# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2015

####################################################################### 
# 
# 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_R1
_database_code_depnum_ccdc_archive 'CCDC 1052590'
_audit_update_record             
;
2015-03-06 deposited with the CCDC.
2015-10-28 downloaded from the CCDC.
;
_audit_creation_date             2015-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_chemical_formula_moiety         'C22 H18 B0.5 N2.5'
_chemical_formula_sum            'C22 H18 B0.5 N2.5'
_chemical_formula_weight         322.82
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
B 0.00141 0.00067 2.05450 1.33260 1.09790 0.70680 23.21850 1.02100 60.34980
0.14030 -0.193200007081
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x+1/2,-y+1/2,-z
3 -x,y,-z+1/2
4 -x+1/2,-y+1/2,z+1/2
5 -x,-y,-z
6 -x-1/2,y-1/2,z
7 x,-y,z-1/2
8 x-1/2,y-1/2,-z-1/2

_symmetry_Int_Tables_number      60
_cell_length_a                   20.669(3)
_cell_length_b                   13.906(3)
_cell_length_c                   12.406(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3565.7(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    296.15
_exptl_absorpt_coefficient_mu    0.071
_exptl_crystal_density_diffrn    1.2026
_exptl_crystal_description       RECTANGULAR
_exptl_crystal_colour            PINK
_exptl_crystal_F_000             1360.4853
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_diffrn_reflns_av_R_equivalents  0.1260
_diffrn_reflns_av_unetI/netI     0.0689
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            51040
_diffrn_reflns_theta_full        27.5118
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.77
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9951
_diffrn_measured_fraction_theta_max 0.9951
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              26
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2343
_reflns_number_total             4085
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_refine_diff_density_max         0.4250
_refine_diff_density_min         -0.3775
_refine_diff_density_rms         0.0934
_refine_ls_d_res_high            0.7693
_refine_ls_d_res_low             11.5375
_refine_ls_goodness_of_fit_ref   0.8987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    8
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4085
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0555
_refine_ls_restrained_S_all      0.8987
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1764P)²+0.7597P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.2508
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C22(H22a,H22b,H22c)
;
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C0aa C 0.0 0.4962(2) 0.25 0.0262(7) Uani 1.000000 2 S T P
N2 N 0.0 0.3934(2) 0.25 0.0275(7) Uani 1.000000 2 S T P
N3 N 0.33619(15) 0.0672(2) -0.0546(2) 0.0614(8) Uani 1.000000 1 . . .
N4 N 0.23038(13) 0.3131(2) -0.1802(2) 0.0538(8) Uani 1.000000 1 . . .
C1 C -0.26613(14) 0.9615(2) 0.3079(3) 0.0495(8) Uani 1.000000 1 . . .
C2 C -0.19584(13) 0.93314(19) 0.2981(2) 0.0368(7) Uani 1.000000 1 . . .
C3 C -0.15964(13) 0.95620(19) 0.2068(2) 0.0337(6) Uani 1.000000 1 . . .
C4 C -0.09636(13) 0.92345(18) 0.1941(2) 0.0316(6) Uani 1.000000 1 . . .
C5 C -0.06663(13) 0.86355(18) 0.2721(2) 0.0305(6) Uani 1.000000 1 . . .
C6 C 0.0 0.6992(2) 0.25 0.0283(8) Uani 1.000000 2 S T P
C7 C 0.05760(13) 0.64611(19) 0.2631(2) 0.0315(6) Uani 1.000000 1 . . .
C8 C 0.05780(13) 0.54630(19) 0.2645(2) 0.0306(6) Uani 1.000000 1 . . .
C9 C 0.04991(12) 0.34188(17) 0.1972(2) 0.0267(6) Uani 1.000000 1 . . .
C10 C 0.07589(12) 0.37255(19) 0.0995(2) 0.0295(6) Uani 1.000000 1 . . .
C11 C 0.12499(13) 0.32076(19) 0.0501(2) 0.0320(6) Uani 1.000000 1 . . .
C12 C 0.14999(13) 0.23726(18) 0.0978(2) 0.0313(6) Uani 1.000000 1 . . .
C13 C 0.20367(14) 0.1798(2) 0.0589(2) 0.0369(7) Uani 1.000000 1 . . .
C14 C 0.24133(13) 0.1867(2) -0.0299(2) 0.0372(7) Uani 1.000000 1 . . .
C15 C 0.29424(15) 0.1200(2) -0.0447(2) 0.0461(8) Uani 1.000000 1 . . .
C16 C 0.23418(13) 0.2578(2) -0.1131(2) 0.0394(7) Uani 1.000000 1 . . .
C17 C 0.12262(14) 0.2068(2) 0.1951(2) 0.0357(7) Uani 1.000000 1 . . .
C18 C 0.07370(13) 0.25809(19) 0.2438(2) 0.0328(6) Uani 1.000000 1 . . .
C19 C -0.10300(14) 0.8437(2) 0.3666(2) 0.0372(7) Uani 1.000000 1 . . .
C20 C -0.16575(14) 0.8803(2) 0.3783(2) 0.0409(7) Uani 1.000000 1 . . .
C21 C -0.06083(15) 0.9506(3) 0.0917(3) 0.0422(8) Uani 1.000000 1 . . .
C22 C -0.07519(16) 0.7856(2) 0.4579(2) 0.0532(9) Uani 1.000000 1 . . .
B1 B 0.0 0.8121(3) 0.25 0.0313(9) Uani 1.000000 2 S T P
H3 H -0.1782(11) 0.9961(18) 0.1467(19) 0.024(6) Uiso 1.000000 1 . . .
H20 H -0.1899(13) 0.871(2) 0.444(2) 0.039(8) Uiso 1.000000 1 . . .
H10 H 0.0557(15) 0.430(2) 0.064(3) 0.051(9) Uiso 1.000000 1 . . .
H8 H 0.0956(14) 0.509(2) 0.280(2) 0.041(8) Uiso 1.000000 1 . . .
H7 H 0.0983(14) 0.680(2) 0.275(2) 0.035(7) Uiso 1.000000 1 . . .
H18 H 0.0579(13) 0.237(2) 0.312(2) 0.043(8) Uiso 1.000000 1 . . .
H17 H 0.1392(15) 0.151(2) 0.230(3) 0.049(9) Uiso 1.000000 1 . . .
H11 H 0.1420(13) 0.3445(19) -0.017(2) 0.037(8) Uiso 1.000000 1 . . .
H13 H 0.2194(15) 0.130(2) 0.104(3) 0.050(9) Uiso 1.000000 1 . . .
H21a H -0.0567(15) 0.894(2) 0.045(3) 0.048(9) Uiso 1.000000 1 . . .
H21b H -0.0837(15) 1.000(3) 0.052(3) 0.062(10) Uiso 1.000000 1 . . .
H21c H -0.0176(17) 0.984(3) 0.109(3) 0.069(10) Uiso 1.000000 1 . . .
H1a H -0.2736(3) 1.0196(9) 0.2680(15) 0.0742(13) Uiso 1.000000 1 GR . .
H1b H -0.29288(14) 0.9111(7) 0.2795(16) 0.0742(13) Uiso 1.000000 1 GR . .
H1c H -0.2766(3) 0.9719(15) 0.3824(3) 0.0742(13) Uiso 1.000000 1 GR . .
H22a H -0.0900(9) 0.7204(4) 0.4525(11) 0.0799(14) Uiso 1.000000 1 GR . .
H22b H -0.02881(16) 0.7871(14) 0.4541(11) 0.0799(14) Uiso 1.000000 1 GR . .
H22c H -0.0891(9) 0.8124(10) 0.5254(2) 0.0799(14) Uiso 1.000000 1 GR . .


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
C0aa N2 1.429(4) . ?
C0aa C8 1.395(3) 3 ?
C0aa C8 1.395(3) . ?
N2 C9 1.416(3) . ?
N2 C9 1.416(3) 3 ?
N3 C15 1.143(4) . ?
N4 C16 1.136(4) . ?
C1 C2 1.510(4) . ?
C1 H1a 0.9600 . ?
C1 H1b 0.9600 . ?
C1 H1c 0.9600 . ?
C2 C3 1.394(4) . ?
C2 C20 1.384(4) . ?
C3 C4 1.394(4) . ?
C3 H3 1.01(2) . ?
C4 C5 1.417(4) . ?
C4 C21 1.516(4) . ?
C5 C19 1.420(4) . ?
C5 B1 1.576(3) 3 ?
C6 C7 1.410(3) . ?
C6 C7 1.410(3) 3 ?
C6 B1 1.570(6) . ?
C7 C8 1.388(4) . ?
C7 H7 0.98(3) . ?
C8 H8 0.96(3) . ?
C9 C10 1.392(3) . ?
C9 C18 1.391(4) . ?
C10 C11 1.387(4) . ?
C10 H10 1.00(3) . ?
C11 C12 1.402(4) . ?
C11 H11 0.96(3) . ?
C12 C13 1.450(4) . ?
C12 C17 1.398(4) . ?
C13 C14 1.352(4) . ?
C13 H13 0.95(3) . ?
C14 C15 1.446(4) . ?
C14 C16 1.437(4) . ?
C17 C18 1.377(4) . ?
C17 H17 0.95(3) . ?
C18 H18 0.95(3) . ?
C19 C20 1.401(4) . ?
C19 C22 1.506(4) . ?
C20 H20 0.97(3) . ?
C21 H21a 0.98(3) . ?
C21 H21b 0.97(4) . ?
C21 H21c 1.03(4) . ?
C22 H22a 0.9600 . ?
C22 H22b 0.9600 . ?
C22 H22c 0.9600 . ?

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
C8 C0aa N2 119.98(16) . . ?
C8 C0aa N2 119.98(16) 3 . ?
C8 C0aa C8 120.0(3) 3 . ?
C9 N2 C0aa 120.39(14) . . ?
C9 N2 C0aa 120.39(14) 3 . ?
C9 N2 C9 119.2(3) 3 . ?
H1a C1 C2 109.5 . . ?
H1b C1 C2 109.5 . . ?
H1b C1 H1a 109.5 . . ?
H1c C1 C2 109.5 . . ?
H1c C1 H1a 109.5 . . ?
H1c C1 H1b 109.5 . . ?
C3 C2 C1 121.4(3) . . ?
C20 C2 C1 120.8(3) . . ?
C20 C2 C3 117.7(3) . . ?
C4 C3 C2 121.3(3) . . ?
H3 C3 C2 121.6(13) . . ?
H3 C3 C4 117.0(13) . . ?
C5 C4 C3 121.5(2) . . ?
C21 C4 C3 117.9(2) . . ?
C21 C4 C5 120.6(3) . . ?
C19 C5 C4 116.6(2) . . ?
B1 C5 C4 121.8(2) 3 . ?
B1 C5 C19 121.2(2) 3 . ?
C7 C6 C7 116.9(3) 3 . ?
B1 C6 C7 121.56(16) . . ?
B1 C6 C7 121.56(16) . 3 ?
C8 C7 C6 121.8(3) . . ?
H7 C7 C6 119.5(16) . . ?
H7 C7 C8 118.6(16) . . ?
C7 C8 C0aa 119.7(2) . . ?
H8 C8 C0aa 117.2(18) . . ?
H8 C8 C7 123.0(18) . . ?
C10 C9 N2 121.9(2) . . ?
C18 C9 N2 119.3(2) . . ?
C18 C9 C10 118.8(2) . . ?
C11 C10 C9 120.5(2) . . ?
H10 C10 C9 117.8(18) . . ?
H10 C10 C11 121.5(18) . . ?
C12 C11 C10 120.8(2) . . ?
H11 C11 C10 118.2(16) . . ?
H11 C11 C12 121.0(16) . . ?
C13 C12 C11 126.7(2) . . ?
C17 C12 C11 117.8(2) . . ?
C17 C12 C13 115.5(2) . . ?
C14 C13 C12 132.3(3) . . ?
H13 C13 C12 117.8(19) . . ?
H13 C13 C14 109.7(19) . . ?
C15 C14 C13 119.6(3) . . ?
C16 C14 C13 125.1(3) . . ?
C16 C14 C15 115.3(2) . . ?
C14 C15 N3 178.9(3) . . ?
C14 C16 N4 177.8(3) . . ?
C18 C17 C12 121.3(3) . . ?
H17 C17 C12 119.5(19) . . ?
H17 C17 C18 119.1(19) . . ?
C17 C18 C9 120.7(3) . . ?
H18 C18 C9 120.7(18) . . ?
H18 C18 C17 118.6(18) . . ?
C20 C19 C5 120.4(3) . . ?
C22 C19 C5 121.6(3) . . ?
C22 C19 C20 118.1(3) . . ?
C19 C20 C2 122.3(3) . . ?
H20 C20 C2 116.4(17) . . ?
H20 C20 C19 121.3(17) . . ?
H21a C21 C4 109.4(18) . . ?
H21b C21 C4 111.6(19) . . ?
H21b C21 H21a 108(3) . . ?
H21c C21 C4 111.0(19) . . ?
H21c C21 H21a 114(3) . . ?
H21c C21 H21b 102(3) . . ?
H22a C22 C19 109.5 . . ?
H22b C22 C19 109.5 . . ?
H22b C22 H22a 109.5 . . ?
H22c C22 C19 109.5 . . ?
H22c C22 H22a 109.5 . . ?
H22c C22 H22b 109.5 . . ?
C5 B1 C5 126.0(3) . 3 ?
C6 B1 C5 117.01(16) . 3 ?
C6 B1 C5 117.01(16) . . ?

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

data_dcv1_0m
_database_code_depnum_ccdc_archive 'CCDC 1417197'
_audit_update_record             
;
2015-08-06 deposited with the CCDC.
2015-10-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H34 B N3'
_chemical_formula_weight         507.46

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'p -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2822(18)
_cell_length_b                   11.668(3)
_cell_length_c                   16.026(4)
_cell_angle_alpha                97.984(6)
_cell_angle_beta                 94.609(6)
_cell_angle_gamma                101.200(6)
_cell_volume                     1495.2(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       cube
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             540
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  bruker
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32454
_diffrn_reflns_av_R_equivalents  0.1456
_diffrn_reflns_av_sigmaI/netI    0.2598
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         30.50
_reflns_number_total             9059
_reflns_number_gt                4011
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0926P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9059
_refine_ls_number_parameters     428
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.3028
_refine_ls_R_factor_gt           0.0992
_refine_ls_wR_factor_ref         0.2293
_refine_ls_wR_factor_gt          0.1718
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_restrained_S_all      0.964
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.013

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.8474(3) -0.12187(19) 0.14490(13) 0.0403(6) Uani 1 1 d . . .
N2 N 0.7861(5) -0.7200(3) -0.0195(3) 0.150(2) Uani 1 1 d . . .
N3 N 0.3357(4) -0.8983(3) 0.05437(18) 0.0731(9) Uani 1 1 d . . .
C34 C 0.8429(5) 0.2501(3) 0.7387(2) 0.0830(12) Uani 1 1 d . . .
H34A H 0.7499 0.2228 0.7681 0.125 Uiso 1 1 calc R . .
H34B H 0.8955 0.3294 0.7640 0.125 Uiso 1 1 calc R . .
H34C H 0.9205 0.1992 0.7424 0.125 Uiso 1 1 calc R . .
C30 C 0.7843(5) 0.2482(3) 0.64694(19) 0.0556(9) Uani 1 1 d . . .
C31 C 0.8935(5) 0.2832(3) 0.5903(2) 0.0566(9) Uani 1 1 d . . .
C32 C 0.8426(4) 0.2797(2) 0.50509(18) 0.0474(8) Uani 1 1 d . . .
C27 C 0.6742(3) 0.2409(2) 0.47374(16) 0.0382(7) Uani 1 1 d . . .
C15 C 0.6931(3) 0.1380(2) 0.31487(17) 0.0359(7) Uani 1 1 d . . .
C16 C 0.7619(3) 0.0486(2) 0.34298(19) 0.0403(7) Uani 1 1 d . . .
C17 C 0.8115(4) -0.0361(3) 0.28805(18) 0.0432(7) Uani 1 1 d . . .
C12 C 0.7973(3) -0.0329(2) 0.20221(17) 0.0354(7) Uani 1 1 d . . .
C8 C 0.7681(3) -0.2379(2) 0.13467(16) 0.0354(7) Uani 1 1 d . . .
C7 C 0.8293(4) -0.3267(3) 0.08688(18) 0.0426(8) Uani 1 1 d . . .
C6 C 0.7506(4) -0.4422(3) 0.07600(19) 0.0445(8) Uani 1 1 d . . .
C5 C 0.6039(3) -0.4794(2) 0.11156(17) 0.0423(7) Uani 1 1 d . . .
C4 C 0.5128(4) -0.5979(3) 0.10141(19) 0.0462(8) Uani 1 1 d . . .
C3 C 0.5386(3) -0.6998(2) 0.05969(18) 0.0419(7) Uani 1 1 d . . .
C2 C 0.6752(5) -0.7105(3) 0.0152(3) 0.0722(11) Uani 1 1 d . . .
C14 C 0.6851(4) 0.1401(3) 0.22808(19) 0.0436(8) Uani 1 1 d . . .
C13 C 0.7371(4) 0.0573(3) 0.1722(2) 0.0439(8) Uani 1 1 d . . .
C18 C 0.4703(3) 0.2768(2) 0.33859(16) 0.0362(7) Uani 1 1 d . . .
C19 C 0.3274(3) 0.2017(2) 0.29174(17) 0.0423(7) Uani 1 1 d . . .
C20 C 0.2009(4) 0.2499(3) 0.2595(2) 0.0493(8) Uani 1 1 d . . .
C21 C 0.2058(4) 0.3694(3) 0.27100(19) 0.0494(8) Uani 1 1 d . . .
C25 C 0.0645(4) 0.4175(3) 0.2335(3) 0.0846(12) Uani 1 1 d . . .
H33 H -0.0195 0.3532 0.2034 0.127 Uiso 1 1 calc R . .
H34 H 0.1047 0.4699 0.1951 0.127 Uiso 1 1 calc R . .
H32 H 0.0184 0.4600 0.2781 0.127 Uiso 1 1 calc R . .
C22 C 0.3432(4) 0.4417(3) 0.3175(2) 0.0489(8) Uani 1 1 d . . .
C23 C 0.4748(3) 0.3987(2) 0.35098(17) 0.0414(7) Uani 1 1 d . . .
C26 C 0.6243(6) 0.4852(3) 0.3988(3) 0.0693(12) Uani 1 1 d . . .
C24 C 0.3028(4) 0.0682(2) 0.2784(2) 0.0573(9) Uani 1 1 d . . .
H24A H 0.3989 0.0461 0.3036 0.086 Uiso 1 1 calc R . .
H24B H 0.2863 0.0384 0.2188 0.086 Uiso 1 1 calc R . .
H24C H 0.2074 0.0355 0.3043 0.086 Uiso 1 1 calc R . .
C35 C 0.9721(4) 0.3224(3) 0.4480(2) 0.0724(11) Uani 1 1 d . . .
H35A H 0.9201 0.3150 0.3912 0.109 Uiso 1 1 calc R . .
H35B H 1.0551 0.2753 0.4483 0.109 Uiso 1 1 calc R . .
H35C H 1.0228 0.4038 0.4684 0.109 Uiso 1 1 calc R . .
C29 C 0.6185(5) 0.2116(3) 0.6160(2) 0.0535(9) Uani 1 1 d . . .
C28 C 0.5616(4) 0.2085(2) 0.53237(18) 0.0451(8) Uani 1 1 d . . .
C33 C 0.3778(4) 0.1666(5) 0.5062(3) 0.0682(11) Uani 1 1 d . . .
C11 C 0.9798(3) -0.0831(2) 0.09401(17) 0.0466(8) Uani 1 1 d . . .
H11A H 1.0208 0.0006 0.1097 0.070 Uiso 1 1 calc R . .
H11B H 0.9377 -0.1006 0.0351 0.070 Uiso 1 1 calc R . .
H11C H 1.0681 -0.1238 0.1038 0.070 Uiso 1 1 calc R . .
C9 C 0.6210(4) -0.2737(3) 0.1706(2) 0.0518(9) Uani 1 1 d . . .
C10 C 0.5444(4) -0.3894(3) 0.1584(2) 0.0535(9) Uani 1 1 d . . .
C1 C 0.4243(4) -0.8096(3) 0.05706(18) 0.0491(8) Uani 1 1 d . . .
B1 B 0.6146(4) 0.2226(3) 0.3762(2) 0.0376(8) Uani 1 1 d . . .
H5 H 0.931(3) -0.305(2) 0.0656(14) 0.030(7) Uiso 1 1 d . . .
H2 H 0.437(3) -0.410(2) 0.1784(16) 0.048(8) Uiso 1 1 d . . .
H3 H 0.800(3) -0.502(2) 0.0468(16) 0.045(8) Uiso 1 1 d . . .
H1 H 0.420(3) -0.602(2) 0.1279(17) 0.055(9) Uiso 1 1 d . . .
H4 H 0.579(3) -0.210(2) 0.1982(17) 0.058(9) Uiso 1 1 d . . .
H10 H 0.855(3) -0.105(2) 0.3087(16) 0.050(8) Uiso 1 1 d . . .
H11 H 0.640(3) 0.202(2) 0.2128(16) 0.048(8) Uiso 1 1 d . . .
H9 H 0.739(3) 0.063(2) 0.1147(17) 0.044(8) Uiso 1 1 d . . .
H12 H 0.771(3) 0.044(2) 0.4011(18) 0.050(8) Uiso 1 1 d . . .
H15 H 0.344(3) 0.522(2) 0.3273(16) 0.044(8) Uiso 1 1 d . . .
H14 H 0.545(4) 0.186(3) 0.6543(19) 0.065(10) Uiso 1 1 d . . .
H16 H 0.110(3) 0.206(2) 0.2273(16) 0.037(8) Uiso 1 1 d . . .
H13 H 1.009(4) 0.317(2) 0.6101(17) 0.059(9) Uiso 1 1 d . . .
H27 H 0.611(5) 0.563(4) 0.407(2) 0.110(14) Uiso 1 1 d . . .
H25 H 0.320(4) 0.171(3) 0.558(2) 0.101(13) Uiso 1 1 d . . .
H23 H 0.331(5) 0.212(4) 0.472(3) 0.107(16) Uiso 1 1 d . . .
H28 H 0.707(5) 0.481(3) 0.365(3) 0.102(17) Uiso 1 1 d . . .
H24 H 0.355(5) 0.078(4) 0.473(3) 0.123(16) Uiso 1 1 d . . .
H26 H 0.652(5) 0.467(4) 0.460(3) 0.127(17) Uiso 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C8 1.367(3) . ?
N1 C12 1.435(3) . ?
N1 C11 1.458(3) . ?
N2 C2 1.126(4) . ?
N3 C1 1.139(3) . ?
C34 C30 1.506(4) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C30 C31 1.378(4) . ?
C30 C29 1.385(4) . ?
C31 C32 1.390(4) . ?
C31 H13 0.97(3) . ?
C32 C27 1.408(4) . ?
C32 C35 1.521(4) . ?
C27 C28 1.413(4) . ?
C27 B1 1.573(4) . ?
C15 C16 1.392(4) . ?
C15 C14 1.391(4) . ?
C15 B1 1.564(4) . ?
C16 C17 1.376(4) . ?
C16 H12 0.94(3) . ?
C17 C12 1.378(4) . ?
C17 H10 1.02(3) . ?
C12 C13 1.375(4) . ?
C8 C9 1.404(4) . ?
C8 C7 1.401(4) . ?
C7 C6 1.359(4) . ?
C7 H5 0.93(2) . ?
C6 C5 1.402(4) . ?
C6 H3 0.96(3) . ?
C5 C10 1.396(4) . ?
C5 C4 1.422(4) . ?
C4 C3 1.343(4) . ?
C4 H1 0.91(3) . ?
C3 C2 1.402(5) . ?
C3 C1 1.431(4) . ?
C14 C13 1.380(4) . ?
C14 H11 0.93(3) . ?
C13 H9 0.94(3) . ?
C18 C23 1.401(3) . ?
C18 C19 1.416(4) . ?
C18 B1 1.573(4) . ?
C19 C20 1.380(4) . ?
C19 C24 1.513(4) . ?
C20 C21 1.373(4) . ?
C20 H16 0.90(2) . ?
C21 C22 1.370(4) . ?
C21 C25 1.511(4) . ?
C25 H33 0.9600 . ?
C25 H34 0.9600 . ?
C25 H32 0.9600 . ?
C22 C23 1.386(4) . ?
C22 H15 0.93(3) . ?
C23 C26 1.513(4) . ?
C26 H27 0.93(4) . ?
C26 H28 0.91(4) . ?
C26 H26 1.06(4) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C29 C28 1.377(4) . ?
C29 H14 0.94(3) . ?
C28 C33 1.511(4) . ?
C33 H25 0.99(4) . ?
C33 H23 0.93(4) . ?
C33 H24 1.07(4) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C9 C10 1.355(4) . ?
C9 H4 0.95(3) . ?
C10 H2 0.96(3) . ?

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
C8 N1 C12 121.4(2) . . ?
C8 N1 C11 121.0(2) . . ?
C12 N1 C11 117.6(2) . . ?
C30 C34 H34A 109.5 . . ?
C30 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C30 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C31 C30 C29 117.2(3) . . ?
C31 C30 C34 121.4(3) . . ?
C29 C30 C34 121.4(3) . . ?
C30 C31 C32 122.3(3) . . ?
C30 C31 H13 120.2(17) . . ?
C32 C31 H13 117.4(17) . . ?
C31 C32 C27 120.2(3) . . ?
C31 C32 C35 118.4(3) . . ?
C27 C32 C35 121.4(3) . . ?
C32 C27 C28 117.4(3) . . ?
C32 C27 B1 121.6(3) . . ?
C28 C27 B1 120.7(2) . . ?
C16 C15 C14 115.8(3) . . ?
C16 C15 B1 121.5(2) . . ?
C14 C15 B1 122.4(3) . . ?
C17 C16 C15 122.2(3) . . ?
C17 C16 H12 119.1(17) . . ?
C15 C16 H12 118.7(17) . . ?
C16 C17 C12 120.1(3) . . ?
C16 C17 H10 121.8(14) . . ?
C12 C17 H10 118.0(14) . . ?
C13 C12 C17 119.5(3) . . ?
C13 C12 N1 120.4(2) . . ?
C17 C12 N1 120.1(2) . . ?
N1 C8 C9 121.8(2) . . ?
N1 C8 C7 121.3(2) . . ?
C9 C8 C7 116.9(3) . . ?
C6 C7 C8 121.7(3) . . ?
C6 C7 H5 120.2(14) . . ?
C8 C7 H5 118.0(14) . . ?
C7 C6 C5 122.1(3) . . ?
C7 C6 H3 119.8(15) . . ?
C5 C6 H3 118.0(15) . . ?
C10 C5 C6 115.3(3) . . ?
C10 C5 C4 119.4(3) . . ?
C6 C5 C4 125.3(3) . . ?
C3 C4 C5 132.2(3) . . ?
C3 C4 H1 116.9(18) . . ?
C5 C4 H1 110.9(18) . . ?
C4 C3 C2 124.9(3) . . ?
C4 C3 C1 121.6(3) . . ?
C2 C3 C1 113.5(3) . . ?
N2 C2 C3 178.8(5) . . ?
C13 C14 C15 122.7(3) . . ?
C13 C14 H11 124.9(16) . . ?
C15 C14 H11 112.4(16) . . ?
C12 C13 C14 119.6(3) . . ?
C12 C13 H9 118.4(16) . . ?
C14 C13 H9 121.9(16) . . ?
C23 C18 C19 117.4(3) . . ?
C23 C18 B1 122.5(2) . . ?
C19 C18 B1 120.1(2) . . ?
C20 C19 C18 119.8(3) . . ?
C20 C19 C24 117.6(3) . . ?
C18 C19 C24 122.6(3) . . ?
C21 C20 C19 122.9(3) . . ?
C21 C20 H16 114.1(16) . . ?
C19 C20 H16 123.0(16) . . ?
C22 C21 C20 117.2(3) . . ?
C22 C21 C25 122.2(3) . . ?
C20 C21 C25 120.7(3) . . ?
C21 C25 H33 109.5 . . ?
C21 C25 H34 109.5 . . ?
H33 C25 H34 109.5 . . ?
C21 C25 H32 109.5 . . ?
H33 C25 H32 109.5 . . ?
H34 C25 H32 109.5 . . ?
C21 C22 C23 122.7(3) . . ?
C21 C22 H15 117.2(16) . . ?
C23 C22 H15 120.2(16) . . ?
C22 C23 C18 120.1(3) . . ?
C22 C23 C26 119.1(3) . . ?
C18 C23 C26 120.8(3) . . ?
C23 C26 H27 113(2) . . ?
C23 C26 H28 105(3) . . ?
H27 C26 H28 107(3) . . ?
C23 C26 H26 112(2) . . ?
H27 C26 H26 105(3) . . ?
H28 C26 H26 114(4) . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C28 C29 C30 122.7(3) . . ?
C28 C29 H14 120.2(19) . . ?
C30 C29 H14 117.1(18) . . ?
C29 C28 C27 120.1(3) . . ?
C29 C28 C33 117.8(3) . . ?
C27 C28 C33 122.1(3) . . ?
C28 C33 H25 108(2) . . ?
C28 C33 H23 115(2) . . ?
H25 C33 H23 105(3) . . ?
C28 C33 H24 109(2) . . ?
H25 C33 H24 111(3) . . ?
H23 C33 H24 108(3) . . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C9 C8 120.3(3) . . ?
C10 C9 H4 125.6(17) . . ?
C8 C9 H4 113.9(17) . . ?
C9 C10 C5 123.8(3) . . ?
C9 C10 H2 118.2(16) . . ?
C5 C10 H2 117.8(16) . . ?
N3 C1 C3 178.6(4) . . ?
C15 B1 C27 118.1(2) . . ?
C15 B1 C18 118.5(2) . . ?
C27 B1 C18 123.2(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
C29 C30 C31 C32 -1.6(4) . . . . ?
C34 C30 C31 C32 178.6(3) . . . . ?
C30 C31 C32 C27 0.8(4) . . . . ?
C30 C31 C32 C35 178.9(3) . . . . ?
C31 C32 C27 C28 1.2(4) . . . . ?
C35 C32 C27 C28 -176.9(3) . . . . ?
C31 C32 C27 B1 -173.3(3) . . . . ?
C35 C32 C27 B1 8.7(4) . . . . ?
C14 C15 C16 C17 -3.0(4) . . . . ?
B1 C15 C16 C17 171.2(3) . . . . ?
C15 C16 C17 C12 1.4(4) . . . . ?
C16 C17 C12 C13 1.6(4) . . . . ?
C16 C17 C12 N1 -179.4(2) . . . . ?
C8 N1 C12 C13 -116.5(3) . . . . ?
C11 N1 C12 C13 59.8(3) . . . . ?
C8 N1 C12 C17 64.5(3) . . . . ?
C11 N1 C12 C17 -119.2(3) . . . . ?
C12 N1 C8 C9 8.6(4) . . . . ?
C11 N1 C8 C9 -167.6(3) . . . . ?
C12 N1 C8 C7 -172.1(2) . . . . ?
C11 N1 C8 C7 11.7(4) . . . . ?
N1 C8 C7 C6 -179.6(3) . . . . ?
C9 C8 C7 C6 -0.3(4) . . . . ?
C8 C7 C6 C5 0.2(5) . . . . ?
C7 C6 C5 C10 0.3(4) . . . . ?
C7 C6 C5 C4 178.5(3) . . . . ?
C10 C5 C4 C3 179.0(3) . . . . ?
C6 C5 C4 C3 0.8(5) . . . . ?
C5 C4 C3 C2 1.6(5) . . . . ?
C5 C4 C3 C1 -178.3(3) . . . . ?
C4 C3 C2 N2 105(21) . . . . ?
C1 C3 C2 N2 -75(21) . . . . ?
C16 C15 C14 C13 1.8(4) . . . . ?
B1 C15 C14 C13 -172.4(3) . . . . ?
C17 C12 C13 C14 -2.8(4) . . . . ?
N1 C12 C13 C14 178.2(2) . . . . ?
C15 C14 C13 C12 1.1(4) . . . . ?
C23 C18 C19 C20 0.9(4) . . . . ?
B1 C18 C19 C20 179.5(3) . . . . ?
C23 C18 C19 C24 -176.3(3) . . . . ?
B1 C18 C19 C24 2.4(4) . . . . ?
C18 C19 C20 C21 -0.4(4) . . . . ?
C24 C19 C20 C21 176.9(3) . . . . ?
C19 C20 C21 C22 -0.5(5) . . . . ?
C19 C20 C21 C25 179.4(3) . . . . ?
C20 C21 C22 C23 1.0(4) . . . . ?
C25 C21 C22 C23 -178.9(3) . . . . ?
C21 C22 C23 C18 -0.5(4) . . . . ?
C21 C22 C23 C26 177.8(3) . . . . ?
C19 C18 C23 C22 -0.4(4) . . . . ?
B1 C18 C23 C22 -179.0(2) . . . . ?
C19 C18 C23 C26 -178.8(3) . . . . ?
B1 C18 C23 C26 2.6(4) . . . . ?
C31 C30 C29 C28 0.5(4) . . . . ?
C34 C30 C29 C28 -179.7(3) . . . . ?
C30 C29 C28 C27 1.4(4) . . . . ?
C30 C29 C28 C33 179.9(3) . . . . ?
C32 C27 C28 C29 -2.2(4) . . . . ?
B1 C27 C28 C29 172.3(3) . . . . ?
C32 C27 C28 C33 179.4(3) . . . . ?
B1 C27 C28 C33 -6.1(4) . . . . ?
N1 C8 C9 C10 179.3(3) . . . . ?
C7 C8 C9 C10 -0.1(4) . . . . ?
C8 C9 C10 C5 0.6(5) . . . . ?
C6 C5 C10 C9 -0.7(5) . . . . ?
C4 C5 C10 C9 -179.0(3) . . . . ?
C4 C3 C1 N3 -166(14) . . . . ?
C2 C3 C1 N3 14(14) . . . . ?
C16 C15 B1 C27 24.2(4) . . . . ?
C14 C15 B1 C27 -161.9(2) . . . . ?
C16 C15 B1 C18 -151.0(2) . . . . ?
C14 C15 B1 C18 22.9(4) . . . . ?
C32 C27 B1 C15 55.6(3) . . . . ?
C28 C27 B1 C15 -118.6(3) . . . . ?
C32 C27 B1 C18 -129.5(3) . . . . ?
C28 C27 B1 C18 56.3(3) . . . . ?
C23 C18 B1 C15 -126.7(3) . . . . ?
C19 C18 B1 C15 54.8(3) . . . . ?
C23 C18 B1 C27 58.4(4) . . . . ?
C19 C18 B1 C27 -120.1(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C11 H11C N2 0.96 2.65 3.436(5) 139.0 2_745
C11 H11B N3 0.96 2.58 3.342(4) 136.7 2_645

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        30.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.046
