# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_I
_database_code_depnum_ccdc_archive 'CCDC 1558717'
_audit_update_record             
;
2017-06-27 deposited with the CCDC.	2021-01-14 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   9.7305(3)
_cell_length_b                   10.3706(4)
_cell_length_c                   13.6626(5)
_cell_angle_alpha                78.159(3)
_cell_angle_beta                 80.220(3)
_cell_angle_gamma                79.813(3)
_cell_volume                     1315.27(8)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

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_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050
1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            1

# Given Formula = C30 H30 N3 O9 Ti3 
# Dc =      1.82 Fooo =    738.00 Mu =      9.57 M =    720.28
# Found Formula = C19 H45 N2 O8.50 Ti2 
# Dc =      1.35 FOOO =    570.00 Mu =      6.51 M =    533.37

_chemical_formula_sum            'C38 H90 N4 O17 Ti4'
_chemical_formula_moiety         '2(C18 H42 N2 O8 Ti2), C2 H6 O'
_chemical_compound_source        ?
_chemical_formula_weight         1066.62


_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    8324
_cell_measurement_theta_min      4.0340
_cell_measurement_theta_max      29.0180

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.190
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_max          0.558

_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             570
_exptl_absorpt_coefficient_mu    0.651

# Sheldrick geometric approximatio 0.81 0.88 
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_detector_area_resol_mean 10.4678
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_reflns_number            27521
_reflns_number_total             6645
_diffrn_reflns_av_R_equivalents  0.034
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6645 
# Theoretical number of reflections is about 15111 


_diffrn_reflns_theta_min         3.164
_diffrn_reflns_theta_max         29.828
_diffrn_measured_fraction_theta_max 0.879

_diffrn_reflns_theta_full        26.620
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              -13
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_oxford_diffrn_Wilson_B_factor   2.11
_oxford_diffrn_Wilson_scale      0.07

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.69
_refine_diff_density_max         1.96


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         6645
_refine_ls_number_restraints     10
_refine_ls_number_parameters     293
_oxford_refine_ls_R_factor_ref   0.0781
_refine_ls_wR_factor_ref         0.1635
_refine_ls_goodness_of_fit_ref   1.0280
_refine_ls_shift/su_max          0.0004664
_refine_ls_shift/su_mean         0.0000208


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6645
_refine_ls_R_factor_all          0.0781
_refine_ls_wR_factor_all         0.1635

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5197
_refine_ls_R_factor_gt           0.0586
_refine_ls_wR_factor_gt          0.1397

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.06P)² + 3.40P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ti1 Ti 0.23143(5) 0.72760(5) 0.27271(4) 0.0249 1.0000 Uani . . . . . .
O2 O 0.0239(2) 0.7299(2) 0.33537(16) 0.0281 1.0000 Uani . . . . . .
Ti3 Ti -0.10129(5) 0.78059(5) 0.22572(4) 0.0279 1.0000 Uani . . . . . .
O4 O 0.1058(2) 0.7516(2) 0.16156(15) 0.0253 1.0000 Uani . . . . . .
C5 C 0.1557(3) 0.8286(3) 0.0676(2) 0.0339 1.0000 Uani . . . . . .
C6 C 0.1751(4) 0.9627(3) 0.0875(3) 0.0368 1.0000 Uani . . . . . .
N7 N 0.2402(3) 0.9475(3) 0.1811(2) 0.0327 1.0000 Uani . . . . . .
C8 C 0.3939(4) 0.9483(4) 0.1600(3) 0.0406 1.0000 Uani . . . . . .
C9 C 0.4632(3) 0.8225(4) 0.1220(3) 0.0421 1.0000 Uani . . . . . .
O10 O 0.3998(2) 0.7142(2) 0.17961(18) 0.0351 1.0000 Uani . . . . . .
H92 H 0.5611 0.8084 0.1257 0.0501 1.0000 Uiso . . . . . .
H91 H 0.4518 0.8308 0.0518 0.0496 1.0000 Uiso . . . . . .
H81 H 0.4274 0.9532 0.2222 0.0489 1.0000 Uiso . . . . . .
H82 H 0.4138 1.0247 0.1095 0.0489 1.0000 Uiso . . . . . .
C11 C 0.1735(4) 1.0564(4) 0.2369(3) 0.0457 1.0000 Uani . . . . . .
H112 H 0.2192 1.0503 0.2942 0.0681 1.0000 Uiso . . . . . .
H111 H 0.1811 1.1398 0.1934 0.0675 1.0000 Uiso . . . . . .
H113 H 0.0778 1.0446 0.2585 0.0666 1.0000 Uiso . . . . . .
H62 H 0.2339 1.0049 0.0314 0.0439 1.0000 Uiso . . . . . .
H61 H 0.0829 1.0157 0.0957 0.0439 1.0000 Uiso . . . . . .
H52 H 0.2460 0.7849 0.0390 0.0406 1.0000 Uiso . . . . . .
H51 H 0.0892 0.8420 0.0204 0.0412 1.0000 Uiso . . . . . .
O12 O -0.2617(2) 0.7477(2) 0.3170(2) 0.0375 1.0000 Uani . . . . . .
C13 C -0.3192(4) 0.6285(4) 0.3424(3) 0.0410 1.0000 Uani . . . . . .
C14 C -0.2043(4) 0.5151(4) 0.3221(3) 0.0422 1.0000 Uani . . . . . .
N15 N -0.1138(3) 0.5564(3) 0.2261(2) 0.0288 1.0000 Uani . . . . . .
C16 C -0.1846(4) 0.5599(4) 0.1374(3) 0.0412 1.0000 Uani . . . . . .
C17 C -0.1363(4) 0.6710(4) 0.0553(3) 0.0453 1.0000 Uani . . . . . .
O18 O -0.1542(3) 0.7855(2) 0.09876(19) 0.0388 1.0000 Uani . . . . . .
H171 H -0.0352 0.6474 0.0303 0.0536 1.0000 Uiso . . . . . .
H172 H -0.1909 0.6861 0.0009 0.0541 1.0000 Uiso . . . . . .
H162 H -0.2871 0.5778 0.1567 0.0504 1.0000 Uiso . . . . . .
H161 H -0.1578 0.4735 0.1150 0.0498 1.0000 Uiso . . . . . .
C19 C 0.0211(4) 0.4658(4) 0.2222(4) 0.0534 1.0000 Uani . . . . . .
H193 H 0.0867 0.4974 0.1617 0.0792 1.0000 Uiso . . . . . .
H192 H 0.0630 0.4635 0.2808 0.0786 1.0000 Uiso . . . . . .
H191 H 0.0062 0.3759 0.2221 0.0782 1.0000 Uiso . . . . . .
H142 H -0.1458 0.4911 0.3761 0.0511 1.0000 Uiso . . . . . .
H141 H -0.2463 0.4369 0.3180 0.0508 1.0000 Uiso . . . . . .
H131 H -0.3546 0.6122 0.4149 0.0493 1.0000 Uiso . . . . . .
H132 H -0.3951 0.6335 0.3041 0.0494 1.0000 Uiso . . . . . .
O20 O -0.1400(2) 0.9594(2) 0.2188(2) 0.0420 1.0000 Uani . . . . . .
C21 C -0.2657(4) 1.0515(4) 0.2163(3) 0.0444 1.0000 Uani . . . . . .
C22 C -0.2366(5) 1.1855(4) 0.2229(4) 0.0573 1.0000 Uani . . . . . .
H222 H -0.3241 1.2443 0.2231 0.0877 1.0000 Uiso . . . . . .
H221 H -0.1968 1.1769 0.2858 0.0875 1.0000 Uiso . . . . . .
H223 H -0.1711 1.2155 0.1659 0.0878 1.0000 Uiso . . . . . .
H212 H -0.3298 1.0228 0.2760 0.0540 1.0000 Uiso . . . . . .
H211 H -0.3077 1.0585 0.1547 0.0542 1.0000 Uiso . . . . . .
C23 C -0.0188(4) 0.7132(4) 0.4419(3) 0.0385 1.0000 Uani . . . . . .
C24 C -0.0634(5) 0.8460(5) 0.4754(4) 0.0607 1.0000 Uani . . . . . .
H243 H -0.0865 0.8299 0.5478 0.0916 1.0000 Uiso . . . . . .
H242 H -0.1452 0.8903 0.4468 0.0916 1.0000 Uiso . . . . . .
H241 H 0.0097 0.8975 0.4543 0.0918 1.0000 Uiso . . . . . .
H232 H 0.0595 0.6652 0.4750 0.0470 1.0000 Uiso . . . . . .
H231 H -0.0970 0.6637 0.4605 0.0467 1.0000 Uiso . . . . . .
O25 O 0.2747(3) 0.8022(2) 0.37082(17) 0.0355 1.0000 Uani . . . . . .
C26 C 0.3232(4) 0.7699(4) 0.4655(3) 0.0461 1.0000 Uani . . . . . .
C27 C 0.4197(4) 0.8661(5) 0.4726(3) 0.0548 1.0000 Uani . . . . . .
H271 H 0.4477 0.8454 0.5390 0.0820 1.0000 Uiso . . . . . .
H273 H 0.3718 0.9546 0.4603 0.0817 1.0000 Uiso . . . . . .
H272 H 0.5011 0.8543 0.4234 0.0813 1.0000 Uiso . . . . . .
H261 H 0.2443 0.7783 0.5182 0.0559 1.0000 Uiso . . . . . .
H262 H 0.3719 0.6788 0.4767 0.0560 1.0000 Uiso . . . . . .
O28 O 0.2722(2) 0.5513(2) 0.32372(18) 0.0336 1.0000 Uani . . . . . .
C29 C 0.3900(4) 0.4503(3) 0.3226(3) 0.0376 1.0000 Uani . . . . . .
C30 C 0.3488(4) 0.3200(4) 0.3131(4) 0.0578 1.0000 Uani . . . . . .
H302 H 0.4320 0.2530 0.3144 0.0877 1.0000 Uiso . . . . . .
H301 H 0.2777 0.2937 0.3700 0.0882 1.0000 Uiso . . . . . .
H303 H 0.3115 0.3307 0.2503 0.0881 1.0000 Uiso . . . . . .
H292 H 0.4259 0.4359 0.3873 0.0448 1.0000 Uiso . . . . . .
H291 H 0.4607 0.4755 0.2674 0.0447 1.0000 Uiso . . . . . .
O31 O 0.3388(6) 0.5246(7) 0.0615(6) 0.0648 0.5000 Uani D U . . . .
C32 C 0.4601(6) 0.4479(5) 0.0330(4) 0.0924 1.0000 Uani D U . . . .
H325 H 0.3738 0.4811 0.0618 0.1123 0.5000 Uiso . . . . . .
H324 H 0.5155 0.4031 0.0921 0.1129 0.5000 Uiso . . . . . .
H323 H 0.5195 0.4041 0.0861 0.1123 0.5000 Uiso . . . . . .
H322 H 0.4444 0.3811 -0.0038 0.1128 0.5000 Uiso . . . . . .
H321 H 0.4564 0.3810 -0.0048 0.1123 0.5000 Uiso . . . . . .
H312 H 0.377(12) 0.560(12) 0.095(8) 0.097(2) 0.5000 Uiso D . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          4.60(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ti1 . O2 . 2.053(2) yes
Ti1 . O4 . 2.057(2) yes
Ti1 . N7 . 2.374(3) yes
Ti1 . O10 . 1.899(2) yes
Ti1 . O25 . 1.818(2) yes
Ti1 . O28 . 1.817(2) yes
O2 . Ti3 . 2.018(2) yes
O2 . C23 . 1.427(4) yes
Ti3 . O4 . 2.053(2) yes
Ti3 . O12 . 1.860(2) yes
Ti3 . N15 . 2.349(3) yes
Ti3 . O18 . 1.880(3) yes
Ti3 . O20 . 1.812(2) yes
O4 . C5 . 1.423(4) yes
C5 . C6 . 1.519(5) yes
C5 . H52 . 0.972 no
C5 . H51 . 0.964 no
C6 . N7 . 1.489(5) yes
C6 . H62 . 0.953 no
C6 . H61 . 0.967 no
N7 . C8 . 1.476(4) yes
N7 . C11 . 1.485(5) yes
C8 . C9 . 1.508(5) yes
C8 . H81 . 0.974 no
C8 . H82 . 0.962 no
C9 . O10 . 1.406(4) yes
C9 . H92 . 0.946 no
C9 . H91 . 0.970 no
C11 . H112 . 0.950 no
C11 . H111 . 0.951 no
C11 . H113 . 0.949 no
O12 . C13 . 1.402(4) yes
C13 . C14 . 1.508(5) yes
C13 . H131 . 0.982 no
C13 . H132 . 0.963 no
C14 . N15 . 1.480(5) yes
C14 . H142 . 0.974 no
C14 . H141 . 0.985 no
N15 . C16 . 1.484(4) yes
N15 . C19 . 1.472(4) yes
C16 . C17 . 1.513(5) yes
C16 . H162 . 0.982 no
C16 . H161 . 0.983 no
C17 . O18 . 1.405(5) yes
C17 . H171 . 0.991 no
C17 . H172 . 0.956 no
C19 . H193 . 0.991 no
C19 . H192 . 0.953 no
C19 . H191 . 0.969 no
O20 . C21 . 1.413(4) yes
C21 . C22 . 1.490(6) yes
C21 . H212 . 0.967 no
C21 . H211 . 0.981 no
C22 . H222 . 0.956 no
C22 . H221 . 0.983 no
C22 . H223 . 0.955 no
C23 . C24 . 1.508(6) yes
C23 . H232 . 0.962 no
C23 . H231 . 0.962 no
C24 . H243 . 0.964 no
C24 . H242 . 0.948 no
C24 . H241 . 0.936 no
O25 . C26 . 1.408(4) yes
C26 . C27 . 1.513(6) yes
C26 . H261 . 0.965 no
C26 . H262 . 0.973 no
C27 . H271 . 0.963 no
C27 . H273 . 0.948 no
C27 . H272 . 0.955 no
O28 . C29 . 1.409(4) yes
C29 . C30 . 1.510(5) yes
C29 . H292 . 0.979 no
C29 . H291 . 0.958 no
C30 . H302 . 0.969 no
C30 . H301 . 0.977 no
C30 . H303 . 0.966 no
O31 . C32 . 1.3484(10) yes
O31 . H312 . 0.81(2) no
C32 . C32 2_665 1.498(8) yes
C32 . H325 . 0.905 no
C32 . H324 . 1.031 no
C32 . H323 . 0.990 no
C32 . H322 . 0.980 no
C32 . H321 . 0.954 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 . Ti1 . O4 . 69.78(8) yes
O2 . Ti1 . N7 . 103.84(9) yes
O4 . Ti1 . N7 . 74.07(9) yes
O2 . Ti1 . O10 . 161.66(10) yes
O4 . Ti1 . O10 . 92.69(9) yes
N7 . Ti1 . O10 . 75.25(10) yes
O2 . Ti1 . O25 . 93.29(10) yes
O4 . Ti1 . O25 . 145.06(10) yes
N7 . Ti1 . O25 . 81.18(10) yes
O10 . Ti1 . O25 . 104.55(11) yes
O2 . Ti1 . O28 . 91.42(9) yes
O4 . Ti1 . O28 . 109.18(10) yes
N7 . Ti1 . O28 . 164.42(10) yes
O10 . Ti1 . O28 . 89.29(10) yes
O25 . Ti1 . O28 . 101.32(11) yes
Ti1 . O2 . Ti3 . 110.02(10) yes
Ti1 . O2 . C23 . 122.12(19) yes
Ti3 . O2 . C23 . 127.4(2) yes
O2 . Ti3 . O4 . 70.53(8) yes
O2 . Ti3 . O12 . 92.46(10) yes
O4 . Ti3 . O12 . 157.65(10) yes
O2 . Ti3 . N15 . 91.85(9) yes
O4 . Ti3 . N15 . 89.24(9) yes
O12 . Ti3 . N15 . 76.56(10) yes
O2 . Ti3 . O18 . 156.53(10) yes
O4 . Ti3 . O18 . 88.61(10) yes
O12 . Ti3 . O18 . 104.47(11) yes
N15 . Ti3 . O18 . 76.79(10) yes
O2 . Ti3 . O20 . 100.65(11) yes
O4 . Ti3 . O20 . 103.31(10) yes
O12 . Ti3 . O20 . 93.82(11) yes
N15 . Ti3 . O20 . 164.61(10) yes
O18 . Ti3 . O20 . 94.41(12) yes
Ti1 . O4 . Ti3 . 108.53(9) yes
Ti1 . O4 . C5 . 114.88(18) yes
Ti3 . O4 . C5 . 121.95(18) yes
O4 . C5 . C6 . 107.7(3) yes
O4 . C5 . H52 . 110.5 no
C6 . C5 . H52 . 108.8 no
O4 . C5 . H51 . 111.0 no
C6 . C5 . H51 . 109.4 no
H52 . C5 . H51 . 109.3 no
C5 . C6 . N7 . 111.4(2) yes
C5 . C6 . H62 . 109.1 no
N7 . C6 . H62 . 109.4 no
C5 . C6 . H61 . 107.8 no
N7 . C6 . H61 . 108.9 no
H62 . C6 . H61 . 110.4 no
Ti1 . N7 . C6 . 108.64(19) yes
Ti1 . N7 . C8 . 100.69(19) yes
C6 . N7 . C8 . 112.6(3) yes
Ti1 . N7 . C11 . 115.8(2) yes
C6 . N7 . C11 . 109.7(3) yes
C8 . N7 . C11 . 109.3(3) yes
N7 . C8 . C9 . 108.7(3) yes
N7 . C8 . H81 . 108.5 no
C9 . C8 . H81 . 110.8 no
N7 . C8 . H82 . 109.4 no
C9 . C8 . H82 . 109.8 no
H81 . C8 . H82 . 109.6 no
C8 . C9 . O10 . 109.3(3) yes
C8 . C9 . H92 . 110.3 no
O10 . C9 . H92 . 110.7 no
C8 . C9 . H91 . 109.7 no
O10 . C9 . H91 . 109.3 no
H92 . C9 . H91 . 107.5 no
C9 . O10 . Ti1 . 125.3(2) yes
N7 . C11 . H112 . 109.7 no
N7 . C11 . H111 . 109.2 no
H112 . C11 . H111 . 109.9 no
N7 . C11 . H113 . 107.1 no
H112 . C11 . H113 . 109.4 no
H111 . C11 . H113 . 111.4 no
Ti3 . O12 . C13 . 126.5(2) yes
O12 . C13 . C14 . 108.9(3) yes
O12 . C13 . H131 . 109.5 no
C14 . C13 . H131 . 107.6 no
O12 . C13 . H132 . 110.2 no
C14 . C13 . H132 . 110.9 no
H131 . C13 . H132 . 109.6 no
C13 . C14 . N15 . 109.6(3) yes
C13 . C14 . H142 . 110.1 no
N15 . C14 . H142 . 108.3 no
C13 . C14 . H141 . 109.9 no
N15 . C14 . H141 . 109.9 no
H142 . C14 . H141 . 109.0 no
Ti3 . N15 . C14 . 103.8(2) yes
Ti3 . N15 . C16 . 104.61(19) yes
C14 . N15 . C16 . 111.6(3) yes
Ti3 . N15 . C19 . 116.3(2) yes
C14 . N15 . C19 . 109.4(3) yes
C16 . N15 . C19 . 110.9(3) yes
N15 . C16 . C17 . 107.6(3) yes
N15 . C16 . H162 . 109.0 no
C17 . C16 . H162 . 110.0 no
N15 . C16 . H161 . 108.9 no
C17 . C16 . H161 . 110.8 no
H162 . C16 . H161 . 110.5 no
C16 . C17 . O18 . 107.3(3) yes
C16 . C17 . H171 . 109.7 no
O18 . C17 . H171 . 109.1 no
C16 . C17 . H172 . 110.2 no
O18 . C17 . H172 . 110.6 no
H171 . C17 . H172 . 110.0 no
C17 . O18 . Ti3 . 122.2(2) yes
N15 . C19 . H193 . 110.5 no
N15 . C19 . H192 . 109.2 no
H193 . C19 . H192 . 108.6 no
N15 . C19 . H191 . 110.7 no
H193 . C19 . H191 . 110.2 no
H192 . C19 . H191 . 107.5 no
Ti3 . O20 . C21 . 133.5(2) yes
O20 . C21 . C22 . 109.8(3) yes
O20 . C21 . H212 . 107.3 no
C22 . C21 . H212 . 107.3 no
O20 . C21 . H211 . 112.3 no
C22 . C21 . H211 . 108.9 no
H212 . C21 . H211 . 111.2 no
C21 . C22 . H222 . 107.4 no
C21 . C22 . H221 . 107.7 no
H222 . C22 . H221 . 111.4 no
C21 . C22 . H223 . 109.3 no
H222 . C22 . H223 . 110.4 no
H221 . C22 . H223 . 110.4 no
O2 . C23 . C24 . 111.1(3) yes
O2 . C23 . H232 . 108.4 no
C24 . C23 . H232 . 109.3 no
O2 . C23 . H231 . 109.9 no
C24 . C23 . H231 . 108.6 no
H232 . C23 . H231 . 109.6 no
C23 . C24 . H243 . 108.1 no
C23 . C24 . H242 . 109.2 no
H243 . C24 . H242 . 108.7 no
C23 . C24 . H241 . 109.6 no
H243 . C24 . H241 . 111.2 no
H242 . C24 . H241 . 110.1 no
Ti1 . O25 . C26 . 142.3(2) yes
O25 . C26 . C27 . 110.2(3) yes
O25 . C26 . H261 . 109.6 no
C27 . C26 . H261 . 107.4 no
O25 . C26 . H262 . 110.8 no
C27 . C26 . H262 . 110.3 no
H261 . C26 . H262 . 108.5 no
C26 . C27 . H271 . 108.9 no
C26 . C27 . H273 . 109.6 no
H271 . C27 . H273 . 110.3 no
C26 . C27 . H272 . 107.8 no
H271 . C27 . H272 . 109.4 no
H273 . C27 . H272 . 110.8 no
Ti1 . O28 . C29 . 138.1(2) yes
O28 . C29 . C30 . 111.1(3) yes
O28 . C29 . H292 . 108.2 no
C30 . C29 . H292 . 107.1 no
O28 . C29 . H291 . 110.1 no
C30 . C29 . H291 . 109.3 no
H292 . C29 . H291 . 111.1 no
C29 . C30 . H302 . 108.5 no
C29 . C30 . H301 . 109.1 no
H302 . C30 . H301 . 109.6 no
C29 . C30 . H303 . 109.5 no
H302 . C30 . H303 . 110.1 no
H301 . C30 . H303 . 110.1 no
C32 . O31 . H312 . 92(9) no
C32 2_665 C32 . O31 . 100.0(6) yes
C32 2_665 C32 . H325 . 113.6 no
C32 2_665 C32 . H324 . 108.2 no
O31 . C32 . H324 . 113.3 no
H325 . C32 . H324 . 105.7 no
C32 2_665 C32 . H323 . 105.5 no
O31 . C32 . H323 . 117.2 no
H325 . C32 . H323 . 109.8 no
C32 2_665 C32 . H322 . 112.7 no
O31 . C32 . H322 . 111.8 no
H325 . C32 . H322 . 106.0 no
H324 . C32 . H322 . 110.4 no
H323 . C32 . H322 . 109.3 no
C32 2_665 C32 . H321 . 109.0 no
O31 . C32 . H321 . 118.3 no
H325 . C32 . H321 . 112.6 no
H324 . C32 . H321 . 107.4 no
H323 . C32 . H321 . 105.9 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C6 . H61 . O20 . 129 0.97 2.58 3.281(6) yes
C19 . H192 . O28 . 137 0.95 2.57 3.332(6) yes
O31 . H312 . O10 . 156(12) 0.809 2.218 2.977(6) yes


####################################################################### 
# 
# 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_smrb101_4
_database_code_depnum_ccdc_archive 'CCDC 2013426'
loop_
_audit_author_name
_audit_author_address
'Erwann Jeanneau'
;universite de Lyon
France
;
_audit_update_record             
;
2020-07-01 deposited with the CCDC.	2021-01-14 downloaded from the CCDC.
;
_audit_creation_date             2020-06-26
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H20 N2 O4 Pb2'
_chemical_formula_sum            'C10 H20 N2 O4 Pb2'
_chemical_formula_weight         646.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C5 H10 N1 O2 Pb1'
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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   16.674(3)
_cell_length_b                   10.4513(13)
_cell_length_c                   22.478(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.767(15)
_cell_angle_gamma                90
_cell_volume                     3709.0(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5417
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.2820
_cell_measurement_theta_min      3.8010
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    18.139
_exptl_absorpt_correction_T_max  0.083
_exptl_absorpt_correction_T_min  0.021
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.316
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -8 24 0.1309
-5 9 -22 0.1737
21 -1 -22 0.1714
-21 1 22 0.1879
-7 -12 -13 0.1377
7 12 13 0.1360
-21 -6 15 0.1680
-15 5 27 0.1562
19 8 -9 0.1832
10 -8 -26 0.2018
0 -13 13 0.0823
0 13 -13 0.1312
-17 10 10 0.1869
17 -10 -10 0.1869
-4 -15 4 0.0865
-6 14 8 0.1332
6 -14 -8 0.1332

_exptl_crystal_size_max          0.517
_exptl_crystal_size_mid          0.366
_exptl_crystal_size_min          0.214
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.3632 -8.1882 24.2370 -0.5999 0.7019 -0.3841
-4.6347 8.5622 -21.6302 0.6296 -0.7374 0.2447
21.1809 -0.7722 -22.0770 -0.0716 0.0890 0.9935
-21.1771 0.7678 22.0865 0.0713 -0.0886 -0.9935
-6.6074 -11.8458 -12.9494 -0.7609 -0.6486 0.0204
6.6045 11.8457 12.9528 0.7609 0.6486 -0.0206
-21.0055 -5.9494 15.0898 -0.3715 -0.3128 -0.8742
-14.5619 5.3121 27.2026 0.3518 0.3037 -0.8855
19.4620 8.2918 -9.0498 0.5236 0.4431 0.7276
10.0863 -7.8503 -26.2415 -0.5129 -0.4404 0.7368
0.3027 -13.2157 13.1064 -0.9178 0.3252 -0.2280
-0.1784 13.1983 -13.2354 0.9165 -0.3247 0.2338
-17.1141 10.0235 9.9919 0.7074 -0.2537 -0.6597
17.1141 -10.0235 -9.9919 -0.7074 0.2537 0.6597
-3.5066 -14.5400 3.7898 -0.9807 -0.0768 -0.1796
-6.4062 13.9536 7.9980 0.9476 0.0725 -0.3112
6.4062 -13.9536 -7.9980 -0.9476 -0.0725 0.3112

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            16609
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.628
_diffrn_reflns_theta_min         3.274
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -41.00  62.00   1.00   10.00    --  -11.61  57.00 -90.00  103
  2  ω   -100.00 -32.00   1.00   10.00    --  -11.61 178.00-120.00   68
  3  ω    -75.00  20.00   1.00   10.00    --  -11.61 -77.00 -90.00   95
  4  ω    -83.00   9.00   1.00   10.00    --  -11.61 -57.00 120.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0027279000
_diffrn_orient_matrix_UB_12      0.0676550000
_diffrn_orient_matrix_UB_13      -0.0017408000
_diffrn_orient_matrix_UB_21      0.0341330000
_diffrn_orient_matrix_UB_22      0.0044963000
_diffrn_orient_matrix_UB_23      0.0285578000
_diffrn_orient_matrix_UB_31      0.0290236000
_diffrn_orient_matrix_UB_32      0.0008736000
_diffrn_orient_matrix_UB_33      -0.0171845000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\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                3790
_reflns_number_total             4637
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.633
_refine_diff_density_min         -2.662
_refine_diff_density_rms         0.350
_refine_ls_extinction_coef       0.00034(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         4637
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0499
_refine_ls_restrained_S_all      1.126
_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)+(0.0652P)²+41.3827P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1403
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Pb1 Pb 0.65503(2) 0.75719(4) 0.67166(2) 0.03031(15) Uani 1 1 d . . . . .
Pb2 Pb 0.50956(2) 0.47454(4) 0.58704(2) 0.02637(15) Uani 1 1 d . . . . .
O1 O 0.5070(5) 0.6975(7) 0.5855(3) 0.0357(17) Uani 1 1 d . . . . .
O2 O 0.6973(5) 0.8030(8) 0.7770(3) 0.0367(17) Uani 1 1 d . . . . .
O3 O 0.6183(4) 0.5593(7) 0.6850(3) 0.0325(15) Uani 1 1 d . . . . .
O4 O 0.5854(4) 0.5037(7) 0.5255(3) 0.0290(15) Uani 1 1 d . . . . .
N1 N 0.5268(6) 0.8154(8) 0.7060(4) 0.0326(19) Uani 1 1 d . . . . .
N2 N 0.6550(5) 0.3280(8) 0.6274(4) 0.0280(17) Uani 1 1 d . . . . .
C1 C 0.4395(8) 0.7524(13) 0.5992(6) 0.052(4) Uani 1 1 d . . . . .
H1 H 0.393047 0.788717 0.569028 0.062 Uiso 1 1 calc R U . . .
C2 C 0.4495(7) 0.7470(9) 0.6686(5) 0.033(2) Uani 1 1 d . . . . .
H2A H 0.400428 0.785628 0.675676 0.039 Uiso 1 1 calc R U . . .
H2B H 0.452689 0.658474 0.682100 0.039 Uiso 1 1 calc R U . . .
C3 C 0.5135(11) 0.9527(13) 0.7017(9) 0.073(5) Uani 1 1 d . . . . .
H3A H 0.564825 0.995503 0.725262 0.109 Uiso 1 1 calc R U . . .
H3B H 0.469198 0.974858 0.718583 0.109 Uiso 1 1 calc R U . . .
H3C H 0.497526 0.978652 0.658523 0.109 Uiso 1 1 calc R U . . .
C4 C 0.5537(8) 0.7775(14) 0.7724(6) 0.048(3) Uani 1 1 d . . . . .
H4A H 0.554354 0.684897 0.775135 0.058 Uiso 1 1 calc R U . . .
H4B H 0.512800 0.809015 0.791340 0.058 Uiso 1 1 calc R U . . .
C5 C 0.6384(7) 0.8271(14) 0.8082(6) 0.052(3) Uani 1 1 d . . . . .
H5 H 0.651042 0.869098 0.846556 0.062 Uiso 1 1 calc R U . . .
C6 C 0.6772(8) 0.4657(11) 0.7213(5) 0.041(3) Uani 1 1 d . . . . .
H6A H 0.647715 0.405513 0.739830 0.049 Uiso 1 1 calc R U . . .
H6B H 0.720654 0.507717 0.755080 0.049 Uiso 1 1 calc R U . . .
C7 C 0.7179(6) 0.3943(11) 0.6791(4) 0.034(2) Uani 1 1 d . . . . .
H7A H 0.748776 0.454713 0.661978 0.040 Uiso 1 1 calc R U . . .
H7B H 0.758055 0.332447 0.704123 0.040 Uiso 1 1 calc R U . . .
C8 C 0.6364(8) 0.2032(12) 0.6459(5) 0.043(3) Uani 1 1 d . . . . .
H8A H 0.616824 0.210477 0.681573 0.064 Uiso 1 1 calc R U . . .
H8B H 0.686657 0.151577 0.656909 0.064 Uiso 1 1 calc R U . . .
H8C H 0.593197 0.163879 0.611753 0.064 Uiso 1 1 calc R U . . .
C9 C 0.6778(6) 0.3250(10) 0.5691(4) 0.029(2) Uani 1 1 d . . . . .
H9A H 0.641702 0.264117 0.540013 0.035 Uiso 1 1 calc R U . . .
H9B H 0.735946 0.296349 0.578833 0.035 Uiso 1 1 calc R U . . .
C10 C 0.6684(6) 0.4541(11) 0.5386(4) 0.032(2) Uani 1 1 d . . . . .
H10A H 0.708552 0.512804 0.566072 0.039 Uiso 1 1 calc R U . . .
H10B H 0.681600 0.447619 0.499706 0.039 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
Pb1 O1 2.676(7) . ?
Pb1 O2 2.292(7) . ?
Pb1 O2 2.441(7) 7_666 ?
Pb1 O3 2.205(7) . ?
Pb1 N1 2.569(9) . ?
Pb2 O1 2.330(8) . ?
Pb2 O3 2.521(7) . ?
Pb2 O4 2.174(6) . ?
Pb2 O4 2.527(6) 5_666 ?
Pb2 N2 2.763(8) . ?
O1 C1 1.383(14) . ?
O2 C5 1.402(13) . ?
O3 C6 1.439(13) . ?
O4 C10 1.417(12) . ?
N1 C2 1.477(14) . ?
N1 C3 1.451(15) . ?
N1 C4 1.467(15) . ?
N2 C7 1.466(13) . ?
N2 C8 1.433(14) . ?
N2 C9 1.478(12) . ?
C1 H1 0.9300 . ?
C1 C2 1.517(16) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.476(17) . ?
C5 H5 0.9300 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.526(15) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.499(14) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?

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
O2 Pb1 O1 134.6(2) . . ?
O2 Pb1 O1 146.9(2) 7_666 . ?
O2 Pb1 O2 68.7(3) . 7_666 ?
O2 Pb1 N1 136.8(2) 7_666 . ?
O2 Pb1 N1 69.5(3) . . ?
O3 Pb1 O1 69.4(2) . . ?
O3 Pb1 O2 88.6(3) . 7_666 ?
O3 Pb1 O2 93.6(3) . . ?
O3 Pb1 N1 83.5(3) . . ?
N1 Pb1 O1 67.0(2) . . ?
O1 Pb2 O3 70.5(2) . . ?
O1 Pb2 O4 83.8(2) . 5_666 ?
O1 Pb2 N2 124.7(3) . . ?
O3 Pb2 O4 152.4(2) . 5_666 ?
O3 Pb2 N2 66.4(2) . . ?
O4 Pb2 O1 82.1(3) . . ?
O4 Pb2 O3 96.0(3) . . ?
O4 Pb2 O4 69.9(3) . 5_666 ?
O4 Pb2 N2 70.0(2) . . ?
O4 Pb2 N2 125.4(2) 5_666 . ?
Pb2 O1 Pb1 102.4(2) . . ?
C1 O1 Pb1 111.7(7) . . ?
C1 O1 Pb2 115.1(8) . . ?
Pb1 O2 Pb1 111.3(3) . 7_666 ?
C5 O2 Pb1 124.9(7) . 7_666 ?
C5 O2 Pb1 121.4(6) . . ?
Pb1 O3 Pb2 111.3(3) . . ?
C6 O3 Pb1 123.1(7) . . ?
C6 O3 Pb2 115.1(6) . . ?
Pb2 O4 Pb2 110.1(3) . 5_666 ?
C10 O4 Pb2 123.1(5) . . ?
C10 O4 Pb2 119.7(5) . 5_666 ?
C2 N1 Pb1 111.9(6) . . ?
C3 N1 Pb1 109.8(8) . . ?
C3 N1 C2 110.7(10) . . ?
C3 N1 C4 108.9(11) . . ?
C4 N1 Pb1 103.3(6) . . ?
C4 N1 C2 111.9(9) . . ?
C7 N2 Pb2 109.1(6) . . ?
C7 N2 C9 113.0(8) . . ?
C8 N2 Pb2 110.6(6) . . ?
C8 N2 C7 111.5(8) . . ?
C8 N2 C9 112.3(8) . . ?
C9 N2 Pb2 99.8(5) . . ?
O1 C1 H1 123.7 . . ?
O1 C1 C2 112.6(9) . . ?
C2 C1 H1 123.7 . . ?
N1 C2 C1 110.8(10) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 . . ?
N1 C4 C5 112.6(11) . . ?
H4A C4 H4B 107.8 . . ?
C5 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
O2 C5 C4 111.5(9) . . ?
O2 C5 H5 124.2 . . ?
C4 C5 H5 124.2 . . ?
O3 C6 H6A 109.7 . . ?
O3 C6 H6B 109.7 . . ?
O3 C6 C7 109.8(8) . . ?
H6A C6 H6B 108.2 . . ?
C7 C6 H6A 109.7 . . ?
C7 C6 H6B 109.7 . . ?
N2 C7 C6 112.1(9) . . ?
N2 C7 H7A 109.2 . . ?
N2 C7 H7B 109.2 . . ?
C6 C7 H7A 109.2 . . ?
C6 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
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 C9 H9A 109.3 . . ?
N2 C9 H9B 109.3 . . ?
N2 C9 C10 111.6(8) . . ?
H9A C9 H9B 108.0 . . ?
C10 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
O4 C10 C9 112.1(8) . . ?
O4 C10 H10A 109.2 . . ?
O4 C10 H10B 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?

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
Pb1 O1 C1 C2 -40.8(12) . . . . ?
Pb1 O2 C5 C4 19.2(15) . . . . ?
Pb1 O2 C5 C4 -141.8(9) 7_666 . . . ?
Pb1 O3 C6 C7 -89.3(10) . . . . ?
Pb1 N1 C2 C1 -45.7(10) . . . . ?
Pb1 N1 C4 C5 49.4(11) . . . . ?
Pb2 O1 C1 C2 75.4(11) . . . . ?
Pb2 O3 C6 C7 52.5(11) . . . . ?
Pb2 O4 C10 C9 -111.3(7) 5_666 . . . ?
Pb2 O4 C10 C9 36.4(11) . . . . ?
Pb2 N2 C7 C6 36.0(9) . . . . ?
Pb2 N2 C9 C10 43.6(8) . . . . ?
O1 C1 C2 N1 59.9(13) . . . . ?
O3 C6 C7 N2 -59.8(12) . . . . ?
N1 C4 C5 O2 -48.7(16) . . . . ?
N2 C9 C10 O4 -56.5(11) . . . . ?
C2 N1 C4 C5 169.9(10) . . . . ?
C3 N1 C2 C1 77.2(12) . . . . ?
C3 N1 C4 C5 -67.4(13) . . . . ?
C4 N1 C2 C1 -161.1(9) . . . . ?
C7 N2 C9 C10 -72.1(10) . . . . ?
C8 N2 C7 C6 -86.4(11) . . . . ?
C8 N2 C9 C10 160.7(9) . . . . ?
C9 N2 C7 C6 146.0(8) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.807 0.000 0.500 497.1 63.6 ?
2 -0.181 0.500 1.000 497.1 63.6 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2016-05-11
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id smeb101_4
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.505
_oxdiff_exptl_absorpt_empirical_full_min 0.668
####################################################################### 
# 
# 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_smr-b-xxx
_database_code_depnum_ccdc_archive 'CCDC 2034796'
loop_
_audit_author_name
_audit_author_address
'Erwann Jeanneau'
;universite de Lyon
France
;
_audit_update_record             
;
2020-09-30 deposited with the CCDC.	2021-01-14 downloaded from the CCDC.
;
_audit_creation_date             2020-09-30
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H27 N2 Nb2 O8'
_chemical_formula_sum            'C12 H27 N2 Nb2 O8'
_chemical_formula_weight         513.17
_chemical_absolute_configuration unk
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C24 H56 N4 Nb4 O16'
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'
Nb Nb -2.0727 0.6215 '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      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'I 1 2 1'
_space_group_name_Hall           'I 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'

_cell_length_a                   12.8106(13)
_cell_length_b                   10.2674(13)
_cell_length_c                   18.4561(18)
_cell_angle_alpha                90
_cell_angle_beta                 106.473(10)
_cell_angle_gamma                90
_cell_volume                     2327.9(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7625
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.2260
_cell_measurement_theta_min      3.3870
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 11 -14 0.0916
8 -5 17 0.0873
-4 -14 7 0.0704
-10 -11 -6 0.1132
10 11 5 0.0992
-17 1 14 0.0726
18 -1 -13 0.0924
2 8 20 0.0900
2 -7 -22 0.1103
3 -14 -3 0.0737
-3 14 3 0.1117
16 4 -17 0.0969
-8 1 26 0.0954

_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.168
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.3486 10.9926 -14.2093 -0.8399 0.5153 0.1702
8.3789 -5.4440 16.6053 0.6604 -0.4063 -0.6316
-3.6599 -13.8439 6.6803 0.7713 -0.4719 0.4270
-10.2156 -10.5061 -5.5203 0.3149 -0.1909 0.9297
10.1943 10.5406 5.4603 -0.3179 0.1928 -0.9283
-17.4242 1.0349 13.5492 0.4749 0.7730 0.4207
17.5792 -0.7596 -12.8799 -0.4667 -0.7595 -0.4532
2.2340 7.6865 19.9669 0.2800 0.4600 -0.8426
2.4404 -7.4291 -22.1168 -0.3841 -0.6291 0.6758
3.3853 -14.1751 -3.1693 0.4448 -0.8182 0.3643
-3.0079 14.2078 3.4549 -0.4400 0.8091 -0.3897
15.7853 3.7591 -16.7358 -0.7499 -0.5159 -0.4142
-7.8002 0.9034 25.6362 0.7817 0.5364 -0.3182

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16317
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.610
_diffrn_reflns_theta_min         3.134
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -38.00  63.00   1.00   42.24    --  -10.24  57.00-180.00  101
  2  ω    -51.00  70.00   1.00   42.24    --  -10.24  19.00 -60.00  121
  3  ω    -21.00  39.00   1.00   42.24    --   11.34  77.00  90.00   60
  4  ω    -85.00  14.00   1.00   42.24    --  -10.24 -37.00 150.00   99
  5  ω    -21.00  39.00   1.00   42.24    --   11.34  77.00 -30.00   60
  6  ω    -18.00   7.00   1.00   42.24    --   11.34 -77.00 -60.00   25
  7  ω    -13.00  47.00   1.00   42.24    --   11.34 -88.00  71.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0063029000
_diffrn_orient_matrix_UB_12      -0.0395880000
_diffrn_orient_matrix_UB_13      0.0299691000
_diffrn_orient_matrix_UB_21      -0.0348082000
_diffrn_orient_matrix_UB_22      0.0474699000
_diffrn_orient_matrix_UB_23      0.0086589000
_diffrn_orient_matrix_UB_31      -0.0455692000
_diffrn_orient_matrix_UB_32      -0.0309513000
_diffrn_orient_matrix_UB_33      -0.0251867000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\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         0.782
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.787
_reflns_number_gt                4310
_reflns_number_total             5581
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         3.208
_refine_diff_density_min         -1.752
_refine_diff_density_rms         0.188
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         5581
_refine_ls_number_restraints     396
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0809
_refine_ls_restrained_S_all      1.166
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1415P)²+15.8238P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2233
_refine_ls_wR_factor_ref         0.2488
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.51(13)
 0.49(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C8-C7
 2.6 with sigma of 0.04
 N1-C5 \\sim N1-C3 \\sim N1-C2 \\sim N2-C8 \\sim N2-C7 \\sim N2-C10
 with sigma of 0.02
 C10-C11 \\sim C9-C8 \\sim C2-C1 \\sim C3-C4
 with sigma of 0.02
 O7-C11 \\sim O5-C9 \\sim O3-C1 \\sim O2-C4 \\sim O4-C6 \\sim O6-C12
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Nb1 \\sim Nb2 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7
\\sim O8 \\sim N1 \\sim N2 \\sim C1 \\sim C2 \\sim C4 \\sim C5 \\sim C6 \\sim
C7 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Nb1 \\sim Nb2 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7
\\sim O8 \\sim N1 \\sim N2 \\sim C1 \\sim C2 \\sim C4 \\sim C5 \\sim C6 \\sim
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Nb1 \\sim Nb2 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7
\\sim O8 \\sim N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim
C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
5. Rigid body (RIGU) restrains
 Nb1, Nb2, O1, O2, O3, O4, O5, O6, O7, O8, N1, N2, C1, C2, C4, C5, C6, C7, C10,
  C11, C12
 with sigma for 1-2 distances of 0.0004 and sigma for 1-3 distances of 0.0004
 Nb1, Nb2, O1, O2, O3, O4, O5, O6, O7, O8, N1, N2, C1, C2, C4, C5, C6, C7, C8,
 C9, C10, C11, C12
 with sigma for 1-2 distances of 0.0004 and sigma for 1-3 distances of 0.0004
 Nb1, Nb2, O1, O2, O3, O4, O5, O6, O7, O8, N1, N2, C1, C2, C3, C4, C5, C6, C7,
 C8, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4)
6.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Nb1 Nb 0.28083(7) 0.63072(9) 0.45341(5) 0.0437(3) Uani 1 1 d . U . . .
Nb2 Nb 0.49409(7) 0.63168(16) 0.64461(5) 0.0514(3) Uani 1 1 d . U . . .
O1 O 0.3681(6) 0.6272(14) 0.5512(4) 0.0481(6) Uani 1 1 d . U . . .
O2 O 0.2738(7) 0.4545(10) 0.4253(5) 0.0487(7) Uani 1 1 d D U . . .
O3 O 0.1402(6) 0.6221(12) 0.4733(4) 0.0487(7) Uani 1 1 d D U . . .
O4 O 0.2729(7) 0.8211(10) 0.4445(5) 0.0475(8) Uani 1 1 d D U . . .
O5 O 0.4689(9) 0.8268(12) 0.6388(5) 0.0602(12) Uani 1 1 d D U . . .
O6 O 0.4720(7) 0.4646(11) 0.6590(5) 0.0551(7) Uani 1 1 d D U . . .
O7 O 0.5667(7) 0.6530(11) 0.7521(4) 0.0573(7) Uani 1 1 d D U . . .
O8 O 0.6117(6) 0.6153(14) 0.6075(4) 0.0536(7) Uani 1 1 d . U . . .
N1 N 0.1512(8) 0.5916(11) 0.3300(6) 0.0545(10) Uani 1 1 d D U . . .
N2 N 0.3479(8) 0.6619(12) 0.7053(5) 0.0625(10) Uani 1 1 d D U . . .
C1 C 0.0425(9) 0.6513(15) 0.4161(6) 0.0521(9) Uani 1 1 d D U . . .
H1A H 0.035004 0.744743 0.408604 0.063 Uiso 1 1 calc R U . . .
H1B H -0.019968 0.619362 0.430542 0.063 Uiso 1 1 calc R U . . .
C2 C 0.0489(10) 0.5868(15) 0.3457(7) 0.0541(10) Uani 1 1 d D U . . .
H2A H 0.028949 0.496121 0.347970 0.065 Uiso 1 1 calc R U . . .
H2B H -0.005048 0.626263 0.303658 0.065 Uiso 1 1 calc R U . . .
C3 C 0.1770(18) 0.4688(17) 0.3053(10) 0.093(5) Uani 1 1 d D U . . .
H3A H 0.219205 0.483048 0.269845 0.111 Uiso 1 1 calc R U . . .
H3B H 0.109586 0.426887 0.277687 0.111 Uiso 1 1 calc R U . . .
C4 C 0.2375(10) 0.3782(14) 0.3635(7) 0.0513(10) Uani 1 1 d D U . . .
H4 H 0.248425 0.289314 0.359078 0.062 Uiso 1 1 calc R U . . .
C5 C 0.1521(11) 0.6858(15) 0.2730(7) 0.0590(15) Uani 1 1 d D U . . .
H5A H 0.089122 0.740687 0.264605 0.088 Uiso 1 1 calc R U . . .
H5B H 0.151171 0.641943 0.226903 0.088 Uiso 1 1 calc R U . . .
H5C H 0.216712 0.738052 0.289331 0.088 Uiso 1 1 calc R U . . .
C6 C 0.2952(11) 0.9196(14) 0.3948(7) 0.0525(14) Uani 1 1 d D U . . .
H6A H 0.275564 0.887032 0.343934 0.079 Uiso 1 1 calc R U . . .
H6B H 0.371363 0.940547 0.410356 0.079 Uiso 1 1 calc R U . . .
H6C H 0.253511 0.996346 0.397050 0.079 Uiso 1 1 calc R U . . .
C7 C 0.2597(11) 0.5698(17) 0.6851(8) 0.0667(16) Uani 1 1 d D U . . .
H7A H 0.242679 0.550631 0.632074 0.100 Uiso 1 1 calc R U . . .
H7B H 0.196854 0.606185 0.696057 0.100 Uiso 1 1 calc R U . . .
H7C H 0.280697 0.491095 0.713567 0.100 Uiso 1 1 calc R U . . .
C8 C 0.2933(13) 0.7827(16) 0.6696(9) 0.0748(19) Uani 1 1 d D U . . .
H8A H 0.258526 0.824067 0.703962 0.090 Uiso 1 1 calc R U . . .
H8B H 0.236707 0.759629 0.624138 0.090 Uiso 1 1 calc R U . . .
C9 C 0.3680(12) 0.8780(18) 0.6496(10) 0.075(2) Uani 1 1 d D U . . .
H9A H 0.328341 0.921720 0.603382 0.090 Uiso 1 1 calc R U . . .
H9B H 0.386832 0.943420 0.689078 0.090 Uiso 1 1 calc R U . . .
C10 C 0.4005(10) 0.7072(18) 0.7795(7) 0.0619(10) Uani 1 1 d D U . . .
H10A H 0.359802 0.676791 0.813220 0.074 Uiso 1 1 calc R U . . .
H10B H 0.398211 0.801618 0.779357 0.074 Uiso 1 1 calc R U . . .
C11 C 0.5121(9) 0.6662(17) 0.8090(7) 0.0599(9) Uani 1 1 d D U . . .
H11A H 0.550732 0.729221 0.846148 0.072 Uiso 1 1 calc R U . . .
H11B H 0.513930 0.583271 0.834574 0.072 Uiso 1 1 calc R U . . .
C12 C 0.4150(11) 0.3562(16) 0.6212(8) 0.0626(15) Uani 1 1 d D U . . .
H12A H 0.436692 0.339560 0.576335 0.094 Uiso 1 1 calc R U . . .
H12B H 0.338248 0.373481 0.607605 0.094 Uiso 1 1 calc R U . . .
H12C H 0.431106 0.281455 0.653697 0.094 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
Nb1 O1 1.834(7) . ?
Nb1 O2 1.877(10) . ?
Nb1 O3 1.940(7) . ?
Nb1 O4 1.962(10) . ?
Nb1 O8 2.015(7) 2_656 ?
Nb1 N1 2.442(11) . ?
Nb2 O1 2.000(7) . ?
Nb2 O5 2.027(12) . ?
Nb2 O6 1.771(11) . ?
Nb2 O7 1.950(8) . ?
Nb2 O8 1.831(7) . ?
Nb2 N2 2.459(10) . ?
O2 C4 1.353(13) . ?
O3 C1 1.421(12) . ?
O4 C6 1.447(13) . ?
O5 C9 1.460(15) . ?
O6 C12 1.404(15) . ?
O7 C11 1.425(12) . ?
N1 C2 1.420(13) . ?
N1 C3 1.412(15) . ?
N1 C5 1.432(13) . ?
N2 C7 1.439(14) . ?
N2 C8 1.484(15) . ?
N2 C10 1.422(14) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.480(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.467(17) . ?
C4 H4 0.9300 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.486(18) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.441(15) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 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
O1 Nb1 O2 102.8(5) . . ?
O1 Nb1 O3 98.8(3) . . ?
O1 Nb1 O4 96.0(5) . . ?
O1 Nb1 O8 103.0(3) . 2_656 ?
O1 Nb1 N1 168.0(5) . . ?
O2 Nb1 O3 91.9(5) . . ?
O2 Nb1 O4 160.1(4) . . ?
O2 Nb1 O8 76.0(5) . 2_656 ?
O2 Nb1 N1 67.5(4) . . ?
O3 Nb1 O4 91.9(4) . . ?
O3 Nb1 O8 156.9(4) . 2_656 ?
O3 Nb1 N1 75.3(3) . . ?
O4 Nb1 O8 93.4(5) . 2_656 ?
O4 Nb1 N1 94.6(4) . . ?
O8 Nb1 N1 81.9(3) 2_656 . ?
O1 Nb2 O5 84.2(5) . . ?
O1 Nb2 N2 82.1(3) . . ?
O5 Nb2 N2 76.6(4) . . ?
O6 Nb2 O1 89.0(5) . . ?
O6 Nb2 O5 159.3(4) . . ?
O6 Nb2 O7 90.3(5) . . ?
O6 Nb2 O8 98.7(5) . . ?
O6 Nb2 N2 83.1(4) . . ?
O7 Nb2 O1 156.2(3) . . ?
O7 Nb2 O5 88.0(4) . . ?
O7 Nb2 N2 74.2(3) . . ?
O8 Nb2 O1 102.9(3) . . ?
O8 Nb2 O5 101.9(5) . . ?
O8 Nb2 O7 100.7(3) . . ?
O8 Nb2 N2 174.7(4) . . ?
Nb1 O1 Nb2 164.9(4) . . ?
C4 O2 Nb1 140.3(9) . . ?
C1 O3 Nb1 121.3(7) . . ?
C6 O4 Nb1 137.2(8) . . ?
C9 O5 Nb2 118.8(10) . . ?
C12 O6 Nb2 140.9(9) . . ?
C11 O7 Nb2 124.7(7) . . ?
Nb2 O8 Nb1 165.1(6) . 2_656 ?
C2 N1 Nb1 103.7(7) . . ?
C2 N1 C5 112.0(11) . . ?
C3 N1 Nb1 106.8(8) . . ?
C3 N1 C2 110.5(14) . . ?
C3 N1 C5 108.3(12) . . ?
C5 N1 Nb1 115.4(8) . . ?
C7 N2 Nb2 116.3(8) . . ?
C7 N2 C8 101.4(11) . . ?
C8 N2 Nb2 103.2(8) . . ?
C10 N2 Nb2 105.4(7) . . ?
C10 N2 C7 126.0(11) . . ?
C10 N2 C8 100.9(12) . . ?
O3 C1 H1A 110.2 . . ?
O3 C1 H1B 110.2 . . ?
O3 C1 C2 107.5(10) . . ?
H1A C1 H1B 108.5 . . ?
C2 C1 H1A 110.2 . . ?
C2 C1 H1B 110.2 . . ?
N1 C2 C1 116.6(11) . . ?
N1 C2 H2A 108.1 . . ?
N1 C2 H2B 108.1 . . ?
C1 C2 H2A 108.1 . . ?
C1 C2 H2B 108.1 . . ?
H2A C2 H2B 107.3 . . ?
N1 C3 H3A 108.1 . . ?
N1 C3 H3B 108.1 . . ?
N1 C3 C4 116.9(13) . . ?
H3A C3 H3B 107.3 . . ?
C4 C3 H3A 108.1 . . ?
C4 C3 H3B 108.1 . . ?
O2 C4 C3 103.5(12) . . ?
O2 C4 H4 128.2 . . ?
C3 C4 H4 128.2 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O4 C6 H6A 109.5 . . ?
O4 C6 H6B 109.5 . . ?
O4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 H8A 108.8 . . ?
N2 C8 H8B 108.8 . . ?
N2 C8 C9 113.9(13) . . ?
H8A C8 H8B 107.7 . . ?
C9 C8 H8A 108.8 . . ?
C9 C8 H8B 108.8 . . ?
O5 C9 C8 117.0(15) . . ?
O5 C9 H9A 108.0 . . ?
O5 C9 H9B 108.0 . . ?
C8 C9 H9A 108.0 . . ?
C8 C9 H9B 108.0 . . ?
H9A C9 H9B 107.3 . . ?
N2 C10 H10A 108.6 . . ?
N2 C10 H10B 108.6 . . ?
N2 C10 C11 114.6(11) . . ?
H10A C10 H10B 107.6 . . ?
C11 C10 H10A 108.6 . . ?
C11 C10 H10B 108.6 . . ?
O7 C11 C10 113.0(10) . . ?
O7 C11 H11A 109.0 . . ?
O7 C11 H11B 109.0 . . ?
C10 C11 H11A 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
O6 C12 H12A 109.5 . . ?
O6 C12 H12B 109.5 . . ?
O6 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 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
Nb1 O2 C4 C3 -7.9(19) . . . . ?
Nb1 O3 C1 C2 43.9(15) . . . . ?
Nb1 N1 C2 C1 21.9(14) . . . . ?
Nb1 N1 C3 C4 22(2) . . . . ?
Nb2 O5 C9 C8 4.2(19) . . . . ?
Nb2 O7 C11 C10 -20.2(19) . . . . ?
Nb2 N2 C8 C9 -32.7(15) . . . . ?
Nb2 N2 C10 C11 -27.5(16) . . . . ?
O1 Nb1 O2 C4 -171.2(12) . . . . ?
O1 Nb2 O6 C12 13.7(14) . . . . ?
O1 Nb2 O8 Nb1 43(3) . . . 2_656 ?
O2 Nb1 O1 Nb2 92(3) . . . . ?
O3 Nb1 O1 Nb2 -174(3) . . . . ?
O3 Nb1 O2 C4 89.3(12) . . . . ?
O3 C1 C2 N1 -41.0(17) . . . . ?
O4 Nb1 O1 Nb2 -81(3) . . . . ?
O4 Nb1 O2 C4 -11.5(18) . . . . ?
O5 Nb2 O6 C12 84.6(18) . . . . ?
O5 Nb2 O8 Nb1 -44(3) . . . 2_656 ?
O6 Nb2 O8 Nb1 134(3) . . . 2_656 ?
O7 Nb2 O6 C12 169.9(14) . . . . ?
O7 Nb2 O8 Nb1 -134(3) . . . 2_656 ?
O8 Nb1 O1 Nb2 14(3) 2_656 . . . ?
O8 Nb1 O2 C4 -70.8(12) 2_656 . . . ?
O8 Nb2 O6 C12 -89.2(14) . . . . ?
N1 Nb1 O1 Nb2 127(3) . . . . ?
N1 Nb1 O2 C4 16.1(12) . . . . ?
N1 C3 C4 O2 -14(2) . . . . ?
N2 Nb2 O6 C12 95.9(14) . . . . ?
N2 C8 C9 O5 23(2) . . . . ?
N2 C10 C11 O7 32(2) . . . . ?
C2 N1 C3 C4 -89.7(19) . . . . ?
C3 N1 C2 C1 136.0(13) . . . . ?
C5 N1 C2 C1 -103.1(15) . . . . ?
C5 N1 C3 C4 147.3(17) . . . . ?
C7 N2 C8 C9 -153.4(14) . . . . ?
C7 N2 C10 C11 112.6(16) . . . . ?
C8 N2 C10 C11 -134.5(14) . . . . ?
C10 N2 C8 C9 76.2(16) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.391 0.119 0.500 296.1 21.6 ?
2 -0.522 0.619 0.000 296.1 21.6 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2

_olex2_date_sample_data_collection 2020-09-24
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id SMR-b-XXX
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.375
_oxdiff_exptl_absorpt_empirical_full_min 0.812
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.51(13)
2 0.49(13)

