 92.4(2) . 2_655 ?
O4 Sc2 O2 179.3(2) . 1_455 ?
O4 Sc2 O2 92.4(2) 2 1_455 ?
O4 Sc2 O4 87.9(3) 2 . ?
O5 Sc2 O2 89.6(2) . 2_655 ?
O5 Sc2 O2 90.27(18) . 1_455 ?
O5 Sc2 O2 90.27(18) 2 2_655 ?
O5 Sc2 O2 89.6(2) 2 1_455 ?
O5 Sc2 O4 91.1(2) 2 . ?
O5 Sc2 O4 89.02(19) 2 2 ?
O5 Sc2 O4 91.1(2) . 2 ?
O5 Sc2 O4 89.02(19) . . ?
O5 Sc2 O5 179.9(3) . 2 ?
C1 O1 Sc1 172.2(4) . . ?
C1 O2 Sc2 132.3(3) . 1_655 ?
C7 O3 Sc1 144.4(3) . . ?
C7 O4 Sc2 152.9(4) . . ?
C13 O5 Sc2 163.3(4) . . ?
C13 O6 Sc1 134.8(3) . 1_455 ?
C6 N1 C3 118.0(5) . . ?
C9 N2 C12 117.4(5) . . ?
C18 N3 C15 117.9(5) . . ?
O1 C1 O2 124.9(4) . . ?
O1 C1 C2 117.5(4) . . ?
O2 C1 C2 117.6(4) . . ?
C3 C2 C1 121.2(5) . . ?
C4 C2 C1 120.4(5) . . ?
C4 C2 C3 118.4(4) . . ?
N1 C3 H3 119.6 . . ?
C2 C3 N1 120.7(5) . . ?
C2 C3 H3 119.6 . . ?
C2 C4 H4 119.4 . . ?
C5 C4 C2 121.1(6) . . ?
C5 C4 H4 119.4 . . ?
C4 C5 H5 120.6 . . ?
C6 C5 C4 118.8(5) . . ?
C6 C5 H5 120.6 . . ?
N1 C6 C6 118.7(6) . 5_665 ?
C5 C6 N1 122.8(4) . . ?
C5 C6 C6 118.5(6) . 5_665 ?
O3 C7 O4 126.2(4) . . ?
O3 C7 C8 117.5(4) . . ?
O4 C7 C8 116.3(4) . . ?
C9 C8 C7 119.9(4) . . ?
C10 C8 C7 121.3(4) . . ?
C10 C8 C9 118.8(4) . . ?
N2 C9 C8 122.0(5) . . ?
N2 C9 H9 119.0 . . ?
C8 C9 H9 119.0 . . ?
C8 C10 H10 119.4 . . ?
C8 C10 C11 121.3(5) . . ?
C11 C10 H10 119.4 . . ?
C10 C11 H11 121.5 . . ?
C12 C11 C10 117.0(5) . . ?
C12 C11 H11 121.5 . . ?
N2 C12 C12 117.1(6) . 7_556 ?
C11 C12 N2 123.4(4) . . ?
C11 C12 C12 119.4(6) . 7_556 ?
O5 C13 C14 115.3(5) . . ?
O6 C13 O5 126.8(4) . . ?
O6 C13 C14 117.8(5) . . ?
C15 C14 C13 119.9(5) . . ?
C15 C14 C16 118.2(5) . . ?
C16 C14 C13 121.8(5) . . ?
N3 C15 C14 121.3(6) . . ?
N3 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C14 C16 H16 119.8 . . ?
C17 C16 C14 120.4(5) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 120.6 . . ?
C18 C17 C16 118.8(5) . . ?
C18 C17 H17 120.6 . . ?
N3 C18 C18 117.0(7) . 2_556 ?
C17 C18 N3 123.0(5) . . ?
C17 C18 C18 119.8(7) . 2_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
Sc1 O3 C7 O4 19.1(15) . . . . ?
Sc1 O3 C7 C8 -163.8(6) . . . . ?
Sc1 O6 C13 O5 -4.0(12) 1_455 . . . ?
Sc1 O6 C13 C14 174.5(5) 1_455 . . . ?
Sc2 O2 C1 O1 -0.7(13) 1_655 . . . ?
Sc2 O2 C1 C2 178.9(5) 1_655 . . . ?
Sc2 O4 C7 O3 18.1(19) . . . . ?
Sc2 O4 C7 C8 -159.0(9) . . . . ?
Sc2 O5 C13 O6 -31(2) . . . . ?
Sc2 O5 C13 C14 150.5(14) . . . . ?
O1 C1 C2 C3 1.4(14) . . . . ?
O1 C1 C2 C4 -176.6(10) . . . . ?
O2 C1 C2 C3 -178.3(9) . . . . ?
O2 C1 C2 C4 3.8(14) . . . . ?
O3 C7 C8 C9 1.7(14) . . . . ?
O3 C7 C8 C10 -178.6(10) . . . . ?
O4 C7 C8 C9 179.1(10) . . . . ?
O4 C7 C8 C10 -1.2(15) . . . . ?
O5 C13 C14 C15 173.6(9) . . . . ?
O5 C13 C14 C16 -5.2(13) . . . . ?
O6 C13 C14 C15 -5.1(13) . . . . ?
O6 C13 C14 C16 176.1(9) . . . . ?
C1 C2 C3 N1 -177.1(10) . . . . ?
C1 C2 C4 C5 180.0(11) . . . . ?
C2 C4 C5 C6 -2(2) . . . . ?
C3 N1 C6 C5 4(2) . . . . ?
C3 N1 C6 C6 -175.1(14) . . . 5_665 ?
C3 C2 C4 C5 2.0(19) . . . . ?
C4 C2 C3 N1 0.9(18) . . . . ?
C4 C5 C6 N1 -1(2) . . . . ?
C4 C5 C6 C6 177.8(14) . . . 5_665 ?
C6 N1 C3 C2 -3.5(19) . . . . ?
C7 C8 C9 N2 177.6(11) . . . . ?
C7 C8 C10 C11 -178.7(12) . . . . ?
C8 C10 C11 C12 -2(2) . . . . ?
C9 N2 C12 C11 -5(2) . . . . ?
C9 N2 C12 C12 179.0(16) . . . 7_556 ?
C9 C8 C10 C11 1(2) . . . . ?
C10 C8 C9 N2 -2(2) . . . . ?
C10 C11 C12 N2 4(2) . . . . ?
C10 C11 C12 C12 179.9(17) . . . 7_556 ?
C12 N2 C9 C8 4(2) . . . . ?
C13 C14 C15 N3 -179.9(9) . . . . ?
C13 C14 C16 C17 -177.0(9) . . . . ?
C14 C16 C17 C18 -2.0(18) . . . . ?
C15 N3 C18 C17 6(2) . . . . ?
C15 N3 C18 C18 -178.0(8) . . . 2_556 ?
C15 C14 C16 C17 4.1(17) . . . . ?
C16 C14 C15 N3 -1.1(17) . . . . ?
C16 C17 C18 N3 -3(2) . . . . ?
C16 C17 C18 C18 -178.9(8) . . . 2_556 ?
C18 N3 C15 C14 -4.0(18) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.627
_oxdiff_exptl_absorpt_empirical_full_min 0.763
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5057(18) 47822 11364 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.4943(18) 47951 11364 nmt 0.9455 0.0000 -0.1094 0.0010 -1.0000 -0.0002
-0.9693 -0.0000 -0.9454



_twin_special_details            
;
Component 2 rotated by 179.9882° 
 around [0.90 0.00 -0.45] (reciprocal) or [1.00 -0.00 -0.06] (direct)
;
####################################################################### 
# 
# 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_2016ncs0703_sq
_database_code_depnum_ccdc_archive 'CCDC 1559286'
_audit_update_record             
;
2017-10-06 deposited with the CCDC.
2017-12-15 downloaded from the CCDC.
;
_audit_creation_date             2017-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2016/6
# start Validation Reply Form
_vrf_PLAT241_2016ncs0703_sq      
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         C4 Check 
RESPONSE: The whole structure shows high levels of atomic vibration 
with some of the linker carbons elongated to a greater extent.
;
_vrf_PLAT987_2016ncs0703_sq      
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: The symmetry of the metallated structure is much lower than that 
of the parent structure 2 with the Cu site ordered on one side of the linker.
The space group P-62c (no. 190) is non-centrosymmetric and the Flack 
parameter is ~0.5, suggesting a racemic twin, which is not unreasonable
given the centrosymmetric nature of the parent structure.
;
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H23 Cl3 Cu1.50 N6 O16 Sc3'
_chemical_formula_sum            'C36 H23 Cl3 Cu1.50 N6 O16 Sc3'
_chemical_formula_weight         1132.14
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
Sc Sc 0.2519 0.3716 '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      hexagonal
_space_group_IT_number           190
_space_group_name_H-M_alt        'P -6 2 c'
_space_group_name_Hall           'P -6c -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   17.9930(10)
_cell_length_b                   17.9930(10)
_cell_length_c                   24.7387(11)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_volume                     6936.1(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12990
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.9880
_cell_measurement_theta_min      2.1130
_cell_oxdiff_angle_alpha         90.062(5)
_cell_oxdiff_angle_beta          90.011(6)
_cell_oxdiff_angle_gamma         119.916(9)
_cell_oxdiff_length_a            17.9854(17)
_cell_oxdiff_length_b            17.9912(15)
_cell_oxdiff_length_c            24.7307(11)
_cell_oxdiff_measurement_reflns_used 12899
_cell_oxdiff_volume              6936.1(9)
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    0.542
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1133
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.045
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1270
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55176
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.102
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  73.00   1.00  120.00    --  -17.00  72.00-180.00  108
  2  ω    -78.00  22.00   1.00  120.00    --  -17.00 -72.00  60.00  100
  3  ω    -66.00  22.00   1.00  120.00    --  -17.00 -72.00-120.00   88
  4  ω    -89.00  21.00   1.00  120.00    --  -17.00   0.00  60.00  110
  5  ω    -32.00 -12.00   1.00  120.00    --  -17.00  54.00  30.00   20
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0330969000
_diffrn_orient_matrix_UB_12      0.0415755000
_diffrn_orient_matrix_UB_13      0.0074686000
_diffrn_orient_matrix_UB_21      0.0297445000
_diffrn_orient_matrix_UB_22      -0.0149888000
_diffrn_orient_matrix_UB_23      0.0006068000
_diffrn_orient_matrix_UB_31      0.0095229000
_diffrn_orient_matrix_UB_32      0.0108066000
_diffrn_orient_matrix_UB_33      -0.0276818000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_reflns_Friedel_coverage         0.813
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2680
_reflns_number_total             4204
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 
;
 Flack x determined using 891 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.508(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         4204
_refine_ls_number_restraints     99
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0614
_refine_ls_restrained_S_all      0.949
_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)+(0.1244P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.1891
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C2-C3 = N1-C3 = N1-C6 = C5-C6 = C4-C2 = C4-C5
 1.39 with sigma of 0.02
3. Restrained planarity
 C2, C4, C5, C3, N1, C6
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cu1(0.25) Cl1(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Cu1 Cu 0.60726(11) 0.60726(11) 0.500000 0.1701(16) Uani 0.5 2 d S TU P . .
Sc1 Sc 0.46103(9) 0.71408(9) 0.750000 0.0798(5) Uani 1 2 d S TU P . .
Cl1 Cl 0.6404(10) 0.7187(9) 0.5411(5) 0.357(6) Uiso 0.5 1 d . U . . .
O1 O 0.5940(4) 0.7642(6) 0.750000 0.141(3) Uani 1 2 d S TU P . .
O2 O 0.333333 0.666667 0.750000 0.0691(19) Uani 1 6 d S TU P . .
O3 O 0.4541(3) 0.6296(3) 0.68802(16) 0.1189(14) Uani 1 1 d . U . . .
O4 O 0.3208(3) 0.5185(3) 0.68915(15) 0.1137(14) Uani 1 1 d . U . . .
N1 N 0.5037(5) 0.5467(5) 0.5443(3) 0.161(3) Uani 1 1 d D U . . .
C1 C 0.3925(5) 0.5586(6) 0.6697(2) 0.121(2) Uani 1 1 d . U . . .
C2 C 0.4093(5) 0.5253(5) 0.6182(3) 0.146(3) Uani 1 1 d D U . . .
C3 C 0.4861(6) 0.5765(5) 0.5928(3) 0.138(3) Uani 1 1 d D U . . .
H3 H 0.525675 0.629525 0.607217 0.166 Uiso 1 1 calc R . . . .
C4 C 0.3499(8) 0.4434(7) 0.5997(4) 0.283(10) Uani 1 1 d D U . . .
H4 H 0.297952 0.407725 0.616827 0.340 Uiso 1 1 calc R . . . .
C5 C 0.3764(9) 0.4210(7) 0.5536(5) 0.282(9) Uani 1 1 d D U . . .
H5 H 0.340217 0.365330 0.541564 0.338 Uiso 1 1 calc R . . . .
C6 C 0.4447(6) 0.4659(6) 0.5242(4) 0.173(4) Uani 1 1 d D U . . .


_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
Cu1 Cl1 2.052(13) 7_556 ?
Cu1 Cl1 2.052(13) . ?
Cu1 N1 1.957(6) . ?
Cu1 N1 1.957(6) 7_556 ?
Sc1 Sc1 3.484(2) 3_565 ?
Sc1 Sc1 3.484(2) 2_665 ?
Sc1 O1 2.093(6) . ?
Sc1 O2 2.0117(14) . ?
Sc1 O3 2.118(4) . ?
Sc1 O3 2.118(4) 4_556 ?
Sc1 O4 2.083(4) 2_665 ?
Sc1 O4 2.083(4) 5_666 ?
O3 C1 1.284(9) . ?
O4 C1 1.217(8) . ?
N1 C3 1.415(8) . ?
N1 C6 1.394(9) . ?
C1 C2 1.502(8) . ?
C2 C3 1.371(10) . ?
C2 C4 1.396(11) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C4 C5 1.372(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.304(11) . ?
C6 C6 1.366(17) 7_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
Cl1 Cu1 Cl1 101.4(9) . 7_556 ?
N1 Cu1 Cl1 89.9(5) . . ?
N1 Cu1 Cl1 89.9(5) 7_556 7_556 ?
N1 Cu1 Cl1 163.5(5) . 7_556 ?
N1 Cu1 Cl1 163.5(5) 7_556 . ?
N1 Cu1 N1 82.0(4) . 7_556 ?
Sc1 Sc1 Sc1 60.0 3_565 2_665 ?
O1 Sc1 Sc1 150.4(3) . 3_565 ?
O1 Sc1 Sc1 149.6(3) . 2_665 ?
O1 Sc1 O3 87.4(2) . . ?
O1 Sc1 O3 87.4(2) . 4_556 ?
O2 Sc1 Sc1 30.0 . 3_565 ?
O2 Sc1 Sc1 30.0 . 2_665 ?
O2 Sc1 O1 179.6(3) . . ?
O2 Sc1 O3 92.90(13) . . ?
O2 Sc1 O3 92.90(13) . 4_556 ?
O2 Sc1 O4 92.99(13) . 2_665 ?
O2 Sc1 O4 92.99(13) . 5_666 ?
O3 Sc1 Sc1 72.53(14) . 3_565 ?
O3 Sc1 Sc1 112.83(13) 4_556 2_665 ?
O3 Sc1 Sc1 72.53(14) 4_556 3_565 ?
O3 Sc1 Sc1 112.83(13) . 2_665 ?
O3 Sc1 O3 92.7(3) . 4_556 ?
O4 Sc1 Sc1 112.93(13) 2_665 3_565 ?
O4 Sc1 Sc1 72.58(13) 2_665 2_665 ?
O4 Sc1 Sc1 72.58(13) 5_666 2_665 ?
O4 Sc1 Sc1 112.93(13) 5_666 3_565 ?
O4 Sc1 O1 86.8(2) 2_665 . ?
O4 Sc1 O1 86.8(2) 5_666 . ?
O4 Sc1 O3 87.03(18) 5_666 4_556 ?
O4 Sc1 O3 174.11(19) 5_666 . ?
O4 Sc1 O3 87.03(18) 2_665 . ?
O4 Sc1 O3 174.11(19) 2_665 4_556 ?
O4 Sc1 O4 92.6(3) 5_666 2_665 ?
Sc1 O2 Sc1 120.002(1) 3_565 . ?
Sc1 O2 Sc1 120.0 2_665 3_565 ?
Sc1 O2 Sc1 120.0 2_665 . ?
C1 O3 Sc1 132.9(4) . . ?
C1 O4 Sc1 136.1(4) . 3_565 ?
C3 N1 Cu1 126.5(6) . . ?
C6 N1 Cu1 113.4(5) . . ?
C6 N1 C3 120.0(7) . . ?
O3 C1 C2 116.7(7) . . ?
O4 C1 O3 125.6(5) . . ?
O4 C1 C2 117.6(7) . . ?
C3 C2 C1 117.2(7) . . ?
C3 C2 C4 122.8(6) . . ?
C4 C2 C1 119.9(7) . . ?
N1 C3 H3 120.8 . . ?
C2 C3 N1 118.4(7) . . ?
C2 C3 H3 120.8 . . ?
C2 C4 H4 123.6 . . ?
C5 C4 C2 112.8(9) . . ?
C5 C4 H4 123.6 . . ?
C4 C5 H5 115.1 . . ?
C6 C5 C4 129.9(10) . . ?
C6 C5 H5 115.1 . . ?
C5 C6 N1 115.9(8) . . ?
C5 C6 C6 128.6(5) . 7_556 ?
C6 C6 N1 115.5(4) 7_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
Cu1 N1 C3 C2 179.4(7) . . . . ?
Cu1 N1 C6 C5 176.6(11) . . . . ?
Cu1 N1 C6 C6 -3.9(18) . . . 7_556 ?
Sc1 O3 C1 O4 -7.0(13) . . . . ?
Sc1 O3 C1 C2 169.3(5) . . . . ?
Sc1 O4 C1 O3 7.6(13) 3_565 . . . ?
Sc1 O4 C1 C2 -168.7(5) 3_565 . . . ?
O3 C1 C2 C3 -5.0(12) . . . . ?
O3 C1 C2 C4 171.5(10) . . . . ?
O4 C1 C2 C3 171.6(8) . . . . ?
O4 C1 C2 C4 -11.9(14) . . . . ?
C1 C2 C3 N1 179.9(7) . . . . ?
C1 C2 C4 C5 -177.2(11) . . . . ?
C2 C4 C5 C6 -4(2) . . . . ?
C3 N1 C6 C5 -2.2(17) . . . . ?
C3 N1 C6 C6 177.2(12) . . . 7_556 ?
C3 C2 C4 C5 -0.8(15) . . . . ?
C4 C2 C3 N1 3.5(15) . . . . ?
C4 C5 C6 N1 6(2) . . . . ?
C4 C5 C6 C6 -173.7(17) . . . 7_556 ?
C6 N1 C3 C2 -1.9(14) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.653
_oxdiff_exptl_absorpt_empirical_full_min 0.390
