# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_2016fmm7662-36r0
_database_code_depnum_ccdc_archive 'CCDC 1590538'
_audit_update_record             
;
2017-12-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H11 Cl3 N3 Sc'
_chemical_formula_sum            'C15 H11 Cl3 N3 Sc'
_chemical_formula_weight         384.58

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.5434(12)
_cell_length_b                   13.9045(12)
_cell_length_c                   14.0175(16)
_cell_angle_alpha                90
_cell_angle_beta                 106.779(13)
_cell_angle_gamma                90
_cell_volume                     1594.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3065
_cell_measurement_theta_min      2.4970
_cell_measurement_theta_max      31.8120

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_F_000             776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.017
_exptl_absorpt_coefficient_mu    0.961
_shelx_estimated_absorpt_T_min   0.981
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.58579
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            14466
_diffrn_reflns_av_unetI/netI     0.1400
_diffrn_reflns_av_R_equivalents  0.1488
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.109
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3144
_reflns_number_gt                1750
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0432P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3144
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1511
_refine_ls_R_factor_gt           0.0704
_refine_ls_wR_factor_ref         0.1446
_refine_ls_wR_factor_gt          0.1156
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sc1 Sc 1.04445(15) 0.12769(7) 0.21471(8) 0.0228(3) Uani 1 1 d . . . . .
Cl1 Cl 0.7841(2) 0.15691(10) 0.09317(11) 0.0359(4) Uani 1 1 d . . . . .
Cl2 Cl 1.1987(2) 0.14860(11) 0.09805(11) 0.0386(5) Uani 1 1 d . . . . .
Cl3 Cl 1.29418(19) 0.09450(9) 0.34953(10) 0.0265(4) Uani 1 1 d . . . . .
N1 N 0.9893(6) -0.0290(3) 0.2141(3) 0.0243(12) Uani 1 1 d . . . . .
N2 N 0.9209(6) 0.0983(3) 0.3318(3) 0.0229(11) Uani 1 1 d . . . . .
N3 N 1.0115(6) 0.2672(3) 0.2876(3) 0.0209(11) Uani 1 1 d . . . . .
C1 C 1.0328(8) -0.0900(4) 0.1524(4) 0.0312(16) Uani 1 1 d . . . . .
H1 H 1.0697 -0.0645 0.0999 0.037 Uiso 1 1 calc R U . . .
C2 C 1.0263(8) -0.1882(4) 0.1620(5) 0.0357(17) Uani 1 1 d . . . . .
H2 H 1.0581 -0.2299 0.1172 0.043 Uiso 1 1 calc R U . . .
C3 C 0.9724(8) -0.2243(4) 0.2383(5) 0.0366(18) Uani 1 1 d . . . . .
H3 H 0.9695 -0.2919 0.2476 0.044 Uiso 1 1 calc R U . . .
C4 C 0.9227(8) -0.1632(4) 0.3012(4) 0.0287(15) Uani 1 1 d . . . . .
H4 H 0.8833 -0.1877 0.3533 0.034 Uiso 1 1 calc R U . . .
C5 C 0.9319(7) -0.0647(4) 0.2864(4) 0.0242(15) Uani 1 1 d . . . . .
C6 C 0.8810(8) 0.0084(4) 0.3491(4) 0.0233(14) Uani 1 1 d . . . . .
C7 C 0.8000(8) -0.0122(4) 0.4182(4) 0.0299(16) Uani 1 1 d . . . . .
H7 H 0.7713 -0.0765 0.4289 0.036 Uiso 1 1 calc R U . . .
C8 C 0.7612(8) 0.0625(4) 0.4716(4) 0.0319(16) Uani 1 1 d . . . . .
H8 H 0.7028 0.0499 0.5185 0.038 Uiso 1 1 calc R U . . .
C9 C 0.8065(8) 0.1552(4) 0.4576(4) 0.0286(15) Uani 1 1 d . . . . .
H9 H 0.7831 0.2068 0.4958 0.034 Uiso 1 1 calc R U . . .
C10 C 0.8874(7) 0.1715(4) 0.3861(4) 0.0209(13) Uani 1 1 d . . . . .
C11 C 0.9383(7) 0.2667(4) 0.3603(4) 0.0200(13) Uani 1 1 d . . . . .
C12 C 0.9127(7) 0.3499(4) 0.4066(4) 0.0258(15) Uani 1 1 d . . . . .
H12 H 0.8646 0.3480 0.4598 0.031 Uiso 1 1 calc R U . . .
C13 C 0.9582(8) 0.4360(4) 0.3743(4) 0.0279(15) Uani 1 1 d . . . . .
H13 H 0.9406 0.4945 0.4048 0.034 Uiso 1 1 calc R U . . .
C14 C 1.0287(8) 0.4375(4) 0.2986(4) 0.0283(15) Uani 1 1 d . . . . .
H14 H 1.0592 0.4966 0.2750 0.034 Uiso 1 1 calc R U . . .
C15 C 1.0547(8) 0.3516(4) 0.2573(4) 0.0286(15) Uani 1 1 d . . . . .
H15 H 1.1053 0.3522 0.2052 0.034 Uiso 1 1 calc R 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
Sc1 N1 2.228(4) . ?
Sc1 N2 2.230(5) . ?
Sc1 N3 2.247(4) . ?
Sc1 Cl2 2.3959(19) . ?
Sc1 Cl1 2.414(2) . ?
Sc1 Cl3 2.4512(19) . ?
N1 C1 1.338(7) . ?
N1 C5 1.344(7) . ?
N2 C6 1.336(6) . ?
N2 C10 1.351(7) . ?
N3 C15 1.335(6) . ?
N3 C11 1.341(6) . ?
C1 C2 1.374(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.375(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.378(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.487(8) . ?
C6 C7 1.374(8) . ?
C7 C8 1.374(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.377(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.390(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.471(7) . ?
C11 C12 1.375(7) . ?
C12 C13 1.375(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.364(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.374(8) . ?
C14 H14 0.9500 . ?
C15 H15 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
N1 Sc1 N2 71.30(17) . . ?
N1 Sc1 N3 142.34(18) . . ?
N2 Sc1 N3 71.09(16) . . ?
N1 Sc1 Cl2 105.85(14) . . ?
N2 Sc1 Cl2 174.21(14) . . ?
N3 Sc1 Cl2 111.79(13) . . ?
N1 Sc1 Cl1 90.63(13) . . ?
N2 Sc1 Cl1 90.85(13) . . ?
N3 Sc1 Cl1 87.98(13) . . ?
Cl2 Sc1 Cl1 94.25(7) . . ?
N1 Sc1 Cl3 87.42(13) . . ?
N2 Sc1 Cl3 83.67(13) . . ?
N3 Sc1 Cl3 90.42(13) . . ?
Cl2 Sc1 Cl3 91.21(7) . . ?
Cl1 Sc1 Cl3 174.52(7) . . ?
C1 N1 C5 118.9(5) . . ?
C1 N1 Sc1 121.7(4) . . ?
C5 N1 Sc1 118.8(3) . . ?
C6 N2 C10 119.8(5) . . ?
C6 N2 Sc1 120.3(4) . . ?
C10 N2 Sc1 119.9(3) . . ?
C15 N3 C11 118.6(5) . . ?
C15 N3 Sc1 122.1(4) . . ?
C11 N3 Sc1 119.2(3) . . ?
N1 C1 C2 122.7(6) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C1 C2 C3 118.1(6) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C2 C3 C4 120.5(5) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C5 118.1(6) . . ?
C3 C4 H4 121.0 . . ?
C5 C4 H4 121.0 . . ?
N1 C5 C4 121.7(5) . . ?
N1 C5 C6 115.2(5) . . ?
C4 C5 C6 123.1(5) . . ?
N2 C6 C7 121.9(5) . . ?
N2 C6 C5 113.5(5) . . ?
C7 C6 C5 124.5(5) . . ?
C6 C7 C8 118.5(5) . . ?
C6 C7 H7 120.8 . . ?
C8 C7 H7 120.8 . . ?
C7 C8 C9 120.5(6) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C8 C9 C10 118.3(5) . . ?
C8 C9 H9 120.9 . . ?
C10 C9 H9 120.9 . . ?
N2 C10 C9 120.9(5) . . ?
N2 C10 C11 114.5(5) . . ?
C9 C10 C11 124.6(5) . . ?
N3 C11 C12 121.9(5) . . ?
N3 C11 C10 115.3(5) . . ?
C12 C11 C10 122.9(5) . . ?
C13 C12 C11 118.6(5) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C14 C13 C12 120.0(5) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 118.5(5) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
N3 C15 C14 122.5(6) . . ?
N3 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?

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
C5 N1 C1 C2 -2.2(9) . . . . ?
Sc1 N1 C1 C2 168.4(5) . . . . ?
N1 C1 C2 C3 0.1(10) . . . . ?
C1 C2 C3 C4 1.6(10) . . . . ?
C2 C3 C4 C5 -1.2(9) . . . . ?
C1 N1 C5 C4 2.6(9) . . . . ?
Sc1 N1 C5 C4 -168.2(4) . . . . ?
C1 N1 C5 C6 -177.9(5) . . . . ?
Sc1 N1 C5 C6 11.2(7) . . . . ?
C3 C4 C5 N1 -0.9(9) . . . . ?
C3 C4 C5 C6 179.7(6) . . . . ?
C10 N2 C6 C7 2.8(9) . . . . ?
Sc1 N2 C6 C7 -177.8(4) . . . . ?
C10 N2 C6 C5 -177.6(5) . . . . ?
Sc1 N2 C6 C5 1.9(7) . . . . ?
N1 C5 C6 N2 -8.4(8) . . . . ?
C4 C5 C6 N2 171.1(5) . . . . ?
N1 C5 C6 C7 171.2(6) . . . . ?
C4 C5 C6 C7 -9.3(10) . . . . ?
N2 C6 C7 C8 -0.9(9) . . . . ?
C5 C6 C7 C8 179.6(5) . . . . ?
C6 C7 C8 C9 -1.6(9) . . . . ?
C7 C8 C9 C10 2.0(9) . . . . ?
C6 N2 C10 C9 -2.3(8) . . . . ?
Sc1 N2 C10 C9 178.2(4) . . . . ?
C6 N2 C10 C11 179.6(5) . . . . ?
Sc1 N2 C10 C11 0.2(6) . . . . ?
C8 C9 C10 N2 0.0(9) . . . . ?
C8 C9 C10 C11 177.8(5) . . . . ?
C15 N3 C11 C12 -2.6(8) . . . . ?
Sc1 N3 C11 C12 -179.1(4) . . . . ?
C15 N3 C11 C10 177.2(5) . . . . ?
Sc1 N3 C11 C10 0.6(6) . . . . ?
N2 C10 C11 N3 -0.5(7) . . . . ?
C9 C10 C11 N3 -178.5(5) . . . . ?
N2 C10 C11 C12 179.2(5) . . . . ?
C9 C10 C11 C12 1.2(9) . . . . ?
N3 C11 C12 C13 2.5(9) . . . . ?
C10 C11 C12 C13 -177.2(5) . . . . ?
C11 C12 C13 C14 -0.7(9) . . . . ?
C12 C13 C14 C15 -0.9(9) . . . . ?
C11 N3 C15 C14 0.8(9) . . . . ?
Sc1 N3 C15 C14 177.2(5) . . . . ?
C13 C14 C15 N3 0.9(9) . . . . ?

_refine_diff_density_max         0.565
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.110


_vrf_RINTA01_2016fmm7662-36r0    


;
PROBLEM:    The value of Rint is greater than 0.12   
RESPONSE: This is due to the size of the crystal. Only small crystals were found. 
;

_vrf_PLAT020_2016fmm7662-36r0    


;
PROBLEM:    The value of Rint is greater than 0.12   
RESPONSE: This is due to the size of the crystal. Only small crystals were found. 
;
####################################################################### 
# 
# 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_2016fmm7662-39ar
_database_code_depnum_ccdc_archive 'CCDC 1590539'
_audit_update_record             
;
2017-12-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
_audit_creation_date             2016-05-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C15 H11 Cl3 N3 O Y'
_chemical_formula_sum            'C15 H11 Cl3 N3 O Y'
_chemical_formula_weight         444.53
_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'
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'
Y Y -2.7962 3.5667 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.5645(7)
_cell_length_b                   9.9623(10)
_cell_length_c                   12.1261(11)
_cell_angle_alpha                70.174(9)
_cell_angle_beta                 83.413(7)
_cell_angle_gamma                73.153(8)
_cell_volume                     822.62(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4654
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0810
_cell_measurement_theta_min      2.3960
_shelx_estimated_absorpt_T_max   0.938
_shelx_estimated_absorpt_T_min   0.827
_exptl_absorpt_coefficient_mu    4.037
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.049
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.016
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_unetI/netI     0.0859
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10392
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.256
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -77.00  37.00   1.00   15.00    --  -23.00   0.00 -60.00  114
  2  ω    -39.00  67.00   1.00   15.00    --  -23.00  72.00  90.00  106
  3  ω    -79.00  16.00   1.00   15.00    --  -23.00 -72.00 -30.00   95
  4  ω    -70.00  16.00   1.00   15.00    --  -23.00 -72.00 150.00   86
  5  ω    -55.00 -24.00   1.00   15.00    --  -23.00  72.00 -60.00   31
  6  ω    -39.00  67.00   1.00   15.00    --  -23.00  72.00-180.00  106
  7  ω    -78.00  16.00   1.00   15.00    --  -23.00 -72.00  60.00   94
  8  ω    -70.00 -52.00   1.00   15.00    --  -23.00 -72.00-120.00   18
;
_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_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0037061000
_diffrn_orient_matrix_UB_12      0.0590921000
_diffrn_orient_matrix_UB_13      0.0210393000
_diffrn_orient_matrix_UB_21      0.0482384000
_diffrn_orient_matrix_UB_22      -0.0512596000
_diffrn_orient_matrix_UB_23      0.0507609000
_diffrn_orient_matrix_UB_31      0.0852120000
_diffrn_orient_matrix_UB_32      0.0073293000
_diffrn_orient_matrix_UB_33      -0.0291243000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2411
_reflns_number_total             3236
_reflns_odcompleteness_completeness 91.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.42
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    ?
_refine_diff_density_max         1.114
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3236
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0531
_refine_ls_restrained_S_all      1.029
_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)+(0.0636P)²+0.1403P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1299
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C7(H7), C9(H9), C8(H8), C2(H2), C15(H15), C13(H13), C1(H1),
 C14(H14), C12(H12)
;
_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
Y1 Y 0.21923(8) 0.33018(5) 0.20771(4) 0.01395(18) Uani 1 1 d . . . . .
Cl2 Cl -0.0094(2) 0.20949(14) 0.15519(10) 0.0168(3) Uani 1 1 d . . . . .
Cl1 Cl 0.4458(2) 0.43723(14) 0.27208(11) 0.0205(3) Uani 1 1 d . . . . .
Cl3 Cl -0.0553(2) 0.57717(14) 0.19514(11) 0.0189(3) Uani 1 1 d . . . . .
O1 O 0.2074(5) 0.4787(4) 0.0100(3) 0.0170(9) Uani 1 1 d . . . . .
N1 N 0.4825(7) 0.1987(5) 0.1043(4) 0.0149(10) Uani 1 1 d . . . . .
N2 N 0.3621(7) 0.0671(5) 0.3189(3) 0.0146(10) Uani 1 1 d . . . . .
N3 N 0.1086(7) 0.2491(5) 0.4172(4) 0.0166(10) Uani 1 1 d . . . . .
C4 C 0.6888(8) -0.0264(6) 0.0891(5) 0.0187(13) Uani 1 1 d . . . . .
H4 H 0.7345 -0.1309 0.1212 0.022 Uiso 1 1 calc R . . . .
C5 C 0.5504(8) 0.0510(6) 0.1480(4) 0.0164(12) Uani 1 1 d . . . . .
C3 C 0.7593(8) 0.0486(6) -0.0155(5) 0.0200(13) Uani 1 1 d . . . . .
H3 H 0.8525 -0.0037 -0.0568 0.024 Uiso 1 1 calc R . . . .
C7 C 0.5311(9) -0.1763(6) 0.3162(5) 0.0206(13) Uani 1 1 d . . . . .
H7 H 0.6067 -0.2379 0.2742 0.025 Uiso 1 1 calc R . . . .
C11 C 0.1757(8) 0.1069(6) 0.4866(4) 0.0169(13) Uani 1 1 d . . . . .
C9 C 0.3596(8) -0.1457(6) 0.4861(5) 0.0201(13) Uani 1 1 d . . . . .
H9 H 0.3197 -0.1861 0.5645 0.024 Uiso 1 1 calc R . . . .
C6 C 0.4787(8) -0.0232(6) 0.2645(5) 0.0163(12) Uani 1 1 d . . . . .
C8 C 0.4724(9) -0.2371(6) 0.4283(5) 0.0252(14) Uani 1 1 d . . . . .
H8 H 0.5090 -0.3412 0.4659 0.030 Uiso 1 1 calc R . . . .
C2 C 0.6939(8) 0.1993(6) -0.0596(5) 0.0203(13) Uani 1 1 d . . . . .
H2 H 0.7415 0.2542 -0.1312 0.024 Uiso 1 1 calc R . . . .
C15 C -0.0100(8) 0.3427(6) 0.4664(5) 0.0188(13) Uani 1 1 d . . . . .
H15 H -0.0614 0.4415 0.4181 0.023 Uiso 1 1 calc R . . . .
C13 C 0.0092(8) 0.1592(6) 0.6523(4) 0.0202(13) Uani 1 1 d . . . . .
H13 H -0.0245 0.1282 0.7331 0.024 Uiso 1 1 calc R . . . .
C1 C 0.5573(8) 0.2687(6) 0.0031(4) 0.0176(12) Uani 1 1 d . . . . .
H1 H 0.5125 0.3735 -0.0273 0.021 Uiso 1 1 calc R . . . .
C10 C 0.3053(8) 0.0039(6) 0.4299(4) 0.0170(13) Uani 1 1 d . . . . .
C14 C -0.0609(9) 0.3033(6) 0.5826(5) 0.0230(14) Uani 1 1 d . . . . .
H14 H -0.1427 0.3738 0.6144 0.028 Uiso 1 1 calc R . . . .
C12 C 0.1289(9) 0.0608(6) 0.6033(5) 0.0214(13) Uani 1 1 d . . . . .
H12 H 0.1789 -0.0390 0.6502 0.026 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
Y1 Cl2 2.6116(14) . ?
Y1 Cl1 2.5716(14) . ?
Y1 Cl3 2.6919(15) . ?
Y1 O1 2.348(3) . ?
Y1 N1 2.506(4) . ?
Y1 N2 2.480(4) . ?
Y1 N3 2.514(4) . ?
N1 C5 1.344(6) . ?
N1 C1 1.342(6) . ?
N2 C6 1.353(7) . ?
N2 C10 1.358(6) . ?
N3 C11 1.358(7) . ?
N3 C15 1.342(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(7) . ?
C4 C3 1.372(8) . ?
C5 C6 1.479(7) . ?
C3 H3 0.9500 . ?
C3 C2 1.368(8) . ?
C7 H7 0.9500 . ?
C7 C6 1.391(7) . ?
C7 C8 1.368(8) . ?
C11 C10 1.491(7) . ?
C11 C12 1.370(7) . ?
C9 H9 0.9500 . ?
C9 C8 1.376(8) . ?
C9 C10 1.369(7) . ?
C8 H8 0.9500 . ?
C2 H2 0.9500 . ?
C2 C1 1.373(7) . ?
C15 H15 0.9500 . ?
C15 C14 1.370(7) . ?
C13 H13 0.9500 . ?
C13 C14 1.376(8) . ?
C13 C12 1.376(8) . ?
C1 H1 0.9500 . ?
C14 H14 0.9500 . ?
C12 H12 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
Cl2 Y1 Cl3 90.55(5) . . ?
Cl1 Y1 Cl2 176.48(4) . . ?
Cl1 Y1 Cl3 90.77(5) . . ?
O1 Y1 Cl2 86.90(10) . . ?
O1 Y1 Cl1 96.60(10) . . ?
O1 Y1 Cl3 74.09(9) . . ?
O1 Y1 N1 73.41(13) . . ?
O1 Y1 N2 135.85(13) . . ?
O1 Y1 N3 156.54(15) . . ?
N1 Y1 Cl2 91.85(10) . . ?
N1 Y1 Cl1 88.81(11) . . ?
N1 Y1 Cl3 147.22(10) . . ?
N1 Y1 N3 129.73(15) . . ?
N2 Y1 Cl2 80.83(11) . . ?
N2 Y1 Cl1 96.34(11) . . ?
N2 Y1 Cl3 147.50(11) . . ?
N2 Y1 N1 64.87(14) . . ?
N2 Y1 N3 65.58(14) . . ?
N3 Y1 Cl2 88.31(10) . . ?
N3 Y1 Cl1 88.61(10) . . ?
N3 Y1 Cl3 83.01(11) . . ?
C5 N1 Y1 119.9(3) . . ?
C1 N1 Y1 122.9(4) . . ?
C1 N1 C5 117.1(5) . . ?
C6 N2 Y1 120.4(3) . . ?
C6 N2 C10 117.6(5) . . ?
C10 N2 Y1 121.2(3) . . ?
C11 N3 Y1 119.8(3) . . ?
C15 N3 Y1 122.6(3) . . ?
C15 N3 C11 117.5(4) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.9(5) . . ?
N1 C5 C4 121.4(5) . . ?
N1 C5 C6 116.6(5) . . ?
C4 C5 C6 121.9(5) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 C4 119.3(5) . . ?
C2 C3 H3 120.3 . . ?
C6 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
C8 C7 C6 119.0(5) . . ?
N3 C11 C10 116.8(4) . . ?
N3 C11 C12 121.6(5) . . ?
C12 C11 C10 121.6(5) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C10 C9 C8 119.6(5) . . ?
N2 C6 C5 115.9(5) . . ?
N2 C6 C7 122.1(5) . . ?
C7 C6 C5 122.0(5) . . ?
C7 C8 C9 119.3(5) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C3 C2 H2 121.1 . . ?
C3 C2 C1 117.8(5) . . ?
C1 C2 H2 121.1 . . ?
N3 C15 H15 118.3 . . ?
N3 C15 C14 123.4(5) . . ?
C14 C15 H15 118.3 . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C12 C13 C14 119.0(5) . . ?
N1 C1 C2 124.5(5) . . ?
N1 C1 H1 117.7 . . ?
C2 C1 H1 117.7 . . ?
N2 C10 C11 116.0(4) . . ?
N2 C10 C9 122.3(5) . . ?
C9 C10 C11 121.7(5) . . ?
C15 C14 C13 118.5(5) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C11 C12 C13 119.9(5) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?

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
Y1 N1 C5 C4 176.1(4) . . . . ?
Y1 N1 C5 C6 -7.5(6) . . . . ?
Y1 N1 C1 C2 -175.9(4) . . . . ?
Y1 N2 C6 C5 15.1(6) . . . . ?
Y1 N2 C6 C7 -166.4(4) . . . . ?
Y1 N2 C10 C11 -9.4(6) . . . . ?
Y1 N2 C10 C9 169.1(4) . . . . ?
Y1 N3 C11 C10 -3.7(6) . . . . ?
Y1 N3 C11 C12 175.4(4) . . . . ?
Y1 N3 C15 C14 -174.8(4) . . . . ?
N1 C5 C6 N2 -4.8(7) . . . . ?
N1 C5 C6 C7 176.6(5) . . . . ?
N3 C11 C10 N2 8.4(7) . . . . ?
N3 C11 C10 C9 -170.1(5) . . . . ?
N3 C11 C12 C13 0.8(9) . . . . ?
N3 C15 C14 C13 -1.7(9) . . . . ?
C4 C5 C6 N2 171.7(5) . . . . ?
C4 C5 C6 C7 -6.9(8) . . . . ?
C4 C3 C2 C1 -1.0(8) . . . . ?
C5 N1 C1 C2 1.7(8) . . . . ?
C5 C4 C3 C2 1.0(9) . . . . ?
C3 C4 C5 N1 0.4(8) . . . . ?
C3 C4 C5 C6 -175.9(5) . . . . ?
C3 C2 C1 N1 -0.4(9) . . . . ?
C11 N3 C15 C14 2.3(8) . . . . ?
C6 N2 C10 C11 -179.5(5) . . . . ?
C6 N2 C10 C9 -1.0(8) . . . . ?
C6 C7 C8 C9 1.5(9) . . . . ?
C8 C7 C6 N2 -4.1(9) . . . . ?
C8 C7 C6 C5 174.4(5) . . . . ?
C8 C9 C10 N2 -1.5(9) . . . . ?
C8 C9 C10 C11 176.9(5) . . . . ?
C15 N3 C11 C10 179.2(5) . . . . ?
C15 N3 C11 C12 -1.8(8) . . . . ?
C1 N1 C5 C4 -1.7(8) . . . . ?
C1 N1 C5 C6 174.8(5) . . . . ?
C10 N2 C6 C5 -174.7(5) . . . . ?
C10 N2 C6 C7 3.9(8) . . . . ?
C10 C11 C12 C13 179.8(5) . . . . ?
C10 C9 C8 C7 1.2(9) . . . . ?
C14 C13 C12 C11 -0.2(9) . . . . ?
C12 C11 C10 N2 -170.7(5) . . . . ?
C12 C11 C10 C9 10.8(8) . . . . ?
C12 C13 C14 C15 0.7(9) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.751
_oxdiff_exptl_absorpt_empirical_full_min 0.368
####################################################################### 
# 
# 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_2016rnw7945-05r
_database_code_depnum_ccdc_archive 'CCDC 1590543'
_audit_update_record             
;
2017-12-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
_audit_creation_date             2016-08-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C30 H26 Cl6 La2 N6 O2'
_chemical_formula_sum            'C30 H26 Cl6 La2 N6 O2'
_chemical_formula_weight         993.09
_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'
La La -0.2871 2.4523 '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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7676(4)
_cell_length_b                   9.9809(4)
_cell_length_c                   10.3396(3)
_cell_angle_alpha                94.048(3)
_cell_angle_beta                 109.768(3)
_cell_angle_gamma                113.865(4)
_cell_volume                     841.92(6)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    11074
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.2440
_cell_measurement_theta_min      2.1740
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.018
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       chunk
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.039
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.019
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10844
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.490
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996


_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3006
_reflns_number_total             3299
_reflns_odcompleteness_completeness 90.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.32
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3299
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0249
_refine_ls_restrained_S_all      0.976
_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)+(0.0370P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0586
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C3(H3), C7(H7), C1(H1), C4(H4), C2(H2), C9(H9), C8(H8), C12(H12),
 C14(H14), C13(H13)
;
_atom_sites_solution_hydrogens   mixed
_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
La1 La 0.97564(2) 0.27579(2) 0.37861(2) 0.00972(7) Uani 1 1 d . . . . .
Cl1 Cl 0.91659(8) -0.00183(8) 0.22267(8) 0.01363(16) Uani 1 1 d . . . . .
Cl3 Cl 1.01034(9) 0.57464(8) 0.36066(8) 0.01666(17) Uani 1 1 d . . . . .
Cl2 Cl 1.27268(8) 0.29309(8) 0.56078(8) 0.01763(17) Uani 1 1 d . . . . .
O1 O 0.8767(3) 0.0710(3) 0.5099(3) 0.0143(5) Uani 1 1 d . . . . .
N1 N 0.6611(3) 0.1918(3) 0.3038(3) 0.0146(6) Uani 1 1 d . . . . .
N3 N 1.1282(3) 0.3602(3) 0.2069(3) 0.0117(5) Uani 1 1 d . . . . .
N2 N 0.7936(3) 0.2479(3) 0.1085(3) 0.0107(5) Uani 1 1 d . . . . .
C10 C 0.8635(3) 0.2833(3) 0.0153(3) 0.0127(6) Uani 1 1 d . . . . .
C11 C 1.0408(3) 0.3269(3) 0.0654(3) 0.0122(6) Uani 1 1 d . . . . .
C15 C 1.2901(3) 0.4099(3) 0.2534(3) 0.0151(7) Uani 1 1 d . . . . .
H15 H 1.3520 0.4352 0.3527 0.018 Uiso 1 1 calc R . . . .
C5 C 0.5577(3) 0.1675(3) 0.1691(3) 0.0125(6) Uani 1 1 d . . . . .
C3 C 0.3278(4) 0.0824(3) 0.2327(4) 0.0178(7) Uani 1 1 d . . . . .
H3 H 0.2136 0.0435 0.2078 0.021 Uiso 1 1 calc R . . . .
C7 C 0.5371(4) 0.2005(3) -0.0734(3) 0.0157(7) Uani 1 1 d . . . . .
H7 H 0.4235 0.1699 -0.1023 0.019 Uiso 1 1 calc R . . . .
C6 C 0.6317(3) 0.2064(3) 0.0639(3) 0.0126(6) Uani 1 1 d . . . . .
C1 C 0.5978(4) 0.1631(4) 0.4016(3) 0.0182(7) Uani 1 1 d . . . . .
H1 H 0.6701 0.1796 0.4964 0.022 Uiso 1 1 calc R . . . .
C4 C 0.3898(3) 0.1110(3) 0.1308(3) 0.0153(7) Uani 1 1 d . . . . .
H4 H 0.3188 0.0924 0.0349 0.018 Uiso 1 1 calc R . . . .
C2 C 0.4335(4) 0.1109(4) 0.3720(3) 0.0178(7) Uani 1 1 d . . . . .
H2 H 0.3943 0.0951 0.4449 0.021 Uiso 1 1 calc R . . . .
C9 C 0.7752(4) 0.2816(3) -0.1233(3) 0.0148(7) Uani 1 1 d . . . . .
H9 H 0.8277 0.3089 -0.1865 0.018 Uiso 1 1 calc R . . . .
C8 C 0.6104(4) 0.2397(3) -0.1674(3) 0.0166(7) Uani 1 1 d . . . . .
H8 H 0.5481 0.2379 -0.2613 0.020 Uiso 1 1 calc R . . . .
C12 C 1.1142(4) 0.3353(3) -0.0303(3) 0.0155(7) Uani 1 1 d . . . . .
H12 H 1.0501 0.3069 -0.1294 0.019 Uiso 1 1 calc R . . . .
C14 C 1.3720(4) 0.4265(3) 0.1648(4) 0.0172(7) Uani 1 1 d . . . . .
H14 H 1.4875 0.4652 0.2025 0.021 Uiso 1 1 calc R . . . .
C13 C 1.2819(4) 0.3855(3) 0.0207(4) 0.0177(7) Uani 1 1 d . . . . .
H13 H 1.3340 0.3915 -0.0429 0.021 Uiso 1 1 calc R . . . .
H1A H 0.836(4) -0.013(4) 0.467(4) 0.024(11) Uiso 1 1 d . . . . .
H1B H 0.942(5) 0.086(4) 0.591(5) 0.029(12) Uiso 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
La1 Cl1 2.8385(8) . ?
La1 Cl3 2.9209(8) 2_766 ?
La1 Cl3 2.8894(7) . ?
La1 Cl2 2.8014(8) . ?
La1 O1 2.576(2) . ?
La1 N1 2.638(2) . ?
La1 N3 2.659(2) . ?
La1 N2 2.677(2) . ?
Cl3 La1 2.9210(8) 2_766 ?
O1 H1A 0.78(4) . ?
O1 H1B 0.83(4) . ?
N1 C5 1.349(4) . ?
N1 C1 1.344(4) . ?
N3 C11 1.355(4) . ?
N3 C15 1.340(4) . ?
N2 C10 1.349(4) . ?
N2 C6 1.355(4) . ?
C10 C11 1.486(4) . ?
C10 C9 1.395(4) . ?
C11 C12 1.394(4) . ?
C15 H15 0.9500 . ?
C15 C14 1.385(4) . ?
C5 C6 1.490(4) . ?
C5 C4 1.395(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.376(4) . ?
C3 C2 1.386(5) . ?
C7 H7 0.9500 . ?
C7 C6 1.389(4) . ?
C7 C8 1.381(4) . ?
C1 H1 0.9500 . ?
C1 C2 1.382(4) . ?
C4 H4 0.9500 . ?
C2 H2 0.9500 . ?
C9 H9 0.9500 . ?
C9 C8 1.380(4) . ?
C8 H8 0.9500 . ?
C12 H12 0.9500 . ?
C12 C13 1.389(4) . ?
C14 H14 0.9500 . ?
C14 C13 1.377(5) . ?
C13 H13 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
Cl1 La1 Cl3 144.65(2) . 2_766 ?
Cl1 La1 Cl3 143.98(2) . . ?
Cl3 La1 Cl3 70.77(2) . 2_766 ?
Cl2 La1 Cl1 86.82(2) . . ?
Cl2 La1 Cl3 82.93(2) . 2_766 ?
Cl2 La1 Cl3 110.27(2) . . ?
O1 La1 Cl1 72.14(6) . . ?
O1 La1 Cl3 72.71(6) . 2_766 ?
O1 La1 Cl3 140.69(6) . . ?
O1 La1 Cl2 78.77(6) . . ?
O1 La1 N1 73.83(7) . . ?
O1 La1 N3 145.03(8) . . ?
O1 La1 N2 121.03(7) . . ?
N1 La1 Cl1 92.84(6) . . ?
N1 La1 Cl3 80.87(6) . 2_766 ?
N1 La1 Cl3 86.46(6) . . ?
N1 La1 Cl2 151.27(5) . . ?
N1 La1 N3 123.53(7) . . ?
N1 La1 N2 61.59(7) . . ?
N3 La1 Cl1 76.58(6) . . ?
N3 La1 Cl3 135.32(5) . 2_766 ?
N3 La1 Cl3 74.01(6) . . ?
N3 La1 Cl2 84.35(6) . . ?
N3 La1 N2 62.21(7) . . ?
N2 La1 Cl1 73.58(6) . . ?
N2 La1 Cl3 74.54(5) . . ?
N2 La1 Cl3 129.74(6) . 2_766 ?
N2 La1 Cl2 144.06(6) . . ?
La1 Cl3 La1 109.24(2) . 2_766 ?
La1 O1 H1A 116(3) . . ?
La1 O1 H1B 115(3) . . ?
H1A O1 H1B 113(4) . . ?
C5 N1 La1 122.86(19) . . ?
C1 N1 La1 119.1(2) . . ?
C1 N1 C5 117.9(3) . . ?
C11 N3 La1 120.09(17) . . ?
C15 N3 La1 120.76(19) . . ?
C15 N3 C11 118.0(3) . . ?
C10 N2 La1 120.40(19) . . ?
C10 N2 C6 118.3(3) . . ?
C6 N2 La1 121.20(19) . . ?
N2 C10 C11 117.7(3) . . ?
N2 C10 C9 122.1(3) . . ?
C9 C10 C11 120.2(3) . . ?
N3 C11 C10 117.7(3) . . ?
N3 C11 C12 121.5(3) . . ?
C12 C11 C10 120.8(3) . . ?
N3 C15 H15 118.2 . . ?
N3 C15 C14 123.6(3) . . ?
C14 C15 H15 118.2 . . ?
N1 C5 C6 116.9(2) . . ?
N1 C5 C4 121.5(3) . . ?
C4 C5 C6 121.6(3) . . ?
C4 C3 H3 120.3 . . ?
C4 C3 C2 119.4(3) . . ?
C2 C3 H3 120.3 . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C8 C7 C6 119.1(3) . . ?
N2 C6 C5 117.1(3) . . ?
N2 C6 C7 122.2(3) . . ?
C7 C6 C5 120.7(3) . . ?
N1 C1 H1 118.1 . . ?
N1 C1 C2 123.7(3) . . ?
C2 C1 H1 118.1 . . ?
C5 C4 H4 120.2 . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 H4 120.2 . . ?
C3 C2 H2 121.1 . . ?
C1 C2 C3 117.9(3) . . ?
C1 C2 H2 121.1 . . ?
C10 C9 H9 120.5 . . ?
C8 C9 C10 119.0(3) . . ?
C8 C9 H9 120.5 . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.3(3) . . ?
C9 C8 H8 120.4 . . ?
C11 C12 H12 120.4 . . ?
C13 C12 C11 119.2(3) . . ?
C13 C12 H12 120.4 . . ?
C15 C14 H14 120.8 . . ?
C13 C14 C15 118.4(3) . . ?
C13 C14 H14 120.8 . . ?
C12 C13 H13 120.4 . . ?
C14 C13 C12 119.2(3) . . ?
C14 C13 H13 120.4 . . ?

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
La1 N1 C5 C6 -6.5(4) . . . . ?
La1 N1 C5 C4 174.5(2) . . . . ?
La1 N1 C1 C2 -176.5(2) . . . . ?
La1 N3 C11 C10 17.0(3) . . . . ?
La1 N3 C11 C12 -164.0(2) . . . . ?
La1 N3 C15 C14 166.5(2) . . . . ?
La1 N2 C10 C11 4.4(3) . . . . ?
La1 N2 C10 C9 -174.9(2) . . . . ?
La1 N2 C6 C5 -3.8(3) . . . . ?
La1 N2 C6 C7 175.8(2) . . . . ?
N1 C5 C6 N2 6.6(4) . . . . ?
N1 C5 C6 C7 -173.0(3) . . . . ?
N1 C5 C4 C3 1.5(5) . . . . ?
N1 C1 C2 C3 2.0(5) . . . . ?
N3 C11 C12 C13 -3.0(4) . . . . ?
N3 C15 C14 C13 -2.0(5) . . . . ?
N2 C10 C11 N3 -14.1(4) . . . . ?
N2 C10 C11 C12 166.9(3) . . . . ?
N2 C10 C9 C8 -1.2(5) . . . . ?
C10 N2 C6 C5 179.8(3) . . . . ?
C10 N2 C6 C7 -0.5(4) . . . . ?
C10 C11 C12 C13 176.0(3) . . . . ?
C10 C9 C8 C7 -0.1(5) . . . . ?
C11 N3 C15 C14 -1.2(4) . . . . ?
C11 C10 C9 C8 179.6(3) . . . . ?
C11 C12 C13 C14 -0.3(4) . . . . ?
C15 N3 C11 C10 -175.3(3) . . . . ?
C15 N3 C11 C12 3.7(4) . . . . ?
C15 C14 C13 C12 2.7(4) . . . . ?
C5 N1 C1 C2 -0.3(5) . . . . ?
C6 N2 C10 C11 -179.3(3) . . . . ?
C6 N2 C10 C9 1.5(4) . . . . ?
C6 C5 C4 C3 -177.4(3) . . . . ?
C6 C7 C8 C9 1.0(5) . . . . ?
C1 N1 C5 C6 177.5(3) . . . . ?
C1 N1 C5 C4 -1.5(4) . . . . ?
C4 C5 C6 N2 -174.4(3) . . . . ?
C4 C5 C6 C7 5.9(4) . . . . ?
C4 C3 C2 C1 -1.9(5) . . . . ?
C2 C3 C4 C5 0.3(5) . . . . ?
C9 C10 C11 N3 165.2(3) . . . . ?
C9 C10 C11 C12 -13.8(4) . . . . ?
C8 C7 C6 N2 -0.7(5) . . . . ?
C8 C7 C6 C5 178.9(3) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.697
_oxdiff_exptl_absorpt_empirical_full_min 0.200
####################################################################### 
# 
# 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_2016fmm7662-54-2r_ml
_database_code_depnum_ccdc_archive 'CCDC 1590544'
_audit_update_record             
;
2018-02-27 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
_audit_creation_date             2018-02-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H30 Cl F3 N3 Sc Sn'
_chemical_formula_sum            'C12 H30 Cl F3 N3 Sc Sn'
_chemical_formula_weight         472.49
_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'
F F 0.0171 0.0103 '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'
Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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           8
_space_group_name_H-M_alt        'C 1 m 1'
_space_group_name_Hall           'C -2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'

_cell_length_a                   11.8495(10)
_cell_length_b                   9.2438(6)
_cell_length_c                   10.9099(7)
_cell_angle_alpha                90
_cell_angle_beta                 118.852(5)
_cell_angle_gamma                90
_cell_volume                     1046.67(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4432
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.3840
_cell_measurement_theta_min      2.1400
_shelx_estimated_absorpt_T_max   0.732
_shelx_estimated_absorpt_T_min   0.732
_exptl_absorpt_coefficient_mu    1.666
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.9g (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             476
_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by slow evaporation'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5546
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.499
_diffrn_reflns_theta_min         2.131
_diffrn_ambient_temperature      100(2)
_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 0.999
_diffrn_measurement_details      
'List of Runs (angles in degrees, time in seconds): # Type Start End Width tₑₓₚ ω θ κ φ Frames -------------------------------------------------------------------------- 1 ω -113.00 26.00 1.00 10.00 -- -23.00 -18.00 -90.00 139 2 ω -45.00 16.00 1.00 10.00 -- -23.00 -72.00 0.00 61 3 ω -44.00 -8.00 1.00 10.00 -- -23.00 72.00 -90.00 36 4 ω -41.00 -29.00 1.00 10.00 -- -23.00 18.00-180.00 12 5 ω -18.00 -8.00 1.00 10.00 -- -23.00 -54.00-150.00 10 6 ω -62.00 67.00 1.00 10.00 -- -23.00 72.00 30.00 129 7 ω -20.00 53.00 1.00 10.00 -- -23.00 54.00 -90.00 73'
_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 FRE-VHF'
_diffrn_measurement_device_type2 'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                2704
_reflns_number_total             2729
_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 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (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    ?
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 
;
 Flack x determined using 1276 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_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     132
_refine_ls_number_reflns         2729
_refine_ls_number_restraints     173
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0271
_refine_ls_restrained_S_all      1.040
_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)+(0.0369P)²+0.2475P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0641
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1B,H1C,H1A} of C1, {H4AA,H4AB,H4BA} of C4A, All C(H,H)
  groups
 At 1.5 times of:
  {H2AA,H2AB,H2AC} of C2A, {H3AA,H3AB,H3AC} of C3A, {H7A,H7B,H7C} of C7,
  {H3BA,H3BB,H3BC} of C3B, {H2BA,H2BB,H2BC} of C2B
2. Uiso/Uaniso restraints and constraints
Uanis(C5A) = Uanis(C5B)
Uanis(C6A) = Uanis(C6B)
Uanis(C3B) = Uanis(C3A)
Uanis(F2B) = Uanis(F2A)
Uanis(C2A) = Uanis(C2B)
Uanis(C4B) = Uanis(C4A)
3. 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
4. Others
 Fixed Sof: F2A(0.5) F2B(0.5) H1B(0.5) H1C(0.5) H1A(0.5) C2A(0.5) H2AA(0.5)
 H2AB(0.5) H2AC(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) C3B(0.5) H3BA(0.5)
 H3BB(0.5) H3BC(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) H4BA(0.5) C4B(0.5) H4BB(0.5)
 C5A(0.5) H5AA(0.5) H5AB(0.5) C5B(0.5) H5BA(0.5) H5BB(0.5) C6A(0.5) H6AA(0.5)
 H6AB(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
 C2B(0.5) H2BA(0.5) H2BB(0.5) H2BC(0.5)
5.a Riding coordinates:
 C1(H1B,H1C,H1A), C4A(H4AA,H4AB,H4BA), C4B(H4BB)
5.b Secondary CH2 refined with riding coordinates:
 C5A(H5AA,H5AB), C5B(H5BA,H5BB), C6A(H6AA,H6AB), C6B(H6BA,H6BB)
5.c Idealised Me refined as rotating group:
 C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,H3BC), C7(H7A,H7B,
 H7C), C2B(H2BA,H2BB,H2BC)
;
_atom_sites_solution_hydrogens   mixed
_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
Sn1 Sn 0.65234(2) 0.500000 1.32150(2) 0.02418(11) Uani 1 2 d S TU P . .
Sc1 Sc 0.41356(10) 0.500000 0.88425(11) 0.0201(2) Uani 1 2 d S TU P A .
Cl1 Cl 0.8220(2) 0.500000 1.5734(3) 0.0374(6) Uani 1 2 d S TU P A .
F1 F 0.4922(6) 0.500000 1.0908(6) 0.0412(16) Uani 1 2 d S TU P A 2
F2A F 0.498(3) 0.350(3) 0.840(3) 0.032(3) Uani 0.5 1 d . U . A 2
F2B F 0.497(3) 0.330(3) 0.869(3) 0.032(3) Uani 0.5 1 d . U . A 1
N1 N 0.2554(6) 0.500000 0.6493(6) 0.0248(12) Uani 1 2 d S TU P A .
N2 N 0.2517(3) 0.3445(4) 0.8729(4) 0.0235(7) Uani 1 1 d . U . . .
C1 C 0.4988(6) 0.500000 1.3698(8) 0.0432(18) Uani 1 2 d S TU P A .
H1B H 0.426563 0.443660 1.299203 0.052 Uiso 0.5 1 d R . . . .
H1C H 0.470743 0.599670 1.370093 0.052 Uiso 0.5 1 d R . . . .
H1A H 0.528213 0.456660 1.462213 0.052 Uiso 0.5 1 d R . . . .
C2A C 0.696(3) 0.712(3) 1.275(4) 0.049(5) Uani 0.5 1 d . U . A 1
H2AA H 0.789148 0.722616 1.315101 0.073 Uiso 0.5 1 calc GR . . A 1
H2AB H 0.663407 0.785135 1.315551 0.073 Uiso 0.5 1 calc GR . . A 1
H2AC H 0.654219 0.725144 1.173415 0.073 Uiso 0.5 1 calc GR . . A 1
C3A C 0.3140(10) 0.2401(11) 0.9945(11) 0.0300(16) Uani 0.5 1 d . U . B 1
H3AA H 0.390119 0.196524 0.996172 0.045 Uiso 0.5 1 calc GR . . B 1
H3AB H 0.252352 0.163959 0.983798 0.045 Uiso 0.5 1 calc GR . . B 1
H3AC H 0.339847 0.292263 1.082295 0.045 Uiso 0.5 1 calc GR . . B 1
C3B C 0.3101(10) 0.2018(11) 0.9337(11) 0.0300(16) Uani 0.5 1 d . U . B 2
H3BA H 0.338461 0.154277 0.872994 0.045 Uiso 0.5 1 calc GR . . B 2
H3BB H 0.245970 0.141094 0.941353 0.045 Uiso 0.5 1 calc GR . . B 2
H3BC H 0.384211 0.216224 1.026848 0.045 Uiso 0.5 1 calc GR . . B 2
C4A C 0.1951(10) 0.4157(12) 0.9463(10) 0.0228(14) Uani 0.5 1 d . U . B 2
H4AA H 0.258869 0.420090 1.047076 0.027 Uiso 0.5 1 d R . . B 2
H4AB H 0.120429 0.358490 0.936386 0.027 Uiso 0.5 1 d R . . B 2
H4BA H 0.131019 0.381900 0.959736 0.027 Uiso 0.5 1 d R . . B 1
C4B C 0.1511(9) 0.4333(12) 0.8930(10) 0.0228(14) Uani 0.5 1 d . U . B 1
H4BB H 0.070647 0.439138 0.802301 0.027 Uiso 0.5 1 d R . . B 1
C5A C 0.2003(9) 0.2707(12) 0.7426(10) 0.0259(15) Uani 0.5 1 d . U . A 1
H5AA H 0.127280 0.209177 0.730556 0.031 Uiso 0.5 1 calc R . . A 1
H5AB H 0.267255 0.207233 0.741880 0.031 Uiso 0.5 1 calc R . . A 1
C5B C 0.1519(10) 0.3160(12) 0.7170(10) 0.0259(15) Uani 0.5 1 d . U . A 2
H5BA H 0.130520 0.211625 0.704525 0.031 Uiso 0.5 1 calc R . . A 2
H5BB H 0.071820 0.369840 0.693690 0.031 Uiso 0.5 1 calc R . . A 2
C6A C 0.1549(10) 0.3769(13) 0.6237(11) 0.0269(16) Uani 0.5 1 d . U . A 1
H6AA H 0.073420 0.421512 0.609294 0.032 Uiso 0.5 1 calc R . . A 1
H6AB H 0.136545 0.324208 0.537092 0.032 Uiso 0.5 1 calc R . . A 1
C6B C 0.1993(10) 0.3602(13) 0.6163(11) 0.0269(16) Uani 0.5 1 d . U . A 2
H6BA H 0.263915 0.289347 0.620974 0.032 Uiso 0.5 1 calc R . . A 2
H6BB H 0.126284 0.359962 0.519649 0.032 Uiso 0.5 1 calc R . . A 2
C7 C 0.3224(9) 0.5414(10) 0.5668(8) 0.033(2) Uani 0.5 1 d . U . A -1
H7A H 0.349344 0.642832 0.585226 0.049 Uiso 0.5 1 calc GR . . A -1
H7B H 0.263107 0.528380 0.466660 0.049 Uiso 0.5 1 calc GR . . A -1
H7C H 0.398227 0.479722 0.594875 0.049 Uiso 0.5 1 calc GR . . A -1
C2B C 0.724(3) 0.681(3) 1.263(3) 0.049(5) Uani 0.5 1 d . U . A 2
H2BA H 0.815740 0.693642 1.329691 0.073 Uiso 0.5 1 calc GR . . A 2
H2BB H 0.676787 0.768183 1.264266 0.073 Uiso 0.5 1 calc GR . . A 2
H2BC H 0.712473 0.666753 1.169045 0.073 Uiso 0.5 1 calc GR . . A 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
Sn1 Cl1 2.503(2) . ?
Sn1 F1 2.308(6) . ?
Sn1 C1 2.124(7) . ?
Sn1 C2A 2.15(3) . ?
Sn1 C2A 2.15(3) 2_565 ?
Sn1 C2B 2.11(3) . ?
Sn1 C2B 2.11(3) 2_565 ?
Sc1 F1 1.980(6) . ?
Sc1 F2A 1.91(3) 2_565 ?
Sc1 F2A 1.91(3) . ?
Sc1 F2B 1.91(3) . ?
Sc1 F2B 1.91(3) 2_565 ?
Sc1 N1 2.334(6) . ?
Sc1 N2 2.352(4) 2_565 ?
Sc1 N2 2.352(4) . ?
N1 C6A 1.571(12) 2_565 ?
N1 C6A 1.571(12) . ?
N1 C6B 1.418(12) 2_565 ?
N1 C6B 1.418(12) . ?
N1 C7 1.509(10) . ?
N2 C3A 1.514(10) . ?
N2 C3B 1.488(11) . ?
N2 C4A 1.430(11) . ?
N2 C4B 1.548(11) . ?
N2 C5A 1.421(10) . ?
N2 C5B 1.556(10) . ?
C1 H1B 0.9799 2_565 ?
C1 H1B 0.9799 . ?
C1 H1C 0.9800 2_565 ?
C1 H1C 0.9800 . ?
C1 H1A 0.9799 . ?
C1 H1A 0.9799 2_565 ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C4A C4A 1.56(2) 2_565 ?
C4A H4AA 0.9901 . ?
C4A H4AB 0.9907 . ?
C4B H4BA 0.9903 . ?
C4B C4B 1.23(2) 2_565 ?
C4B H4BB 0.9900 . ?
C5A H5AA 0.9900 . ?
C5A H5AB 0.9900 . ?
C5A C6A 1.504(16) . ?
C5B H5BA 0.9900 . ?
C5B H5BB 0.9900 . ?
C5B C6B 1.511(14) . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C6B H6BA 0.9900 . ?
C6B H6BB 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?

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
F1 Sn1 Cl1 178.6(2) . . ?
C1 Sn1 Cl1 93.3(2) . . ?
C1 Sn1 F1 85.3(3) . . ?
C1 Sn1 C2A 112.9(6) . . ?
C1 Sn1 C2A 112.9(6) . 2_565 ?
C2A Sn1 Cl1 95.9(10) 2_565 . ?
C2A Sn1 Cl1 95.9(10) . . ?
C2A Sn1 C2A 131.7(10) . 2_565 ?
C2B Sn1 Cl1 96.0(9) 2_565 . ?
C2B Sn1 Cl1 96.0(9) . . ?
C2B Sn1 F1 84.9(10) . . ?
C2B Sn1 F1 84.9(10) 2_565 . ?
C2B Sn1 C1 126.2(6) . . ?
C2B Sn1 C1 126.2(6) 2_565 . ?
C2B Sn1 C2B 105.2(11) . 2_565 ?
F1 Sc1 N1 159.6(3) . . ?
F1 Sc1 N2 89.08(17) . . ?
F2A Sc1 F1 105.9(7) 2_565 . ?
F2A Sc1 F1 105.9(7) . . ?
F2A Sc1 F2A 93.6(14) 2_565 . ?
F2A Sc1 N1 87.8(8) . . ?
F2A Sc1 N1 87.8(8) 2_565 . ?
F2A Sc1 N2 161.2(10) 2_565 . ?
F2A Sc1 N2 93.2(9) . . ?
F2B Sc1 F2B 110.9(15) 2_565 . ?
F2B Sc1 N1 94.6(9) . . ?
F2B Sc1 N1 94.6(9) 2_565 . ?
F2B Sc1 N2 86.4(8) 2_565 2_565 ?
F2B Sc1 N2 160.7(10) . 2_565 ?
F2B Sc1 N2 160.7(10) 2_565 . ?
F2B Sc1 N2 86.4(8) . . ?
N1 Sc1 N2 74.92(14) . 2_565 ?
N1 Sc1 N2 74.92(14) . . ?
N2 Sc1 N2 75.36(18) . 2_565 ?
Sc1 F1 Sn1 158.3(3) . . ?
C6A N1 Sc1 109.4(5) 2_565 . ?
C6A N1 Sc1 109.4(5) . . ?
C6A N1 C6A 92.8(9) . 2_565 ?
C6B N1 Sc1 107.9(5) 2_565 . ?
C6B N1 Sc1 107.9(5) . . ?
C7 N1 Sc1 106.3(4) . . ?
C7 N1 C6A 106.4(6) . 2_565 ?
C7 N1 C6A 130.5(6) . . ?
C3A N2 Sc1 107.7(4) . . ?
C3A N2 C4B 107.3(6) . . ?
C3B N2 Sc1 109.1(4) . . ?
C3B N2 C5B 106.4(6) . . ?
C4A N2 Sc1 106.3(5) . . ?
C4A N2 C3B 113.6(6) . . ?
C4A N2 C5B 112.1(6) . . ?
C4B N2 Sc1 109.4(4) . . ?
C5A N2 Sc1 106.9(4) . . ?
C5A N2 C3A 111.3(6) . . ?
C5A N2 C4B 114.1(6) . . ?
C5B N2 Sc1 109.4(4) . . ?
Sn1 C1 H1B 109.5 . . ?
Sn1 C1 H1B 109.46(16) . 2_565 ?
Sn1 C1 H1C 109.470(15) . 2_565 ?
Sn1 C1 H1C 109.5 . . ?
Sn1 C1 H1A 109.5 . . ?
Sn1 C1 H1A 109.45(18) . 2_565 ?
H1B C1 H1B 64.2 . 2_565 ?
H1B C1 H1C 109.5 2_565 2_565 ?
H1B C1 H1C 48.3 . 2_565 ?
H1B C1 H1C 109.5 . . ?
H1B C1 H1A 140.2 . 2_565 ?
H1B C1 H1A 109.5 2_565 2_565 ?
H1B C1 H1A 109.5 . . ?
H1C C1 H1B 48.3 . 2_565 ?
H1C C1 H1C 140.2 . 2_565 ?
H1C C1 H1A 109.5 2_565 2_565 ?
H1C C1 H1A 109.5 . . ?
H1C C1 H1A 64.2 . 2_565 ?
H1A C1 H1B 140.2 . 2_565 ?
H1A C1 H1C 64.2 . 2_565 ?
H1A C1 H1A 48.3 . 2_565 ?
Sn1 C2A H2AA 109.5 . . ?
Sn1 C2A H2AB 109.5 . . ?
Sn1 C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
N2 C3A H3AA 109.5 . . ?
N2 C3A H3AB 109.5 . . ?
N2 C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
N2 C3B H3BA 109.5 . . ?
N2 C3B H3BB 109.5 . . ?
N2 C3B H3BC 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
N2 C4A C4A 117.4(5) . 2_565 ?
N2 C4A H4AA 109.1 . . ?
N2 C4A H4AB 109.2 . . ?
C4A C4A H4AA 87.7 2_565 . ?
C4A C4A H4AB 122.3 2_565 . ?
H4AA C4A H4AB 107.8 . . ?
N2 C4B H4BA 108.9 . . ?
N2 C4B H4BB 108.9 . . ?
H4BA C4B H4BB 107.7 . . ?
C4B C4B N2 122.0(4) 2_565 . ?
C4B C4B H4BA 118.7 2_565 . ?
C4B C4B H4BB 86.9 2_565 . ?
N2 C5A H5AA 109.5 . . ?
N2 C5A H5AB 109.5 . . ?
N2 C5A C6A 110.6(8) . . ?
H5AA C5A H5AB 108.1 . . ?
C6A C5A H5AA 109.5 . . ?
C6A C5A H5AB 109.5 . . ?
N2 C5B H5BA 108.9 . . ?
N2 C5B H5BB 108.9 . . ?
H5BA C5B H5BB 107.7 . . ?
C6B C5B N2 113.3(7) . . ?
C6B C5B H5BA 108.9 . . ?
C6B C5B H5BB 108.9 . . ?
N1 C6A H6AA 108.9 . . ?
N1 C6A H6AB 108.9 . . ?
C5A C6A N1 113.2(8) . . ?
C5A C6A H6AA 108.9 . . ?
C5A C6A H6AB 108.9 . . ?
H6AA C6A H6AB 107.7 . . ?
N1 C6B C5B 110.8(8) . . ?
N1 C6B H6BA 109.5 . . ?
N1 C6B H6BB 109.5 . . ?
C5B C6B H6BA 109.5 . . ?
C5B C6B H6BB 109.5 . . ?
H6BA C6B H6BB 108.1 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Sn1 C2B H2BA 109.5 . . ?
Sn1 C2B H2BB 109.5 . . ?
Sn1 C2B H2BC 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?

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 N1 C6A C5A -13.6(9) . . . . ?
Sc1 N1 C6B C5B 53.9(9) . . . . ?
Sc1 N2 C4A C4A 29.7(3) . . . 2_565 ?
Sc1 N2 C4B C4B 9.8(4) . . . 2_565 ?
Sc1 N2 C5A C6A -55.1(8) . . . . ?
Sc1 N2 C5B C6B 14.8(9) . . . . ?
N2 C5A C6A N1 47.1(10) . . . . ?
N2 C5B C6B N1 -46.8(11) . . . . ?
C3A N2 C4B C4B 126.4(5) . . . 2_565 ?
C3A N2 C5A C6A -172.4(7) . . . . ?
C3B N2 C4A C4A 149.6(5) . . . 2_565 ?
C3B N2 C5B C6B -102.9(9) . . . . ?
C4A N2 C5B C6B 132.4(9) . . . . ?
C4B N2 C5A C6A 66.0(9) . . . . ?
C5A N2 C4B C4B -109.9(6) . . . 2_565 ?
C5B N2 C4A C4A -89.8(6) . . . 2_565 ?
C6A N1 C6A C5A -125.4(7) 2_565 . . . ?
C6B N1 C6B C5B -82.0(14) 2_565 . . . ?
C7 N1 C6A C5A 120.2(9) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_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
- Detector area scaling
;
####################################################################### 
# 
# 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_2016fmm7662-33dr
_database_code_depnum_ccdc_archive 'CCDC 1590540'
_audit_update_record             
;
2017-12-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
_audit_creation_date             2017-06-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C9 H21 Cl F2 N3 Sc'
_chemical_formula_sum            'C9 H21 Cl F2 N3 Sc'
_chemical_formula_weight         289.70
_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'
F F 0.0171 0.0103 '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'
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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.9938(9)
_cell_length_b                   6.8826(7)
_cell_length_c                   15.8721(19)
_cell_angle_alpha                90
_cell_angle_beta                 90.292(8)
_cell_angle_gamma                90
_cell_volume                     1310.2(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2643
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.7050
_cell_measurement_theta_min      2.5930
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       chip
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.051
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.021
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1744
_diffrn_reflns_av_unetI/netI     0.1629
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7730
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.567
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_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    -84.00  36.00   1.00   10.00    --  -23.00  18.00 -90.00  120
  2  ω    -59.00  67.00   1.00   10.00    --  -23.00  54.00 -90.00  126
  3  ω    -62.00 -52.00   1.00   10.00    --  -23.00  72.00-120.00   10
  4  ω   -113.00 -20.00   1.00   10.00    --  -23.00 -18.00 150.00   93
;
_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0449676000
_diffrn_orient_matrix_UB_12      -0.0661267000
_diffrn_orient_matrix_UB_13      0.0045863000
_diffrn_orient_matrix_UB_21      -0.0362698000
_diffrn_orient_matrix_UB_22      -0.0680030000
_diffrn_orient_matrix_UB_23      0.0192278000
_diffrn_orient_matrix_UB_31      -0.0125075000
_diffrn_orient_matrix_UB_32      -0.0401779000
_diffrn_orient_matrix_UB_33      -0.0401258000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1550
_reflns_number_total             2568
_reflns_odcompleteness_completeness 91.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.38
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.016
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2568
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.0724
_refine_ls_restrained_S_all      0.982
_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)+(0.0984P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.2063
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C3(H3A,H3B), C5(H5A,H5B), C4(H4A,H4B), C2(H2A,H2B), C1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C)
;
_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
Sc1 Sc 0.26066(7) 0.48817(15) 0.12170(7) 0.0155(3) Uani 1 1 d . . . . .
Cl1 Cl 0.25122(10) 0.4226(2) 0.27281(10) 0.0281(4) Uani 1 1 d . . . . .
F1 F 0.1469(2) 0.3133(4) 0.0776(2) 0.0263(9) Uani 1 1 d . . . . .
F2 F 0.3989(2) 0.3602(5) 0.0914(2) 0.0240(8) Uani 1 1 d . . . . .
N3 N 0.1272(3) 0.7380(6) 0.1372(3) 0.0170(11) Uani 1 1 d . . . . .
N2 N 0.3638(3) 0.7732(6) 0.1394(3) 0.0148(11) Uani 1 1 d . . . . .
N1 N 0.2533(3) 0.6459(8) -0.0087(3) 0.0240(12) Uani 1 1 d . . . . .
C6 C 0.1344(4) 0.7048(10) -0.0188(4) 0.0294(16) Uani 1 1 d . . . . .
H6A H 0.0870 0.5873 -0.0228 0.035 Uiso 1 1 calc R . . . .
H6B H 0.1254 0.7794 -0.0717 0.035 Uiso 1 1 calc R . . . .
C8 C 0.4539(4) 0.7437(8) 0.2027(4) 0.0187(13) Uani 1 1 d . . . . .
H8A H 0.4214 0.7383 0.2592 0.028 Uiso 1 1 calc GR . . . .
H8B H 0.5069 0.8518 0.1998 0.028 Uiso 1 1 calc GR . . . .
H8C H 0.4928 0.6215 0.1910 0.028 Uiso 1 1 calc GR . . . .
C3 C 0.2927(4) 0.9440(8) 0.1641(4) 0.0232(14) Uani 1 1 d . . . . .
H3A H 0.2831 1.0308 0.1149 0.028 Uiso 1 1 calc R . . . .
H3B H 0.3313 1.0185 0.2090 0.028 Uiso 1 1 calc R . . . .
C5 C 0.0968(4) 0.8275(8) 0.0545(4) 0.0233(14) Uani 1 1 d . . . . .
H5A H 0.1315 0.9577 0.0505 0.028 Uiso 1 1 calc R . . . .
H5B H 0.0149 0.8445 0.0515 0.028 Uiso 1 1 calc R . . . .
C4 C 0.1788(4) 0.8809(8) 0.1955(4) 0.0222(14) Uani 1 1 d . . . . .
H4A H 0.1867 0.8222 0.2521 0.027 Uiso 1 1 calc R . . . .
H4B H 0.1298 0.9960 0.2003 0.027 Uiso 1 1 calc R . . . .
C9 C 0.0261(4) 0.6574(9) 0.1780(4) 0.0228(14) Uani 1 1 d . . . . .
H9A H -0.0082 0.5603 0.1408 0.034 Uiso 1 1 calc GR . . . .
H9B H -0.0272 0.7624 0.1885 0.034 Uiso 1 1 calc GR . . . .
H9C H 0.0469 0.5961 0.2315 0.034 Uiso 1 1 calc GR . . . .
C2 C 0.4171(4) 0.8079(10) 0.0558(4) 0.0313(17) Uani 1 1 d . . . . .
H2A H 0.4705 0.7018 0.0439 0.038 Uiso 1 1 calc R . . . .
H2B H 0.4593 0.9315 0.0577 0.038 Uiso 1 1 calc R . . . .
C1 C 0.3303(5) 0.8175(11) -0.0149(4) 0.0339(17) Uani 1 1 d . . . . .
H1A H 0.2869 0.9395 -0.0102 0.041 Uiso 1 1 calc R . . . .
H1B H 0.3680 0.8169 -0.0702 0.041 Uiso 1 1 calc R . . . .
C7 C 0.2801(5) 0.4982(11) -0.0746(4) 0.0396(18) Uani 1 1 d . . . . .
H7A H 0.3586 0.4602 -0.0694 0.059 Uiso 1 1 calc GR . . . .
H7B H 0.2668 0.5539 -0.1306 0.059 Uiso 1 1 calc GR . . . .
H7C H 0.2327 0.3837 -0.0670 0.059 Uiso 1 1 calc GR . . . .


_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 Cl1 2.444(2) . ?
Sc1 F1 1.948(3) . ?
Sc1 F2 1.940(3) . ?
Sc1 N3 2.363(4) . ?
Sc1 N2 2.336(4) . ?
Sc1 N1 2.339(5) . ?
N3 C5 1.494(7) . ?
N3 C4 1.484(7) . ?
N3 C9 1.485(6) . ?
N2 C8 1.486(6) . ?
N2 C3 1.506(7) . ?
N2 C2 1.494(7) . ?
N1 C6 1.490(6) . ?
N1 C1 1.503(8) . ?
N1 C7 1.495(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C5 1.509(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.520(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.529(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

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
F1 Sc1 Cl1 101.72(11) . . ?
F1 Sc1 N3 90.76(14) . . ?
F1 Sc1 N2 158.78(14) . . ?
F1 Sc1 N1 86.85(15) . . ?
F2 Sc1 Cl1 101.71(11) . . ?
F2 Sc1 F1 103.23(14) . . ?
F2 Sc1 N3 159.46(15) . . ?
F2 Sc1 N2 87.58(14) . . ?
F2 Sc1 N1 91.16(15) . . ?
N3 Sc1 Cl1 89.84(13) . . ?
N2 Sc1 Cl1 93.70(12) . . ?
N2 Sc1 N3 74.65(14) . . ?
N2 Sc1 N1 74.57(16) . . ?
N1 Sc1 Cl1 162.31(14) . . ?
N1 Sc1 N3 74.44(17) . . ?
C5 N3 Sc1 111.8(3) . . ?
C4 N3 Sc1 105.4(3) . . ?
C4 N3 C5 111.9(4) . . ?
C4 N3 C9 108.4(4) . . ?
C9 N3 Sc1 109.2(3) . . ?
C9 N3 C5 109.9(4) . . ?
C8 N2 Sc1 110.4(3) . . ?
C8 N2 C3 109.9(4) . . ?
C8 N2 C2 108.1(4) . . ?
C3 N2 Sc1 112.8(3) . . ?
C2 N2 Sc1 104.9(3) . . ?
C2 N2 C3 110.6(4) . . ?
C6 N1 Sc1 104.7(3) . . ?
C6 N1 C1 111.5(5) . . ?
C6 N1 C7 108.6(4) . . ?
C1 N1 Sc1 113.7(3) . . ?
C7 N1 Sc1 107.2(4) . . ?
C7 N1 C1 110.7(5) . . ?
N1 C6 H6A 109.4 . . ?
N1 C6 H6B 109.4 . . ?
N1 C6 C5 111.0(4) . . ?
H6A C6 H6B 108.0 . . ?
C5 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C3 H3A 109.2 . . ?
N2 C3 H3B 109.2 . . ?
N2 C3 C4 111.9(4) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
N3 C5 C6 112.0(5) . . ?
N3 C5 H5A 109.2 . . ?
N3 C5 H5B 109.2 . . ?
C6 C5 H5A 109.2 . . ?
C6 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
N3 C4 C3 111.0(5) . . ?
N3 C4 H4A 109.4 . . ?
N3 C4 H4B 109.4 . . ?
C3 C4 H4A 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
N2 C2 C1 111.4(4) . . ?
H2A C2 H2B 108.0 . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
N1 C1 C2 109.6(5) . . ?
N1 C1 H1A 109.8 . . ?
N1 C1 H1B 109.8 . . ?
C2 C1 H1A 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_olex2_exptl_crystal_mounting_method MiTeGen
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.070
_oxdiff_exptl_absorpt_empirical_full_min 0.188

_vrf_RINTA01_2016fmm7662-33dr    


;
PROBLEM:    The value of Rint is greater than 0.12   
RESPONSE: This is due to the size of the crystal. Only small crystals were found. 
;

_vrf_PLAT020_2016fmm7662-33dr    


;
PROBLEM:    The value of Rint is greater than 0.12   
RESPONSE: This is due to the size of the crystal. Only small crystals were found. 
;
####################################################################### 
# 
# 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_2016fmm7662-37a2ndr
_database_code_depnum_ccdc_archive 'CCDC 1590541'
_audit_update_record             
;
2017-12-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
_audit_creation_date             2016-05-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C9 H21 I3 N3 Y, C2 H3 N'
_chemical_formula_sum            'C11 H24 I3 N4 Y'
_chemical_formula_weight         681.95
_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'
I I -0.4742 1.8119 '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'
Y Y -2.7962 3.5667 '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                   10.5669(5)
_cell_length_b                   15.9059(7)
_cell_length_c                   11.7484(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.139(5)
_cell_angle_gamma                90
_cell_volume                     1974.61(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6512
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4390
_cell_measurement_theta_min      2.3040
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.294
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       chip
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.038
_exptl_crystal_size_mid          0.024
_exptl_crystal_size_min          0.016
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13372
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.733
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00  67.00   1.00    7.00    --  -23.00   0.00 -60.00  180
  2  ω    -57.00  16.00   1.00    7.00    --  -23.00 -72.00 -60.00   73
  3  ω    -78.00  11.00   1.00    7.00    --  -23.00 -72.00 120.00   89
;
_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_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0568792000
_diffrn_orient_matrix_UB_12      0.0192559000
_diffrn_orient_matrix_UB_13      0.0189033000
_diffrn_orient_matrix_UB_21      0.0338518000
_diffrn_orient_matrix_UB_22      -0.0373210000
_diffrn_orient_matrix_UB_23      -0.0127101000
_diffrn_orient_matrix_UB_31      0.0113121000
_diffrn_orient_matrix_UB_32      0.0150069000
_diffrn_orient_matrix_UB_33      -0.0558846000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3327
_reflns_number_total             3887
_reflns_odcompleteness_completeness 91.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.31
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3887
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0391
_refine_ls_restrained_S_all      1.004
_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)+(0.0233P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0686
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.7876(8) 0.2124(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B), C1(H1A,H1B), C6(H6A,H6B)
3.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C)
;
_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
I1 I 0.33924(5) 0.11661(3) 0.08026(4) 0.01532(13) Uani 1 1 d . . . . .
I2 I 0.65998(5) 0.25031(3) 0.25992(4) 0.01862(13) Uani 1 1 d . . . . .
I3 I 0.37083(5) 0.10298(3) 0.45413(4) 0.01668(14) Uani 1 1 d . . . . .
Y1 Y 0.38259(7) 0.23215(4) 0.27476(6) 0.01061(17) Uani 1 1 d . . . . .
N2 N 0.3606(6) 0.3519(3) 0.4085(5) 0.0101(14) Uani 1 1 d . . . . .
N3 N 0.1555(7) 0.2640(4) 0.2968(5) 0.0137(14) Uani 1 1 d . . . . .
N1 N 0.3338(6) 0.3591(4) 0.1622(5) 0.0120(14) Uani 1 1 d . . . . .
C9 C 0.0734(7) 0.1880(4) 0.2847(6) 0.0151(18) Uani 1 1 d . . . . .
H9A H 0.0805 0.1658 0.2072 0.023 Uiso 1 1 calc GR . . . .
H9B H -0.0148 0.2034 0.2998 0.023 Uiso 1 1 calc GR . . . .
H9C H 0.1005 0.1450 0.3393 0.023 Uiso 1 1 calc GR . . . .
C5 C 0.1078(7) 0.3309(4) 0.2164(6) 0.0135(17) Uani 1 1 d . . . . .
H5A H 0.0944 0.3839 0.2590 0.016 Uiso 1 1 calc R . . . .
H5B H 0.0254 0.3132 0.1841 0.016 Uiso 1 1 calc R . . . .
C8 C 0.4397(8) 0.3399(5) 0.5108(6) 0.0171(19) Uani 1 1 d . . . . .
H8A H 0.4095 0.2909 0.5533 0.026 Uiso 1 1 calc GR . . . .
H8B H 0.4342 0.3901 0.5591 0.026 Uiso 1 1 calc GR . . . .
H8C H 0.5278 0.3310 0.4881 0.026 Uiso 1 1 calc GR . . . .
C4 C 0.1404(8) 0.2928(4) 0.4172(6) 0.0152(18) Uani 1 1 d . . . . .
H4A H 0.1601 0.2456 0.4692 0.018 Uiso 1 1 calc R . . . .
H4B H 0.0512 0.3094 0.4299 0.018 Uiso 1 1 calc R . . . .
C7 C 0.4183(8) 0.3668(4) 0.0615(7) 0.0185(19) Uani 1 1 d . . . . .
H7A H 0.5060 0.3736 0.0872 0.028 Uiso 1 1 calc GR . . . .
H7B H 0.3931 0.4158 0.0163 0.028 Uiso 1 1 calc GR . . . .
H7C H 0.4113 0.3159 0.0148 0.028 Uiso 1 1 calc GR . . . .
C3 C 0.2260(7) 0.3664(5) 0.4449(6) 0.0148(18) Uani 1 1 d . . . . .
H3A H 0.1932 0.4174 0.4064 0.018 Uiso 1 1 calc R . . . .
H3B H 0.2241 0.3768 0.5279 0.018 Uiso 1 1 calc R . . . .
C2 C 0.4127(8) 0.4248(4) 0.3415(6) 0.0121(17) Uani 1 1 d . . . . .
H2A H 0.4072 0.4765 0.3883 0.014 Uiso 1 1 calc R . . . .
H2B H 0.5031 0.4144 0.3249 0.014 Uiso 1 1 calc R . . . .
C1 C 0.3426(8) 0.4384(4) 0.2317(6) 0.0155(17) Uani 1 1 d . . . . .
H1A H 0.3865 0.4822 0.1867 0.019 Uiso 1 1 calc R . . . .
H1B H 0.2562 0.4589 0.2485 0.019 Uiso 1 1 calc R . . . .
C6 C 0.2012(7) 0.3463(4) 0.1202(6) 0.0129(18) Uani 1 1 d . . . . .
H6A H 0.1995 0.2977 0.0676 0.015 Uiso 1 1 calc R . . . .
H6B H 0.1743 0.3967 0.0768 0.015 Uiso 1 1 calc R . . . .
N4 N 0.6238(8) 0.5354(4) 0.2183(7) 0.0315(19) Uani 1 1 d . . . . .
C11 C 0.8530(8) 0.4901(5) 0.2620(7) 0.0238(19) Uani 1 1 d . . . . .
H11A H 0.9079 0.5051 0.1980 0.036 Uiso 1 1 calc GR . . . .
H11B H 0.8558 0.4292 0.2740 0.036 Uiso 1 1 calc GR . . . .
H11C H 0.8823 0.5189 0.3309 0.036 Uiso 1 1 calc GR . . . .
C10 C 0.7239(8) 0.5156(5) 0.2368(7) 0.0191(19) 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
I1 Y1 2.9672(8) . ?
I2 Y1 2.9509(9) . ?
I3 Y1 2.9460(8) . ?
Y1 N2 2.480(6) . ?
Y1 N3 2.466(7) . ?
Y1 N1 2.468(6) . ?
N2 C8 1.474(9) . ?
N2 C3 1.504(10) . ?
N2 C2 1.507(9) . ?
N3 C9 1.495(9) . ?
N3 C5 1.509(8) . ?
N3 C4 1.496(9) . ?
N1 C7 1.489(9) . ?
N1 C1 1.504(8) . ?
N1 C6 1.498(10) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.523(10) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.515(10) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.502(9) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
N4 C10 1.125(10) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C11 C10 1.452(11) . ?

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
I2 Y1 I1 99.59(3) . . ?
I3 Y1 I1 96.44(2) . . ?
I3 Y1 I2 98.87(3) . . ?
N2 Y1 I1 161.62(14) . . ?
N2 Y1 I2 93.26(15) . . ?
N2 Y1 I3 94.48(13) . . ?
N3 Y1 I1 93.40(13) . . ?
N3 Y1 I2 162.33(13) . . ?
N3 Y1 I3 91.45(13) . . ?
N3 Y1 N2 71.5(2) . . ?
N3 Y1 N1 71.7(2) . . ?
N1 Y1 I1 93.59(14) . . ?
N1 Y1 I2 95.43(16) . . ?
N1 Y1 I3 160.89(15) . . ?
N1 Y1 N2 72.02(18) . . ?
C8 N2 Y1 111.4(4) . . ?
C8 N2 C3 108.8(6) . . ?
C8 N2 C2 108.5(6) . . ?
C3 N2 Y1 112.8(4) . . ?
C3 N2 C2 112.1(6) . . ?
C2 N2 Y1 103.0(4) . . ?
C9 N3 Y1 112.9(4) . . ?
C9 N3 C5 108.5(6) . . ?
C9 N3 C4 105.9(6) . . ?
C5 N3 Y1 113.8(5) . . ?
C4 N3 Y1 105.6(4) . . ?
C4 N3 C5 109.8(5) . . ?
C7 N1 Y1 111.6(4) . . ?
C7 N1 C1 109.0(6) . . ?
C7 N1 C6 108.1(6) . . ?
C1 N1 Y1 112.5(4) . . ?
C6 N1 Y1 105.1(4) . . ?
C6 N1 C1 110.5(6) . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C5 H5A 109.4 . . ?
N3 C5 H5B 109.4 . . ?
N3 C5 C6 111.2(6) . . ?
H5A C5 H5B 108.0 . . ?
C6 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C4 H4A 109.2 . . ?
N3 C4 H4B 109.2 . . ?
N3 C4 C3 112.0(6) . . ?
H4A C4 H4B 107.9 . . ?
C3 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C3 C4 112.6(6) . . ?
N2 C3 H3A 109.1 . . ?
N2 C3 H3B 109.1 . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
N2 C2 H2A 109.1 . . ?
N2 C2 H2B 109.1 . . ?
H2A C2 H2B 107.9 . . ?
C1 C2 N2 112.3(6) . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
N1 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 N1 112.1(6) . . ?
C2 C1 H1A 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
N1 C6 C5 112.6(6) . . ?
N1 C6 H6A 109.1 . . ?
N1 C6 H6B 109.1 . . ?
C5 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
N4 C10 C11 179.4(10) . . ?

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
Y1 N2 C3 C4 14.9(7) . . . . ?
Y1 N2 C2 C1 58.3(6) . . . . ?
Y1 N3 C5 C6 15.2(7) . . . . ?
Y1 N3 C4 C3 56.0(6) . . . . ?
Y1 N1 C1 C2 15.9(8) . . . . ?
Y1 N1 C6 C5 56.3(6) . . . . ?
N2 C2 C1 N1 -52.1(9) . . . . ?
N3 C5 C6 N1 -49.4(8) . . . . ?
N3 C4 C3 N2 -48.8(8) . . . . ?
C9 N3 C5 C6 -111.4(7) . . . . ?
C9 N3 C4 C3 175.9(6) . . . . ?
C5 N3 C4 C3 -67.1(8) . . . . ?
C8 N2 C3 C4 -109.3(7) . . . . ?
C8 N2 C2 C1 176.5(6) . . . . ?
C4 N3 C5 C6 133.3(6) . . . . ?
C7 N1 C1 C2 -108.4(7) . . . . ?
C7 N1 C6 C5 175.6(6) . . . . ?
C3 N2 C2 C1 -63.3(8) . . . . ?
C2 N2 C3 C4 130.7(6) . . . . ?
C1 N1 C6 C5 -65.2(7) . . . . ?
C6 N1 C1 C2 132.9(6) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.077
_oxdiff_exptl_absorpt_empirical_full_min 0.494
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.7876(8)
2 0.2124(8)

####################################################################### 
# 
# 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_2016fmm7662-37ar
_database_code_depnum_ccdc_archive 'CCDC 1590542'
_audit_update_record             
;
2017-12-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
_audit_creation_date             2016-05-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C9 H21 I2 N3 O0.5 Y), C2 H3 N'
_chemical_formula_sum            'C20 H45 I4 N7 O Y2'
_chemical_formula_weight         1085.05
_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'
I I -0.4742 1.8119 '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'
Y Y -2.7962 3.5667 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6352(3)
_cell_length_b                   8.6395(3)
_cell_length_c                   23.7313(8)
_cell_angle_alpha                90.160(3)
_cell_angle_beta                 90.941(3)
_cell_angle_gamma                108.966(3)
_cell_volume                     1674.05(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7741
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0750
_cell_measurement_theta_min      2.4580
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.162
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.153
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.067
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.026
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11161
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.494
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00   1.00   1.00   10.00    --  -23.00 -18.00   0.00  114
  2  ω    -62.00  53.00   1.00   10.00    --  -23.00  72.00 120.00  115
  3  ω    -88.00  15.00   1.00   10.00    --  -23.00 -72.00 -60.00  103
  4  ω    -39.00 -27.00   1.00    5.00    --  -23.00 -72.00-120.00   12
;
_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_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0183563000
_diffrn_orient_matrix_UB_12      -0.0308259000
_diffrn_orient_matrix_UB_13      0.0276391000
_diffrn_orient_matrix_UB_21      0.0740451000
_diffrn_orient_matrix_UB_22      -0.0188341000
_diffrn_orient_matrix_UB_23      0.0011280000
_diffrn_orient_matrix_UB_31      0.0415589000
_diffrn_orient_matrix_UB_32      0.0789425000
_diffrn_orient_matrix_UB_33      0.0113412000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5686
_reflns_number_total             6471
_reflns_odcompleteness_completeness 85.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.31
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.448
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6471
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0354
_refine_ls_restrained_S_all      1.118
_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)+(0.0370P)²+5.4138P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0847
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C2(H2A,H2B), C12(H12A,H12B), C5(H5A,H5B), C4(H4A,
 H4B), C6(H6A,H6B), C10(H10A,H10B), C11(H11A,H11B), C15(H15A,H15B), C13(H13A,
 H13B), C14(H14A,H14B)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C7(H7A,H7B,H7C),
 C18(H18A,H18B,H18C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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
I1 I 0.17970(5) 0.32071(5) 0.86758(2) 0.02062(10) Uani 1 1 d . . . . .
I2 I -0.34707(5) 0.20745(5) 0.89752(2) 0.02580(11) Uani 1 1 d . . . . .
Y2 Y 0.48659(6) 0.43307(6) 0.58230(2) 0.01148(12) Uani 1 1 d . . . . .
Y1 Y -0.04190(6) 0.49445(6) 0.91534(2) 0.01156(12) Uani 1 1 d . . . . .
I4 I 0.66151(4) 0.18319(4) 0.59024(2) 0.01722(10) Uani 1 1 d . . . . .
I3 I 0.76453(5) 0.70073(4) 0.63676(2) 0.01896(10) Uani 1 1 d . . . . .
O1 O 0.0000 0.5000 1.0000 0.0146(11) Uani 1 2 d S T P . .
N2 N -0.0639(6) 0.6147(6) 0.8173(2) 0.0162(10) Uani 1 1 d . . . . .
N1 N 0.1559(6) 0.7737(5) 0.90657(19) 0.0146(10) Uani 1 1 d . . . . .
N3 N -0.1941(6) 0.6950(6) 0.9197(2) 0.0189(11) Uani 1 1 d . . . . .
N5 N 0.2708(6) 0.5577(5) 0.60111(19) 0.0140(10) Uani 1 1 d . . . . .
N6 N 0.3352(6) 0.3177(6) 0.6748(2) 0.0210(11) Uani 1 1 d . . . . .
N4 N 0.2163(6) 0.2236(6) 0.5613(2) 0.0185(10) Uani 1 1 d . . . . .
O2 O 0.5000 0.5000 0.5000 0.0154(11) Uani 1 2 d S T P . .
C16 C 0.2427(7) 0.1167(7) 0.5174(2) 0.0175(12) Uani 1 1 d . . . . .
H16A H 0.3124 0.1831 0.4883 0.026 Uiso 1 1 calc GR . . . .
H16B H 0.1371 0.0520 0.5005 0.026 Uiso 1 1 calc GR . . . .
H16C H 0.2964 0.0431 0.5340 0.026 Uiso 1 1 calc GR . . . .
C1 C 0.1786(8) 0.8457(7) 0.8492(2) 0.0212(13) Uani 1 1 d . . . . .
H1A H 0.2969 0.8986 0.8425 0.025 Uiso 1 1 calc R . . . .
H1B H 0.1251 0.9310 0.8467 0.025 Uiso 1 1 calc R . . . .
C8 C -0.1180(7) 0.4787(7) 0.7750(2) 0.0189(12) Uani 1 1 d . . . . .
H8A H -0.0471 0.4106 0.7780 0.028 Uiso 1 1 calc GR . . . .
H8B H -0.1110 0.5245 0.7370 0.028 Uiso 1 1 calc GR . . . .
H8C H -0.2314 0.4119 0.7822 0.028 Uiso 1 1 calc GR . . . .
C3 C -0.1789(8) 0.7121(8) 0.8155(3) 0.0238(14) Uani 1 1 d . . . . .
H3A H -0.2470 0.6841 0.7806 0.029 Uiso 1 1 calc R . . . .
H3B H -0.1148 0.8301 0.8143 0.029 Uiso 1 1 calc R . . . .
C17 C 0.3234(8) 0.7257(7) 0.5784(3) 0.0219(13) Uani 1 1 d . . . . .
H17A H 0.4360 0.7840 0.5911 0.033 Uiso 1 1 calc GR . . . .
H17B H 0.2507 0.7838 0.5919 0.033 Uiso 1 1 calc GR . . . .
H17C H 0.3186 0.7207 0.5371 0.033 Uiso 1 1 calc GR . . . .
C2 C 0.1075(8) 0.7181(7) 0.8046(3) 0.0220(13) Uani 1 1 d . . . . .
H2A H 0.1080 0.7724 0.7678 0.026 Uiso 1 1 calc R . . . .
H2B H 0.1769 0.6472 0.8013 0.026 Uiso 1 1 calc R . . . .
C12 C 0.2575(8) 0.5684(8) 0.6632(3) 0.0263(14) Uani 1 1 d . . . . .
H12A H 0.1684 0.6133 0.6716 0.032 Uiso 1 1 calc R . . . .
H12B H 0.3609 0.6462 0.6785 0.032 Uiso 1 1 calc R . . . .
C7 C 0.3153(7) 0.7670(7) 0.9300(3) 0.0228(13) Uani 1 1 d . . . . .
H7A H 0.2975 0.7129 0.9667 0.034 Uiso 1 1 calc GR . . . .
H7B H 0.3920 0.8785 0.9345 0.034 Uiso 1 1 calc GR . . . .
H7C H 0.3608 0.7052 0.9041 0.034 Uiso 1 1 calc GR . . . .
C5 C -0.0812(8) 0.8651(8) 0.9301(3) 0.0250(14) Uani 1 1 d . . . . .
H5A H -0.1245 0.9154 0.9610 0.030 Uiso 1 1 calc R . . . .
H5B H -0.0785 0.9309 0.8958 0.030 Uiso 1 1 calc R . . . .
C4 C -0.2883(8) 0.6801(9) 0.8655(3) 0.0264(15) Uani 1 1 d . . . . .
H4A H -0.3497 0.7590 0.8657 0.032 Uiso 1 1 calc R . . . .
H4B H -0.3688 0.5686 0.8622 0.032 Uiso 1 1 calc R . . . .
C6 C 0.0899(8) 0.8709(7) 0.9453(3) 0.0219(13) Uani 1 1 d . . . . .
H6A H 0.1625 0.9862 0.9451 0.026 Uiso 1 1 calc R . . . .
H6B H 0.0912 0.8293 0.9841 0.026 Uiso 1 1 calc R . . . .
C10 C 0.1226(7) 0.3276(7) 0.5361(3) 0.0231(14) Uani 1 1 d . . . . .
H10A H 0.1768 0.3779 0.5011 0.028 Uiso 1 1 calc R . . . .
H10B H 0.0107 0.2561 0.5257 0.028 Uiso 1 1 calc R . . . .
C11 C 0.1104(7) 0.4596(7) 0.5744(3) 0.0216(13) Uani 1 1 d . . . . .
H11A H 0.0320 0.4099 0.6044 0.026 Uiso 1 1 calc R . . . .
H11B H 0.0660 0.5340 0.5527 0.026 Uiso 1 1 calc R . . . .
C15 C 0.1288(8) 0.1273(8) 0.6092(3) 0.0267(14) Uani 1 1 d . . . . .
H15A H 0.0852 0.0103 0.5981 0.032 Uiso 1 1 calc R . . . .
H15B H 0.0349 0.1638 0.6187 0.032 Uiso 1 1 calc R . . . .
C13 C 0.2245(9) 0.4095(9) 0.6924(3) 0.0299(15) Uani 1 1 d . . . . .
H13A H 0.1096 0.3411 0.6845 0.036 Uiso 1 1 calc R . . . .
H13B H 0.2372 0.4297 0.7335 0.036 Uiso 1 1 calc R . . . .
C18 C 0.4543(8) 0.3211(8) 0.7206(3) 0.0256(14) Uani 1 1 d . . . . .
H18A H 0.5228 0.2557 0.7094 0.038 Uiso 1 1 calc GR . . . .
H18B H 0.3954 0.2754 0.7549 0.038 Uiso 1 1 calc GR . . . .
H18C H 0.5236 0.4343 0.7279 0.038 Uiso 1 1 calc GR . . . .
C14 C 0.2391(8) 0.1458(8) 0.6603(3) 0.0308(16) Uani 1 1 d . . . . .
H14A H 0.1713 0.0959 0.6930 0.037 Uiso 1 1 calc R . . . .
H14B H 0.3159 0.0842 0.6538 0.037 Uiso 1 1 calc R . . . .
C9 C -0.3141(8) 0.6460(9) 0.9658(3) 0.0289(15) Uani 1 1 d . . . . .
H9A H -0.3838 0.5322 0.9600 0.043 Uiso 1 1 calc GR . . . .
H9B H -0.3822 0.7173 0.9659 0.043 Uiso 1 1 calc GR . . . .
H9C H -0.2554 0.6562 1.0021 0.043 Uiso 1 1 calc GR . . . .
C20 C -0.2291(8) 1.0564(8) 0.7434(3) 0.0263(14) Uani 1 1 d . . . . .
H20A H -0.2281 1.1463 0.7181 0.039 Uiso 1 1 calc GR . . . .
H20B H -0.1621 0.9951 0.7275 0.039 Uiso 1 1 calc GR . . . .
H20C H -0.1842 1.1010 0.7804 0.039 Uiso 1 1 calc GR . . . .
C19 C -0.3924(9) 0.9504(9) 0.7492(3) 0.0329(16) Uani 1 1 d . . . . .
N7 N -0.5219(9) 0.8613(10) 0.7553(3) 0.063(2) 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
I1 Y1 3.0213(6) . ?
I2 Y1 2.9969(7) . ?
Y2 I4 3.0149(6) . ?
Y2 I3 3.0087(6) . ?
Y2 N5 2.482(5) . ?
Y2 N6 2.605(5) . ?
Y2 N4 2.486(5) . ?
Y2 O2 2.0328(5) . ?
Y1 O1 2.0332(5) . ?
Y1 N2 2.580(5) . ?
Y1 N1 2.473(5) . ?
Y1 N3 2.495(5) . ?
O1 Y1 2.0333(5) 2_567 ?
N2 C8 1.492(7) . ?
N2 C3 1.496(7) . ?
N2 C2 1.496(8) . ?
N1 C1 1.489(7) . ?
N1 C7 1.494(7) . ?
N1 C6 1.483(7) . ?
N3 C5 1.493(8) . ?
N3 C4 1.493(7) . ?
N3 C9 1.485(8) . ?
N5 C17 1.479(7) . ?
N5 C12 1.483(8) . ?
N5 C11 1.498(7) . ?
N6 C13 1.490(8) . ?
N6 C18 1.478(7) . ?
N6 C14 1.483(8) . ?
N4 C16 1.458(7) . ?
N4 C10 1.510(7) . ?
N4 C15 1.477(8) . ?
O2 Y2 2.0328(5) 2_666 ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.498(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.498(9) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.485(9) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.501(9) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.487(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C14 1.506(9) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 C19 1.419(10) . ?
C19 N7 1.145(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I3 Y2 I4 93.842(17) . . ?
N5 Y2 I4 157.12(11) . . ?
N5 Y2 I3 96.38(11) . . ?
N5 Y2 N6 69.45(15) . . ?
N5 Y2 N4 72.04(15) . . ?
N6 Y2 I4 89.08(11) . . ?
N6 Y2 I3 96.70(12) . . ?
N4 Y2 I4 93.39(11) . . ?
N4 Y2 I3 163.89(12) . . ?
N4 Y2 N6 69.03(16) . . ?
O2 Y2 I4 105.21(2) . . ?
O2 Y2 I3 102.87(2) . . ?
O2 Y2 N5 92.40(10) . . ?
O2 Y2 N6 154.73(11) . . ?
O2 Y2 N4 89.07(12) . . ?
I2 Y1 I1 93.991(19) . . ?
O1 Y1 I1 104.69(2) . . ?
O1 Y1 I2 104.12(2) . . ?
O1 Y1 N2 156.16(11) . . ?
O1 Y1 N1 90.72(11) . . ?
O1 Y1 N3 93.79(11) . . ?
N2 Y1 I1 89.71(11) . . ?
N2 Y1 I2 93.49(11) . . ?
N1 Y1 I1 95.67(11) . . ?
N1 Y1 I2 159.62(10) . . ?
N1 Y1 N2 68.69(15) . . ?
N1 Y1 N3 71.34(16) . . ?
N3 Y1 I1 157.70(12) . . ?
N3 Y1 I2 93.47(12) . . ?
N3 Y1 N2 68.87(15) . . ?
Y1 O1 Y1 180.00(3) . 2_567 ?
C8 N2 Y1 109.2(3) . . ?
C8 N2 C3 109.5(4) . . ?
C8 N2 C2 108.7(5) . . ?
C3 N2 Y1 113.2(3) . . ?
C2 N2 Y1 104.5(3) . . ?
C2 N2 C3 111.6(5) . . ?
C1 N1 Y1 116.9(3) . . ?
C1 N1 C7 110.3(5) . . ?
C7 N1 Y1 106.2(3) . . ?
C6 N1 Y1 102.7(3) . . ?
C6 N1 C1 111.1(4) . . ?
C6 N1 C7 109.1(4) . . ?
C5 N3 Y1 111.6(3) . . ?
C4 N3 Y1 107.1(4) . . ?
C4 N3 C5 112.1(5) . . ?
C9 N3 Y1 108.3(4) . . ?
C9 N3 C5 109.8(5) . . ?
C9 N3 C4 107.8(5) . . ?
C17 N5 Y2 108.6(3) . . ?
C17 N5 C12 108.3(5) . . ?
C17 N5 C11 109.7(4) . . ?
C12 N5 Y2 107.5(3) . . ?
C12 N5 C11 111.3(5) . . ?
C11 N5 Y2 111.3(3) . . ?
C13 N6 Y2 111.8(4) . . ?
C18 N6 Y2 110.5(4) . . ?
C18 N6 C13 110.1(5) . . ?
C18 N6 C14 109.8(5) . . ?
C14 N6 Y2 104.1(4) . . ?
C14 N6 C13 110.5(5) . . ?
C16 N4 Y2 106.8(3) . . ?
C16 N4 C10 108.9(4) . . ?
C16 N4 C15 110.9(5) . . ?
C10 N4 Y2 101.3(3) . . ?
C15 N4 Y2 117.0(4) . . ?
C15 N4 C10 111.3(5) . . ?
Y2 O2 Y2 180.0 2_666 . ?
N4 C16 H16A 109.5 . . ?
N4 C16 H16B 109.5 . . ?
N4 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
N1 C1 C2 111.5(5) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C3 H3A 109.2 . . ?
N2 C3 H3B 109.2 . . ?
N2 C3 C4 112.0(5) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
N5 C17 H17A 109.5 . . ?
N5 C17 H17B 109.5 . . ?
N5 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C2 C1 112.0(5) . . ?
N2 C2 H2A 109.2 . . ?
N2 C2 H2B 109.2 . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N5 C12 H12A 108.7 . . ?
N5 C12 H12B 108.7 . . ?
N5 C12 C13 114.1(5) . . ?
H12A C12 H12B 107.6 . . ?
C13 C12 H12A 108.7 . . ?
C13 C12 H12B 108.7 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C5 H5A 109.0 . . ?
N3 C5 H5B 109.0 . . ?
N3 C5 C6 112.8(5) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.0 . . ?
C6 C5 H5B 109.0 . . ?
N3 C4 C3 112.1(5) . . ?
N3 C4 H4A 109.2 . . ?
N3 C4 H4B 109.2 . . ?
C3 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N1 C6 C5 113.4(5) . . ?
N1 C6 H6A 108.9 . . ?
N1 C6 H6B 108.9 . . ?
C5 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
N4 C10 H10A 108.8 . . ?
N4 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C11 C10 N4 113.9(5) . . ?
C11 C10 H10A 108.8 . . ?
C11 C10 H10B 108.8 . . ?
N5 C11 H11A 108.9 . . ?
N5 C11 H11B 108.9 . . ?
C10 C11 N5 113.5(5) . . ?
C10 C11 H11A 108.9 . . ?
C10 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
N4 C15 H15A 109.3 . . ?
N4 C15 H15B 109.3 . . ?
N4 C15 C14 111.8(5) . . ?
H15A C15 H15B 107.9 . . ?
C14 C15 H15A 109.3 . . ?
C14 C15 H15B 109.3 . . ?
N6 C13 H13A 109.0 . . ?
N6 C13 H13B 109.0 . . ?
C12 C13 N6 113.1(5) . . ?
C12 C13 H13A 109.0 . . ?
C12 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
N6 C18 H18A 109.5 . . ?
N6 C18 H18B 109.5 . . ?
N6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N6 C14 C15 114.2(5) . . ?
N6 C14 H14A 108.7 . . ?
N6 C14 H14B 108.7 . . ?
C15 C14 H14A 108.7 . . ?
C15 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
N7 C19 C20 177.4(9) . . ?

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
Y2 N5 C12 C13 -55.9(6) . . . . ?
Y2 N5 C11 C10 -8.9(6) . . . . ?
Y2 N6 C13 C12 -15.2(7) . . . . ?
Y2 N6 C14 C15 -54.3(6) . . . . ?
Y2 N4 C10 C11 -58.7(5) . . . . ?
Y2 N4 C15 C14 -14.0(7) . . . . ?
Y1 N2 C3 C4 -15.7(6) . . . . ?
Y1 N2 C2 C1 -56.6(5) . . . . ?
Y1 N1 C1 C2 -14.5(6) . . . . ?
Y1 N1 C6 C5 -59.2(5) . . . . ?
Y1 N3 C5 C6 -10.0(6) . . . . ?
Y1 N3 C4 C3 -58.4(6) . . . . ?
N2 C3 C4 N3 50.1(7) . . . . ?
N1 C1 C2 N2 49.5(6) . . . . ?
N3 C5 C6 N1 48.8(7) . . . . ?
N5 C12 C13 N6 48.6(8) . . . . ?
N4 C10 C11 N5 48.2(7) . . . . ?
N4 C15 C14 N6 48.5(8) . . . . ?
C16 N4 C10 C11 -171.1(5) . . . . ?
C16 N4 C15 C14 108.8(6) . . . . ?
C1 N1 C6 C5 66.6(6) . . . . ?
C8 N2 C3 C4 106.4(6) . . . . ?
C8 N2 C2 C1 -173.1(5) . . . . ?
C3 N2 C2 C1 66.0(6) . . . . ?
C17 N5 C12 C13 -173.2(5) . . . . ?
C17 N5 C11 C10 111.4(6) . . . . ?
C2 N2 C3 C4 -133.3(6) . . . . ?
C12 N5 C11 C10 -128.7(5) . . . . ?
C7 N1 C1 C2 107.0(6) . . . . ?
C7 N1 C6 C5 -171.7(5) . . . . ?
C5 N3 C4 C3 64.3(7) . . . . ?
C4 N3 C5 C6 -130.2(5) . . . . ?
C6 N1 C1 C2 -131.9(5) . . . . ?
C10 N4 C15 C14 -129.8(6) . . . . ?
C11 N5 C12 C13 66.2(7) . . . . ?
C15 N4 C10 C11 66.4(6) . . . . ?
C13 N6 C14 C15 65.8(7) . . . . ?
C18 N6 C13 C12 108.0(6) . . . . ?
C18 N6 C14 C15 -172.6(6) . . . . ?
C14 N6 C13 C12 -130.7(6) . . . . ?
C9 N3 C5 C6 110.1(6) . . . . ?
C9 N3 C4 C3 -174.8(5) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.177
_oxdiff_exptl_absorpt_empirical_full_min 0.407
####################################################################### 
# 
# 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_2016rnw7945-09ar
_database_code_depnum_ccdc_archive 'CCDC 1590545'
_audit_update_record             
;
2017-12-11 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;
_audit_creation_date             2017-01-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C15 H13 Cl3 Lu N3 O'
_chemical_formula_sum            'C15 H13 Cl3 Lu N3 O'
_chemical_formula_weight         532.60
_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'
Lu Lu -0.4720 5.8584 '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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_symmetry_space_group_name_H-M_alt 'P 1'
_cell_length_a                   7.5588(5)
_cell_length_b                   10.0003(7)
_cell_length_c                   12.0814(9)
_cell_angle_alpha                69.953(7)
_cell_angle_beta                 82.993(6)
_cell_angle_gamma                72.341(6)
_cell_volume                     817.32(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.1020
_cell_measurement_theta_min      2.2800
_cell_oxdiff_angle_alpha         69.953(7)
_cell_oxdiff_angle_beta          82.993(6)
_cell_oxdiff_angle_gamma         72.341(6)
_cell_oxdiff_length_a            7.5588(5)
_cell_oxdiff_length_b            10.0003(7)
_cell_oxdiff_length_c            12.0814(9)
_cell_oxdiff_measurement_reflns_used 9792
_cell_oxdiff_volume              817.32(10)
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.535
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.164
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       chunk
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.019
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1136
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12609
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.259
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00  67.00   1.00   10.00    --  -23.00   0.00 -60.00  180
  2  ω    -87.00  16.00   1.00   10.00    --  -23.00 -72.00 120.00  103
  3  ω    -69.00  16.00   1.00   10.00    --  -23.00 -72.00-120.00   85
  4  ω    -34.00   4.00   1.00   10.00    --  -23.00  72.00   0.00   38
  5  ω    -57.00 -13.00   1.00   10.00    --  -23.00 -72.00  60.00   44
  6  ω    -39.00  67.00   1.00   10.00    --  -23.00  72.00 -60.00  106
  7  ω    -73.00  16.00   1.00   10.00    --  -23.00 -72.00-180.00   89
  8  ω    -75.00  16.00   1.00   10.00    --  -23.00 -72.00   0.00   91
  9  ω    -69.00  26.00   1.00   10.00    --  -23.00   0.00 -30.00   95
 10  ω    -31.00  -7.00   1.00   10.00    --  -23.00  72.00 120.00   24
 11  ω    -39.00 -28.00   1.00   10.00    --  -23.00  72.00 -90.00   11
;
_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 micromount'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0463927000
_diffrn_orient_matrix_UB_12      -0.0603265000
_diffrn_orient_matrix_UB_13      0.0478514000
_diffrn_orient_matrix_UB_21      0.0819128000
_diffrn_orient_matrix_UB_22      0.0234509000
_diffrn_orient_matrix_UB_23      -0.0154714000
_diffrn_orient_matrix_UB_31      -0.0289745000
_diffrn_orient_matrix_UB_32      0.0446954000
_diffrn_orient_matrix_UB_33      0.0371280000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2859
_reflns_number_total             3214
_reflns_odcompleteness_completeness 92.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.31
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.977
_refine_diff_density_min         -2.946
_refine_diff_density_rms         0.294
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3214
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0434
_refine_ls_restrained_S_all      1.026
_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)+(0.0603P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1061
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15)
2.c Fitted hexagon refined as free rotating group:
 N1(C1,C2,C3,C4,C5), N2(C6,C7,C8,C9,C10), N3(C11,C12,C13,C14,C15)
;
_atom_sites_solution_hydrogens   mixed
_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
Lu1 Lu 0.21806(4) 0.82756(3) 0.70843(2) 0.00983(12) Uani 1 1 d . . . . .
Cl1 Cl 0.4413(2) 0.9308(2) 0.77066(16) 0.0163(4) Uani 1 1 d . . . . .
Cl2 Cl -0.0054(2) 0.71093(19) 0.65538(15) 0.0136(4) Uani 1 1 d . . . . .
Cl3 Cl -0.0565(2) 1.0733(2) 0.69540(15) 0.0160(4) Uani 1 1 d . . . . .
O1 O 0.2027(6) 0.9774(5) 0.5138(4) 0.0139(11) Uani 1 1 d . . . . .
H1A H 0.2340 0.9223 0.4660 0.021 Uiso 1 1 d GR . . . .
H1B H 0.2808 1.0333 0.4991 0.021 Uiso 1 1 d GR . . . .
N1 N 0.4826(5) 0.7020(4) 0.6042(3) 0.0141(13) Uani 1 1 d . . . . .
C1 C 0.5556(6) 0.7799(3) 0.4993(4) 0.0147(15) Uani 1 1 d G . . . .
H1 H 0.5100 0.8849 0.4690 0.018 Uiso 1 1 calc R . . . .
C2 C 0.6954(6) 0.7042(4) 0.4387(3) 0.0169(16) Uani 1 1 d G . . . .
H2 H 0.7453 0.7575 0.3669 0.020 Uiso 1 1 calc R . . . .
C3 C 0.7622(6) 0.5507(4) 0.4830(4) 0.0173(16) Uani 1 1 d G . . . .
H3 H 0.8578 0.4989 0.4416 0.021 Uiso 1 1 calc R . . . .
C4 C 0.6892(6) 0.4728(3) 0.5879(4) 0.0163(16) Uani 1 1 d G . . . .
H4 H 0.7348 0.3678 0.6182 0.020 Uiso 1 1 calc R . . . .
C5 C 0.5494(6) 0.5485(4) 0.6486(3) 0.0131(15) Uani 1 1 d G . . . .
N2 N 0.3601(5) 0.5686(3) 0.8190(3) 0.0098(12) Uani 1 1 d . . . . .
C6 C 0.4787(6) 0.4778(4) 0.7598(3) 0.0154(15) Uani 1 1 d G . . . .
C7 C 0.5351(6) 0.3252(4) 0.8145(4) 0.0155(16) Uani 1 1 d G . . . .
H7 H 0.6162 0.2632 0.7741 0.019 Uiso 1 1 calc R . . . .
C8 C 0.4731(6) 0.2632(3) 0.9284(4) 0.0176(16) Uani 1 1 d G . . . .
H8 H 0.5117 0.1588 0.9659 0.021 Uiso 1 1 calc R . . . .
C9 C 0.3545(6) 0.3539(4) 0.9876(3) 0.0178(16) Uani 1 1 d G . . . .
H9 H 0.3121 0.3116 1.0655 0.021 Uiso 1 1 calc R . . . .
C10 C 0.2980(6) 0.5066(4) 0.9329(3) 0.0152(15) Uani 1 1 d G . . . .
N3 N 0.1048(6) 0.7508(4) 0.9155(3) 0.0150(13) Uani 1 1 d . . . . .
C11 C 0.1761(6) 0.6048(4) 0.9862(3) 0.0144(15) Uani 1 1 d G . . . .
C12 C 0.1272(7) 0.5612(4) 1.1052(3) 0.0175(16) Uani 1 1 d G . . . .
H12 H 0.1759 0.4614 1.1535 0.021 Uiso 1 1 calc R . . . .
C13 C 0.0070(7) 0.6637(5) 1.1535(3) 0.0162(16) Uani 1 1 d G . . . .
H13 H -0.0264 0.6340 1.2348 0.019 Uiso 1 1 calc R . . . .
C14 C -0.0642(6) 0.8097(4) 1.0828(4) 0.0185(16) Uani 1 1 d G . . . .
H14 H -0.1464 0.8798 1.1158 0.022 Uiso 1 1 calc R . . . .
C15 C -0.0153(6) 0.8533(4) 0.9638(3) 0.0199(17) Uani 1 1 d G . . . .
H15 H -0.0641 0.9531 0.9155 0.024 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
Lu1 Cl1 2.5256(18) . ?
Lu1 Cl2 2.5681(18) . ?
Lu1 Cl3 2.6634(17) . ?
Lu1 O1 2.309(5) . ?
Lu1 N1 2.471(3) . ?
Lu1 N2 2.436(3) . ?
Lu1 N3 2.478(3) . ?
O1 H1A 0.8935 . ?
O1 H1B 0.8939 . ?
N1 C1 1.3900 . ?
N1 C5 1.3900 . ?
C1 H1 0.9500 . ?
C1 C2 1.3900 . ?
C2 H2 0.9500 . ?
C2 C3 1.3900 . ?
C3 H3 0.9500 . ?
C3 C4 1.3900 . ?
C4 H4 0.9500 . ?
C4 C5 1.3900 . ?
C5 C6 1.412(4) . ?
N2 C6 1.3900 . ?
N2 C10 1.3900 . ?
C6 C7 1.3900 . ?
C7 H7 0.9500 . ?
C7 C8 1.3900 . ?
C8 H8 0.9500 . ?
C8 C9 1.3900 . ?
C9 H9 0.9500 . ?
C9 C10 1.3900 . ?
C10 C11 1.403(4) . ?
N3 C11 1.3900 . ?
N3 C15 1.3900 . ?
C11 C12 1.3900 . ?
C12 H12 0.9500 . ?
C12 C13 1.3900 . ?
C13 H13 0.9500 . ?
C13 C14 1.3900 . ?
C14 H14 0.9500 . ?
C14 C15 1.3900 . ?
C15 H15 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
Cl1 Lu1 Cl2 176.96(5) . . ?
Cl1 Lu1 Cl3 91.01(6) . . ?
Cl2 Lu1 Cl3 90.57(6) . . ?
O1 Lu1 Cl1 96.16(13) . . ?
O1 Lu1 Cl2 86.79(13) . . ?
O1 Lu1 Cl3 72.99(12) . . ?
O1 Lu1 N1 73.61(14) . . ?
O1 Lu1 N2 137.07(15) . . ?
O1 Lu1 N3 154.89(15) . . ?
N1 Lu1 Cl1 87.52(11) . . ?
N1 Lu1 Cl2 92.61(11) . . ?
N1 Lu1 Cl3 146.20(10) . . ?
N1 Lu1 N3 131.29(13) . . ?
N2 Lu1 Cl1 96.26(11) . . ?
N2 Lu1 Cl2 81.04(11) . . ?
N2 Lu1 Cl3 147.41(10) . . ?
N2 Lu1 N1 66.08(13) . . ?
N2 Lu1 N3 66.08(13) . . ?
N3 Lu1 Cl1 89.02(12) . . ?
N3 Lu1 Cl2 88.62(12) . . ?
N3 Lu1 Cl3 82.40(10) . . ?
Lu1 O1 H1A 110.4 . . ?
Lu1 O1 H1B 110.6 . . ?
H1A O1 H1B 108.1 . . ?
C1 N1 Lu1 121.61(19) . . ?
C1 N1 C5 120.0 . . ?
C5 N1 Lu1 118.23(19) . . ?
N1 C1 H1 120.0 . . ?
C2 C1 N1 120.0 . . ?
C2 C1 H1 120.0 . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.0 . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 C6 116.8(3) . . ?
C4 C5 N1 120.0 . . ?
C4 C5 C6 123.0(3) . . ?
C6 N2 Lu1 118.77(19) . . ?
C6 N2 C10 120.0 . . ?
C10 N2 Lu1 120.21(19) . . ?
N2 C6 C5 117.1(3) . . ?
C7 C6 C5 122.6(3) . . ?
C7 C6 N2 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 120.0 . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.0 . . ?
C10 C9 H9 120.0 . . ?
N2 C10 C11 116.8(3) . . ?
C9 C10 N2 120.0 . . ?
C9 C10 C11 123.2(3) . . ?
C11 N3 Lu1 118.59(19) . . ?
C11 N3 C15 120.0 . . ?
C15 N3 Lu1 121.2(2) . . ?
N3 C11 C10 117.5(3) . . ?
C12 C11 C10 122.5(3) . . ?
C12 C11 N3 120.0 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 C11 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 . . ?
C13 C14 C15 120.0 . . ?
C15 C14 H14 120.0 . . ?
N3 C15 H15 120.0 . . ?
C14 C15 N3 120.0 . . ?
C14 C15 H15 120.0 . . ?

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
Lu1 N1 C1 C2 -175.3(3) . . . . ?
Lu1 N1 C5 C4 175.4(3) . . . . ?
Lu1 N1 C5 C6 -9.2(4) . . . . ?
Lu1 N2 C6 C5 16.9(4) . . . . ?
Lu1 N2 C6 C7 -168.4(3) . . . . ?
Lu1 N2 C10 C9 168.3(3) . . . . ?
Lu1 N2 C10 C11 -10.6(4) . . . . ?
Lu1 N3 C11 C10 -4.8(4) . . . . ?
Lu1 N3 C11 C12 174.7(3) . . . . ?
Lu1 N3 C15 C14 -174.5(3) . . . . ?
N1 C1 C2 C3 0.0 . . . . ?
N1 C5 C6 N2 -4.9(5) . . . . ?
N1 C5 C6 C7 -179.4(3) . . . . ?
C1 N1 C5 C4 0.0 . . . . ?
C1 N1 C5 C6 175.4(4) . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 N1 0.0 . . . . ?
C3 C4 C5 C6 -175.1(4) . . . . ?
C4 C5 C6 N2 170.4(3) . . . . ?
C4 C5 C6 C7 -4.1(5) . . . . ?
C5 N1 C1 C2 0.0 . . . . ?
C5 C6 C7 C8 174.3(5) . . . . ?
N2 C6 C7 C8 0.0 . . . . ?
N2 C10 C11 N3 9.9(5) . . . . ?
N2 C10 C11 C12 -169.5(3) . . . . ?
C6 N2 C10 C9 0.0 . . . . ?
C6 N2 C10 C11 -178.9(4) . . . . ?
C6 C7 C8 C9 0.0 . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C8 C9 C10 N2 0.0 . . . . ?
C8 C9 C10 C11 178.8(5) . . . . ?
C9 C10 C11 N3 -168.9(3) . . . . ?
C9 C10 C11 C12 11.6(5) . . . . ?
C10 N2 C6 C5 -174.6(4) . . . . ?
C10 N2 C6 C7 0.0 . . . . ?
C10 C11 C12 C13 179.4(5) . . . . ?
N3 C11 C12 C13 0.0 . . . . ?
C11 N3 C15 C14 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C13 C14 C15 N3 0.0 . . . . ?
C15 N3 C11 C10 -179.4(5) . . . . ?
C15 N3 C11 C12 0.0 . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.061
_oxdiff_exptl_absorpt_empirical_full_min 0.115

_vrf_PLAT420_2016rnw7945-09ar    


;
PROBLEM:    D-H Without Acceptor O1 -- H1B   
RESPONSE: Due to the ambiguity about the exact location of the water hydrogens.
	It is not clear from the difference map 
;
