# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_mx4_a
_database_code_depnum_ccdc_archive 'CCDC 1905674'
_audit_update_record             
;
2019-03-26 deposited with the CCDC.	2020-08-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H21 N O'
_chemical_formula_weight         291.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.162(15)
_cell_length_b                   19.10(3)
_cell_length_c                   8.941(13)
_cell_angle_alpha                90
_cell_angle_beta                 109.780(18)
_cell_angle_gamma                90
_cell_volume                     1633(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5114
_cell_measurement_theta_min      4.26
_cell_measurement_theta_max      29.34

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_F_000             624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.072
_shelx_estimated_absorpt_T_min   0.994
_shelx_estimated_absorpt_T_max   0.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6455
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS-2012/1 (Bruker,2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa APEX-Duo CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11359
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.265
_diffrn_reflns_theta_max         29.342
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             4432
_reflns_number_gt                3691
_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 APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0731P)²+0.2852P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4432
_refine_ls_number_parameters     283
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0484
_refine_ls_wR_factor_ref         0.1373
_refine_ls_wR_factor_gt          0.1261
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_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
N1 N 0.74973(9) 0.47534(5) 0.67381(11) 0.0353(2) Uani 1 1 d . . . . .
H1 H 0.4152(18) 0.4458(9) 0.8743(19) 0.059(4) Uiso 1 1 d . . . . .
O1 O 0.81444(13) 0.65660(6) 1.06696(11) 0.0665(3) Uani 1 1 d . . . . .
C1 C 0.57465(11) 0.53719(6) 0.74246(13) 0.0366(2) Uani 1 1 d . . . . .
C2 C 0.57309(11) 0.46015(6) 0.78042(12) 0.0351(2) Uani 1 1 d . . . . .
H2 H 0.4442(19) 0.3195(10) 0.899(2) 0.073(5) Uiso 1 1 d . . . . .
C3 C 0.48628(13) 0.42154(7) 0.84126(14) 0.0437(3) Uani 1 1 d . . . . .
H3 H 0.622(2) 0.2635(11) 0.824(2) 0.077(5) Uiso 1 1 d . . . . .
C6 C 0.69617(15) 0.35389(6) 0.75031(17) 0.0496(3) Uani 1 1 d . . . . .
H6 H 0.733(2) 0.4174(10) 0.125(2) 0.071(5) Uiso 1 1 d . . . . .
C5 C 0.60739(18) 0.31563(7) 0.81192(19) 0.0597(4) Uani 1 1 d . . . . .
H5 H 0.7520(17) 0.4837(9) 0.3585(18) 0.056(4) Uiso 1 1 d . . . . .
C4 C 0.50412(16) 0.34836(8) 0.85663(17) 0.0557(3) Uani 1 1 d . . . . .
H4 H 0.7667(17) 0.3302(9) 0.7177(18) 0.054(4) Uiso 1 1 d . . . . .
C7 C 0.67748(11) 0.42667(5) 0.73485(12) 0.0356(2) Uani 1 1 d . . . . .
H7 H 0.845(2) 0.3050(10) 0.150(2) 0.075(5) Uiso 1 1 d . . . . .
C8 C 0.72064(10) 0.54732(5) 0.72201(11) 0.0317(2) Uani 1 1 d . . . . .
H8 H 0.9798(19) 0.2643(11) 0.404(2) 0.075(5) Uiso 1 1 d . . . . .
C9 C 0.71534(14) 0.60222(6) 0.59503(13) 0.0408(2) Uani 1 1 d . . . . .
H9 H 1.0025(18) 0.3335(9) 0.635(2) 0.064(5) Uiso 1 1 d . . . . .
C10 C 0.67887(17) 0.67498(7) 0.64387(16) 0.0507(3) Uani 1 1 d . . . . .
H10 H 0.9367(16) 0.5030(8) 0.6618(17) 0.048(4) Uiso 1 1 d . . . . .
C11 C 0.78334(18) 0.69853(7) 0.80413(17) 0.0535(3) Uani 1 1 d . . . . .
H11 H 0.9449(16) 0.4311(8) 0.7594(18) 0.051(4) Uiso 1 1 d . . . . .
C12 C 0.80937(12) 0.64302(6) 0.93187(14) 0.0427(3) Uani 1 1 d . . . . .
H12 H 0.9252(18) 0.5693(9) 0.8716(18) 0.056(4) Uiso 1 1 d . . . . .
C13 C 0.83184(12) 0.56878(6) 0.88293(13) 0.0390(2) Uani 1 1 d . . . . .
H13 H 0.8320(15) 0.5360(8) 0.9671(18) 0.051(4) Uiso 1 1 d . . . . .
C14 C 0.88774(11) 0.45765(6) 0.66405(14) 0.0398(2) Uani 1 1 d . . . . .
H14 H 0.879(2) 0.7065(10) 0.788(2) 0.074(5) Uiso 1 1 d . . . . .
C15 C 0.87717(10) 0.41444(6) 0.51693(13) 0.0357(2) Uani 1 1 d . . . . .
H15 H 0.7537(18) 0.7412(10) 0.843(2) 0.069(5) Uiso 1 1 d . . . . .
C16 C 0.94567(14) 0.35005(7) 0.52969(15) 0.0454(3) Uani 1 1 d . . . . .
H16 H 0.8090(16) 0.6035(8) 0.5787(17) 0.051(4) Uiso 1 1 d . . . . .
C17 C 0.93381(16) 0.31012(7) 0.39441(17) 0.0544(3) Uani 1 1 d . . . . .
H17 H 0.6444(17) 0.5868(8) 0.4912(19) 0.055(4) Uiso 1 1 d . . . . .
C18 C 0.85383(15) 0.33450(8) 0.24526(17) 0.0554(3) Uani 1 1 d . . . . .
H18 H 0.4974(15) 0.5480(7) 0.6376(17) 0.043(3) Uiso 1 1 d . . . . .
C19 C 0.78748(14) 0.39935(8) 0.23045(16) 0.0536(3) Uani 1 1 d . . . . .
H19 H 0.5630(15) 0.5672(8) 0.8254(17) 0.051(4) Uiso 1 1 d . . . . .
C20 C 0.79909(13) 0.43907(7) 0.36595(15) 0.0450(3) Uani 1 1 d . . . . .
H21 H 0.6760(18) 0.7096(9) 0.562(2) 0.066(5) Uiso 1 1 d . . . . .
H20 H 0.5810(17) 0.6737(8) 0.6505(18) 0.053(4) 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
N1 C7 1.4044(18) . ?
N1 C14 1.474(2) . ?
N1 C8 1.500(2) . ?
O1 C12 1.219(2) . ?
C1 C2 1.511(3) . ?
C1 C8 1.567(3) . ?
C1 H18 1.020(14) . ?
C1 H19 0.976(15) . ?
C2 C3 1.3938(19) . ?
C2 C7 1.412(2) . ?
C3 C4 1.410(3) . ?
C3 H1 0.984(17) . ?
C6 C7 1.403(3) . ?
C6 C5 1.410(2) . ?
C6 H4 0.972(17) . ?
C5 C4 1.391(3) . ?
C5 H3 1.01(2) . ?
C4 H2 0.985(19) . ?
C8 C9 1.533(2) . ?
C8 C13 1.554(2) . ?
C9 C10 1.539(2) . ?
C9 H16 1.011(15) . ?
C9 H17 1.007(16) . ?
C10 C11 1.534(3) . ?
C10 H21 0.982(19) . ?
C10 H20 1.016(16) . ?
C11 C12 1.515(2) . ?
C11 H14 1.042(19) . ?
C11 H15 0.970(19) . ?
C12 C13 1.524(2) . ?
C13 H12 0.988(17) . ?
C13 H13 0.978(16) . ?
C14 C15 1.526(2) . ?
C14 H10 1.002(16) . ?
C14 H11 0.992(16) . ?
C15 C20 1.396(2) . ?
C15 C16 1.399(2) . ?
C16 C17 1.400(2) . ?
C16 H9 0.973(18) . ?
C17 C18 1.386(3) . ?
C17 H8 0.98(2) . ?
C18 C19 1.395(3) . ?
C18 H7 1.00(2) . ?
C19 C20 1.400(2) . ?
C19 H6 0.978(18) . ?
C20 H5 0.969(17) . ?

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
C7 N1 C14 120.30(12) . . ?
C7 N1 C8 108.38(12) . . ?
C14 N1 C8 120.75(8) . . ?
C2 C1 C8 103.22(8) . . ?
C2 C1 H18 109.9(8) . . ?
C8 C1 H18 109.4(8) . . ?
C2 C1 H19 112.9(9) . . ?
C8 C1 H19 112.3(9) . . ?
H18 C1 H19 109.0(12) . . ?
C3 C2 C7 120.64(14) . . ?
C3 C2 C1 131.22(11) . . ?
C7 C2 C1 108.07(10) . . ?
C2 C3 C4 119.01(13) . . ?
C2 C3 H1 119.6(10) . . ?
C4 C3 H1 121.4(10) . . ?
C7 C6 C5 117.95(14) . . ?
C7 C6 H4 121.4(10) . . ?
C5 C6 H4 120.6(10) . . ?
C4 C5 C6 121.60(15) . . ?
C4 C5 H3 120.7(11) . . ?
C6 C5 H3 117.7(11) . . ?
C5 C4 C3 120.13(12) . . ?
C5 C4 H2 118.8(11) . . ?
C3 C4 H2 121.1(11) . . ?
C6 C7 N1 128.52(12) . . ?
C6 C7 C2 120.67(11) . . ?
N1 C7 C2 110.80(13) . . ?
N1 C8 C9 112.03(12) . . ?
N1 C8 C13 110.83(9) . . ?
C9 C8 C13 109.73(12) . . ?
N1 C8 C1 101.94(9) . . ?
C9 C8 C1 111.93(9) . . ?
C13 C8 C1 110.19(12) . . ?
C8 C9 C10 111.04(13) . . ?
C8 C9 H16 108.9(9) . . ?
C10 C9 H16 110.3(9) . . ?
C8 C9 H17 108.5(9) . . ?
C10 C9 H17 111.1(9) . . ?
H16 C9 H17 106.8(12) . . ?
C11 C10 C9 111.89(12) . . ?
C11 C10 H21 109.7(10) . . ?
C9 C10 H21 110.2(10) . . ?
C11 C10 H20 109.5(9) . . ?
C9 C10 H20 109.2(9) . . ?
H21 C10 H20 106.2(13) . . ?
C12 C11 C10 112.84(13) . . ?
C12 C11 H14 106.0(11) . . ?
C10 C11 H14 107.1(10) . . ?
C12 C11 H15 108.4(10) . . ?
C10 C11 H15 112.2(11) . . ?
H14 C11 H15 110.1(15) . . ?
O1 C12 C11 122.42(14) . . ?
O1 C12 C13 121.48(12) . . ?
C11 C12 C13 116.09(14) . . ?
C12 C13 C8 112.26(10) . . ?
C12 C13 H12 105.2(10) . . ?
C8 C13 H12 109.3(9) . . ?
C12 C13 H13 109.6(9) . . ?
C8 C13 H13 110.8(9) . . ?
H12 C13 H13 109.5(13) . . ?
N1 C14 C15 112.60(9) . . ?
N1 C14 H10 107.0(9) . . ?
C15 C14 H10 109.9(8) . . ?
N1 C14 H11 111.0(9) . . ?
C15 C14 H11 108.3(9) . . ?
H10 C14 H11 107.9(12) . . ?
C20 C15 C16 118.66(11) . . ?
C20 C15 C14 120.17(14) . . ?
C16 C15 C14 121.16(11) . . ?
C15 C16 C17 120.90(13) . . ?
C15 C16 H9 118.7(10) . . ?
C17 C16 H9 120.4(10) . . ?
C18 C17 C16 119.93(15) . . ?
C18 C17 H8 119.2(11) . . ?
C16 C17 H8 120.8(11) . . ?
C17 C18 C19 119.78(13) . . ?
C17 C18 H7 119.0(11) . . ?
C19 C18 H7 121.2(11) . . ?
C18 C19 C20 120.17(14) . . ?
C18 C19 H6 120.2(11) . . ?
C20 C19 H6 119.6(11) . . ?
C15 C20 C19 120.53(15) . . ?
C15 C20 H5 118.0(9) . . ?
C19 C20 H5 121.5(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
C8 C1 C2 C3 165.64(11) . . . . ?
C8 C1 C2 C7 -17.57(11) . . . . ?
C7 C2 C3 C4 -0.04(17) . . . . ?
C1 C2 C3 C4 176.41(12) . . . . ?
C7 C6 C5 C4 -0.1(2) . . . . ?
C6 C5 C4 C3 -0.2(2) . . . . ?
C2 C3 C4 C5 0.2(2) . . . . ?
C5 C6 C7 N1 -178.35(12) . . . . ?
C5 C6 C7 C2 0.22(19) . . . . ?
C14 N1 C7 C6 -19.91(17) . . . . ?
C8 N1 C7 C6 -164.80(12) . . . . ?
C14 N1 C7 C2 161.41(9) . . . . ?
C8 N1 C7 C2 16.52(12) . . . . ?
C3 C2 C7 C6 -0.17(16) . . . . ?
C1 C2 C7 C6 -177.37(11) . . . . ?
C3 C2 C7 N1 178.63(10) . . . . ?
C1 C2 C7 N1 1.43(12) . . . . ?
C7 N1 C8 C9 -146.12(10) . . . . ?
C14 N1 C8 C9 69.18(13) . . . . ?
C7 N1 C8 C13 90.95(15) . . . . ?
C14 N1 C8 C13 -53.75(14) . . . . ?
C7 N1 C8 C1 -26.30(11) . . . . ?
C14 N1 C8 C1 -171.00(9) . . . . ?
C2 C1 C8 N1 25.85(11) . . . . ?
C2 C1 C8 C9 145.75(9) . . . . ?
C2 C1 C8 C13 -91.86(11) . . . . ?
N1 C8 C9 C10 177.46(10) . . . . ?
C13 C8 C9 C10 -58.99(15) . . . . ?
C1 C8 C9 C10 63.67(13) . . . . ?
C8 C9 C10 C11 57.53(17) . . . . ?
C9 C10 C11 C12 -49.07(17) . . . . ?
C10 C11 C12 O1 -136.41(15) . . . . ?
C10 C11 C12 C13 44.71(18) . . . . ?
O1 C12 C13 C8 134.10(14) . . . . ?
C11 C12 C13 C8 -47.01(16) . . . . ?
N1 C8 C13 C12 177.37(9) . . . . ?
C9 C8 C13 C12 53.12(14) . . . . ?
C1 C8 C13 C12 -70.56(13) . . . . ?
C7 N1 C14 C15 82.03(15) . . . . ?
C8 N1 C14 C15 -137.40(10) . . . . ?
N1 C14 C15 C20 55.32(15) . . . . ?
N1 C14 C15 C16 -125.19(12) . . . . ?
C20 C15 C16 C17 -1.50(19) . . . . ?
C14 C15 C16 C17 179.01(12) . . . . ?
C15 C16 C17 C18 0.3(2) . . . . ?
C16 C17 C18 C19 1.1(2) . . . . ?
C17 C18 C19 C20 -1.4(2) . . . . ?
C16 C15 C20 C19 1.26(18) . . . . ?
C14 C15 C20 C19 -179.23(11) . . . . ?
C18 C19 C20 C15 0.1(2) . . . . ?

_refine_diff_density_max         0.280
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.040



####################################################################### 
# 
# 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_x_a
_database_code_depnum_ccdc_archive 'CCDC 1905675'
_audit_update_record             
;
2019-03-26 deposited with the CCDC.	2020-08-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H27 N O'
_chemical_formula_weight         381.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_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, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   13.7872(5)
_cell_length_b                   16.2182(8)
_cell_length_c                   9.4765(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.759(3)
_cell_angle_gamma                90
_cell_volume                     2104.25(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4041
_cell_measurement_theta_min      4.23
_cell_measurement_theta_max      66.45

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.555
_shelx_estimated_absorpt_T_min   0.936
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5648
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS-2012/1 (Bruker,2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa APEX-Duo CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5476
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         4.226
_diffrn_reflns_theta_max         66.443
_diffrn_reflns_theta_full        66.443
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.755
_diffrn_reflns_point_group_measured_fraction_full 0.755
_reflns_number_total             2802
_reflns_number_gt                2726
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.518
_reflns_Friedel_fraction_max     0.516
_reflns_Friedel_fraction_full    0.516

_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 APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0759P)²+0.1062P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 896 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         2802
_refine_ls_number_parameters     262
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.1063
_refine_ls_wR_factor_gt          0.1050
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.048
_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
O1 O 0.47554(15) 0.55110(15) 0.9686(2) 0.0759(6) Uani 1 1 d . . . . .
N1 N 0.28995(13) 0.66144(11) 0.5541(2) 0.0493(4) Uani 1 1 d . . . . .
C1 C 0.37511(18) 0.73648(15) 0.7438(3) 0.0579(6) Uani 1 1 d . . . . .
H1A H 0.398802 0.726785 0.842839 0.069 Uiso 1 1 calc R U . . .
H1AB H 0.412956 0.780550 0.707819 0.069 Uiso 1 1 calc R U . . .
C2 C 0.26862(17) 0.75699(14) 0.7261(3) 0.0549(5) Uani 1 1 d . . . . .
C3 C 0.2153(2) 0.81210(18) 0.7978(3) 0.0698(7) Uani 1 1 d . . . . .
H3 H 0.245675 0.842724 0.873416 0.084 Uiso 1 1 calc R U . . .
C4 C 0.1169(2) 0.8211(2) 0.7561(4) 0.0778(9) Uani 1 1 d . . . . .
H4 H 0.080768 0.857920 0.803996 0.093 Uiso 1 1 calc R U . . .
C5 C 0.0712(2) 0.7758(2) 0.6437(4) 0.0755(8) Uani 1 1 d . . . . .
H5 H 0.004699 0.782825 0.616139 0.091 Uiso 1 1 calc R U . . .
C6 C 0.12435(17) 0.71957(18) 0.5709(3) 0.0630(6) Uani 1 1 d . . . . .
H6 H 0.093777 0.688686 0.495799 0.076 Uiso 1 1 calc R U . . .
C7 C 0.22250(16) 0.71107(14) 0.6131(2) 0.0511(5) Uani 1 1 d . . . . .
C8 C 0.38098(15) 0.65695(13) 0.6549(2) 0.0477(5) Uani 1 1 d . . . . .
C9 C 0.25565(17) 0.58946(15) 0.4701(3) 0.0555(5) Uani 1 1 d . . . . .
H9A H 0.202313 0.564266 0.512781 0.067 Uiso 1 1 calc R U . . .
H9AB H 0.308210 0.549484 0.473679 0.067 Uiso 1 1 calc R U . . .
C10 C 0.22116(16) 0.60920(14) 0.3161(3) 0.0522(5) Uani 1 1 d . . . . .
C11 C 0.1334(2) 0.5808(2) 0.2507(3) 0.0686(7) Uani 1 1 d . . . . .
H11 H 0.092837 0.550431 0.302824 0.082 Uiso 1 1 calc R U . . .
C12 C 0.1042(2) 0.5966(2) 0.1091(4) 0.0772(8) Uani 1 1 d . . . . .
H12 H 0.044999 0.576021 0.066269 0.093 Uiso 1 1 calc R U . . .
C13 C 0.1622(2) 0.6426(2) 0.0311(3) 0.0725(7) Uani 1 1 d . . . . .
H13 H 0.141992 0.654618 -0.063831 0.087 Uiso 1 1 calc R U . . .
C14 C 0.2498(2) 0.6705(2) 0.0947(3) 0.0778(8) Uani 1 1 d . . . . .
H14 H 0.290238 0.700628 0.041991 0.093 Uiso 1 1 calc R U . . .
C15 C 0.27932(19) 0.65458(19) 0.2363(3) 0.0662(6) Uani 1 1 d . . . . .
H15 H 0.339026 0.674677 0.278252 0.079 Uiso 1 1 calc R U . . .
C16 C 0.38040(16) 0.57937(15) 0.7493(3) 0.0543(5) Uani 1 1 d . . . . .
H16A H 0.327539 0.584006 0.807908 0.065 Uiso 1 1 calc R U . . .
H16B H 0.367650 0.531408 0.688775 0.065 Uiso 1 1 calc R U . . .
C17 C 0.47451(17) 0.56645(13) 0.8437(3) 0.0545(5) Uani 1 1 d . . . . .
C18 C 0.56746(16) 0.57150(15) 0.7705(3) 0.0539(5) Uani 1 1 d . . . . .
H18 H 0.567283 0.524204 0.706115 0.065 Uiso 1 1 calc R U . . .
C19 C 0.56518(16) 0.64984(16) 0.6795(3) 0.0559(5) Uani 1 1 d . . . . .
H19A H 0.570050 0.697774 0.741137 0.067 Uiso 1 1 calc R U . . .
H19B H 0.621122 0.650010 0.626267 0.067 Uiso 1 1 calc R U . . .
C20 C 0.47149(16) 0.65563(15) 0.5761(2) 0.0527(5) Uani 1 1 d . . . . .
H20A H 0.473142 0.705390 0.519657 0.063 Uiso 1 1 calc R U . . .
H20B H 0.467786 0.608811 0.511985 0.063 Uiso 1 1 calc R U . . .
C21 C 0.65850(19) 0.56450(17) 0.8781(3) 0.0617(6) Uani 1 1 d . . . . .
H21A H 0.656323 0.607221 0.949328 0.074 Uiso 1 1 calc R U . . .
H21B H 0.657452 0.511660 0.925902 0.074 Uiso 1 1 calc R U . . .
C22 C 0.75305(16) 0.57207(15) 0.8140(3) 0.0550(5) Uani 1 1 d . . . . .
C23 C 0.77732(19) 0.51632(17) 0.7126(4) 0.0690(7) Uani 1 1 d . . . . .
H23 H 0.734447 0.473632 0.683910 0.083 Uiso 1 1 calc R U . . .
C24 C 0.8634(2) 0.5230(2) 0.6540(4) 0.0818(9) Uani 1 1 d . . . . .
H24 H 0.877594 0.485860 0.584545 0.098 Uiso 1 1 calc R U . . .
C25 C 0.9288(2) 0.5846(2) 0.6978(4) 0.0790(8) Uani 1 1 d . . . . .
H25 H 0.987871 0.588637 0.660004 0.095 Uiso 1 1 calc R U . . .
C26 C 0.9055(2) 0.64027(19) 0.7984(4) 0.0766(8) Uani 1 1 d . . . . .
H26 H 0.948970 0.682382 0.828082 0.092 Uiso 1 1 calc R U . . .
C27 C 0.8193(2) 0.63407(17) 0.8546(3) 0.0663(6) Uani 1 1 d . . . . .
H27 H 0.804738 0.672443 0.921865 0.080 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
O1 C17 1.208(3) . ?
N1 C7 1.396(3) . ?
N1 C9 1.460(3) . ?
N1 C8 1.487(3) . ?
C1 C2 1.496(4) . ?
C1 C8 1.548(3) . ?
C1 H1A 0.9700 . ?
C1 H1AB 0.9700 . ?
C2 C3 1.385(4) . ?
C2 C7 1.395(4) . ?
C3 C4 1.375(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.401(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.372(3) . ?
C6 H6 0.9300 . ?
C8 C20 1.528(3) . ?
C8 C16 1.544(3) . ?
C9 C10 1.515(3) . ?
C9 H9A 0.9700 . ?
C9 H9AB 0.9700 . ?
C10 C11 1.372(4) . ?
C10 C15 1.378(4) . ?
C11 C12 1.379(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.371(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.362(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.380(4) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.502(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.530(3) . ?
C18 C21 1.525(3) . ?
C18 C19 1.534(3) . ?
C18 H18 0.9800 . ?
C19 C20 1.530(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.507(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C27 1.383(4) . ?
C22 C23 1.388(4) . ?
C23 C24 1.373(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.377(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.377(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.362(5) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?

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
C7 N1 C9 119.41(18) . . ?
C7 N1 C8 108.82(19) . . ?
C9 N1 C8 120.38(17) . . ?
C2 C1 C8 103.78(19) . . ?
C2 C1 H1A 111.0 . . ?
C8 C1 H1A 111.0 . . ?
C2 C1 H1AB 111.0 . . ?
C8 C1 H1AB 111.0 . . ?
H1A C1 H1AB 109.0 . . ?
C3 C2 C7 120.1(2) . . ?
C3 C2 C1 131.3(3) . . ?
C7 C2 C1 108.6(2) . . ?
C4 C3 C2 119.3(3) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C6 120.5(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 118.5(3) . . ?
C7 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
C6 C7 C2 121.0(2) . . ?
C6 C7 N1 128.5(2) . . ?
C2 C7 N1 110.53(19) . . ?
N1 C8 C20 111.26(18) . . ?
N1 C8 C16 110.52(17) . . ?
C20 C8 C16 109.38(17) . . ?
N1 C8 C1 102.39(17) . . ?
C20 C8 C1 112.06(18) . . ?
C16 C8 C1 111.09(19) . . ?
N1 C9 C10 113.62(19) . . ?
N1 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N1 C9 H9AB 108.8 . . ?
C10 C9 H9AB 108.8 . . ?
H9A C9 H9AB 107.7 . . ?
C11 C10 C15 118.0(2) . . ?
C11 C10 C9 121.6(2) . . ?
C15 C10 C9 120.3(2) . . ?
C10 C11 C12 121.2(3) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C13 C12 C11 120.3(3) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C14 C13 C12 119.0(3) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 120.9(3) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C10 C15 C14 120.6(2) . . ?
C10 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 C8 113.32(17) . . ?
C17 C16 H16A 108.9 . . ?
C8 C16 H16A 108.9 . . ?
C17 C16 H16B 108.9 . . ?
C8 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
O1 C17 C16 121.5(2) . . ?
O1 C17 C18 122.8(2) . . ?
C16 C17 C18 115.7(2) . . ?
C21 C18 C17 111.1(2) . . ?
C21 C18 C19 113.48(19) . . ?
C17 C18 C19 109.66(18) . . ?
C21 C18 H18 107.4 . . ?
C17 C18 H18 107.4 . . ?
C19 C18 H18 107.4 . . ?
C20 C19 C18 111.77(18) . . ?
C20 C19 H19A 109.3 . . ?
C18 C19 H19A 109.3 . . ?
C20 C19 H19B 109.3 . . ?
C18 C19 H19B 109.3 . . ?
H19A C19 H19B 107.9 . . ?
C8 C20 C19 111.38(19) . . ?
C8 C20 H20A 109.4 . . ?
C19 C20 H20A 109.4 . . ?
C8 C20 H20B 109.4 . . ?
C19 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C22 C21 C18 114.0(2) . . ?
C22 C21 H21A 108.8 . . ?
C18 C21 H21A 108.8 . . ?
C22 C21 H21B 108.7 . . ?
C18 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C27 C22 C23 117.4(2) . . ?
C27 C22 C21 121.5(2) . . ?
C23 C22 C21 121.1(2) . . ?
C24 C23 C22 121.2(2) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C23 C24 C25 120.1(3) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C26 119.1(3) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
C27 C26 C25 120.5(3) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C26 C27 C22 121.6(3) . . ?
C26 C27 H27 119.2 . . ?
C22 C27 H27 119.2 . . ?

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
C8 C1 C2 C3 167.4(2) . . . . ?
C8 C1 C2 C7 -14.6(2) . . . . ?
C7 C2 C3 C4 -0.2(4) . . . . ?
C1 C2 C3 C4 177.7(2) . . . . ?
C2 C3 C4 C5 -0.1(4) . . . . ?
C3 C4 C5 C6 0.5(4) . . . . ?
C4 C5 C6 C7 -0.6(4) . . . . ?
C5 C6 C7 C2 0.3(4) . . . . ?
C5 C6 C7 N1 -177.7(2) . . . . ?
C3 C2 C7 C6 0.1(3) . . . . ?
C1 C2 C7 C6 -178.2(2) . . . . ?
C3 C2 C7 N1 178.4(2) . . . . ?
C1 C2 C7 N1 0.1(2) . . . . ?
C9 N1 C7 C6 -22.7(3) . . . . ?
C8 N1 C7 C6 -166.4(2) . . . . ?
C9 N1 C7 C2 159.14(19) . . . . ?
C8 N1 C7 C2 15.5(2) . . . . ?
C7 N1 C8 C20 -143.38(18) . . . . ?
C9 N1 C8 C20 73.4(2) . . . . ?
C7 N1 C8 C16 94.9(2) . . . . ?
C9 N1 C8 C16 -48.3(3) . . . . ?
C7 N1 C8 C1 -23.5(2) . . . . ?
C9 N1 C8 C1 -166.75(19) . . . . ?
C2 C1 C8 N1 22.4(2) . . . . ?
C2 C1 C8 C20 141.72(19) . . . . ?
C2 C1 C8 C16 -95.6(2) . . . . ?
C7 N1 C9 C10 84.2(3) . . . . ?
C8 N1 C9 C10 -136.4(2) . . . . ?
N1 C9 C10 C11 -131.4(3) . . . . ?
N1 C9 C10 C15 50.6(3) . . . . ?
C15 C10 C11 C12 0.5(5) . . . . ?
C9 C10 C11 C12 -177.6(3) . . . . ?
C10 C11 C12 C13 -1.2(6) . . . . ?
C11 C12 C13 C14 1.7(6) . . . . ?
C12 C13 C14 C15 -1.5(6) . . . . ?
C11 C10 C15 C14 -0.3(5) . . . . ?
C9 C10 C15 C14 177.9(3) . . . . ?
C13 C14 C15 C10 0.8(6) . . . . ?
N1 C8 C16 C17 174.26(19) . . . . ?
C20 C8 C16 C17 51.4(3) . . . . ?
C1 C8 C16 C17 -72.8(3) . . . . ?
C8 C16 C17 O1 132.4(3) . . . . ?
C8 C16 C17 C18 -49.3(3) . . . . ?
O1 C17 C18 C21 -6.4(3) . . . . ?
C16 C17 C18 C21 175.4(2) . . . . ?
O1 C17 C18 C19 -132.7(3) . . . . ?
C16 C17 C18 C19 49.1(3) . . . . ?
C21 C18 C19 C20 -178.4(2) . . . . ?
C17 C18 C19 C20 -53.5(3) . . . . ?
N1 C8 C20 C19 -179.24(18) . . . . ?
C16 C8 C20 C19 -56.9(2) . . . . ?
C1 C8 C20 C19 66.8(2) . . . . ?
C18 C19 C20 C8 59.8(3) . . . . ?
C17 C18 C21 C22 -177.9(2) . . . . ?
C19 C18 C21 C22 -53.8(3) . . . . ?
C18 C21 C22 C27 119.6(3) . . . . ?
C18 C21 C22 C23 -61.1(3) . . . . ?
C27 C22 C23 C24 -0.6(5) . . . . ?
C21 C22 C23 C24 -180.0(3) . . . . ?
C22 C23 C24 C25 1.6(6) . . . . ?
C23 C24 C25 C26 -1.5(6) . . . . ?
C24 C25 C26 C27 0.5(6) . . . . ?
C25 C26 C27 C22 0.4(5) . . . . ?
C23 C22 C27 C26 -0.4(4) . . . . ?
C21 C22 C27 C26 179.0(3) . . . . ?

_refine_diff_density_max         0.208
_refine_diff_density_min         -0.144
_refine_diff_density_rms         0.039



