# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_mo_jvr171212P1_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1821182'
_audit_update_record             
;
2018-02-01 deposited with the CCDC.
2018-05-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C76 H62 N4 P2'
_chemical_formula_sum            'C76 H62 N4 P2'
_chemical_formula_weight         1093.23

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   13.406(4)
_cell_length_b                   29.170(9)
_cell_length_c                   14.794(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.859(11)
_cell_angle_gamma                90
_cell_volume                     5765(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    165289
_cell_measurement_theta_min      2.089
_cell_measurement_theta_max      27.572

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_F_000             2304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.234
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5646
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_absorpt_special_details   
;
The ratio of minimum to maximum
apparent transmission was 0.757
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            163760
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.089
_diffrn_reflns_theta_max         27.572
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             13307
_reflns_number_gt                11729
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0534P)²+2.5458P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13307
_refine_ls_number_parameters     739
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.1082
_refine_ls_wR_factor_gt          0.1041
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.23126(2) 0.63920(2) 0.23395(2) 0.01437(7) Uani 1 1 d . U . . .
C1 C 0.27175(9) 0.55653(4) 0.13538(8) 0.0189(2) Uani 1 1 d . . . . .
N1 N 0.27993(8) 0.58654(4) 0.21666(7) 0.0189(2) Uani 1 1 d . U . . .
H1 H 0.3161 0.5751 0.2638 0.023 Uiso 1 1 calc . U . . .
P2 P 0.25226(2) 0.65920(2) 0.40817(2) 0.01459(7) Uani 1 1 d . . . . .
N2 N 0.31922(8) 0.61834(4) 0.46747(7) 0.0183(2) Uani 1 1 d . . . . .
H2 H 0.3559 0.6009 0.4348 0.022 Uiso 1 1 calc . U . . .
C2 C 0.19246(10) 0.51877(4) 0.14509(9) 0.0205(3) Uani 1 1 d . . . . .
N3 N 0.16318(7) 0.63254(3) 0.32978(7) 0.01497(19) Uani 1 1 d . . . . .
C3 C 0.17177(11) 0.50314(5) 0.23038(10) 0.0250(3) Uani 1 1 d . . . . .
H3 H 0.2053 0.5167 0.2829 0.030 Uiso 1 1 calc R U . . .
N4 N 0.31986(7) 0.66249(3) 0.31378(7) 0.0156(2) Uani 1 1 d . . . . .
C4 C 0.10312(12) 0.46813(5) 0.24037(11) 0.0319(3) Uani 1 1 d . . . . .
H4 H 0.0890 0.4585 0.2993 0.038 Uiso 1 1 calc R U . . .
C8 C 0.24425(10) 0.58529(4) 0.04948(9) 0.0211(3) Uani 1 1 d . . . . .
C7 C 0.14407(11) 0.49734(5) 0.06944(10) 0.0278(3) Uani 1 1 d . . . . .
H7 H 0.1572 0.5072 0.0104 0.033 Uiso 1 1 calc R U . . .
C6 C 0.07633(12) 0.46148(5) 0.07922(11) 0.0328(3) Uani 1 1 d . . . . .
H6 H 0.0448 0.4469 0.0270 0.039 Uiso 1 1 calc R U . . .
C5 C 0.05529(12) 0.44727(5) 0.16443(12) 0.0338(3) Uani 1 1 d . . . . .
H5 H 0.0084 0.4234 0.1711 0.041 Uiso 1 1 calc R U . . .
C9 C 0.15023(11) 0.60606(5) 0.03621(9) 0.0261(3) Uani 1 1 d . . . . .
H9 H 0.1035 0.6022 0.0804 0.031 Uiso 1 1 calc R U . . .
C10 C 0.12418(13) 0.63216(6) -0.04028(11) 0.0342(3) Uani 1 1 d . . . . .
H10 H 0.0605 0.6466 -0.0473 0.041 Uiso 1 1 calc R U . . .
C11 C 0.19061(14) 0.63733(6) -0.10693(11) 0.0379(4) Uani 1 1 d . . . . .
H11 H 0.1725 0.6549 -0.1599 0.045 Uiso 1 1 calc R U . . .
C12 C 0.28285(14) 0.61664(6) -0.09494(10) 0.0375(4) Uani 1 1 d . . . . .
H12 H 0.3286 0.6198 -0.1402 0.045 Uiso 1 1 calc R U . . .
C13 C 0.31020(12) 0.59108(5) -0.01726(10) 0.0292(3) Uani 1 1 d . . . . .
H13 H 0.3747 0.5774 -0.0098 0.035 Uiso 1 1 calc R U . . .
C16 C 0.48311(14) 0.46831(6) 0.11575(14) 0.0453(4) Uani 1 1 d . . . . .
H16 H 0.4903 0.4366 0.1036 0.054 Uiso 1 1 calc R U . . .
C15 C 0.38766(12) 0.48728(5) 0.11510(11) 0.0340(3) Uani 1 1 d . . . . .
H15 H 0.3304 0.4684 0.1027 0.041 Uiso 1 1 calc R U . . .
C14 C 0.37563(10) 0.53364(5) 0.13243(9) 0.0232(3) Uani 1 1 d . . . . .
C17 C 0.56753(13) 0.49521(7) 0.13390(13) 0.0462(4) Uani 1 1 d . . . . .
H17 H 0.6324 0.4819 0.1358 0.055 Uiso 1 1 calc R U . . .
C18 C 0.55646(12) 0.54111(7) 0.14911(12) 0.0425(4) Uani 1 1 d . . . . .
H18 H 0.6140 0.5599 0.1605 0.051 Uiso 1 1 calc R U . . .
C19 C 0.46138(11) 0.56048(6) 0.14796(11) 0.0319(3) Uani 1 1 d . . . . .
H19 H 0.4549 0.5925 0.1579 0.038 Uiso 1 1 calc R U . . .
C20 C 0.06126(9) 0.65538(4) 0.32602(8) 0.0158(2) Uani 1 1 d . . . . .
C21 C 0.01792(9) 0.64653(4) 0.41770(8) 0.0170(2) Uani 1 1 d . . . . .
C22 C 0.03277(10) 0.60345(4) 0.45759(9) 0.0210(3) Uani 1 1 d . . . . .
H22 H 0.0721 0.5813 0.4296 0.025 Uiso 1 1 calc R U . . .
C23 C -0.00901(11) 0.59244(5) 0.53746(10) 0.0261(3) Uani 1 1 d . . . . .
H23 H 0.0023 0.5631 0.5641 0.031 Uiso 1 1 calc R U . . .
C24 C -0.06766(11) 0.62451(5) 0.57850(10) 0.0294(3) Uani 1 1 d . . . . .
H24 H -0.0956 0.6173 0.6337 0.035 Uiso 1 1 calc R U . . .
C28 C 0.10186(10) 0.73965(4) 0.36629(10) 0.0231(3) Uani 1 1 d . . . . .
H28 H 0.1068 0.7317 0.4288 0.028 Uiso 1 1 calc R U . . .
C27 C 0.07287(9) 0.70642(4) 0.30107(9) 0.0191(2) Uani 1 1 d . . . . .
C26 C -0.04322(10) 0.67763(5) 0.45816(9) 0.0217(3) Uani 1 1 d . . . . .
H26 H -0.0567 0.7067 0.4307 0.026 Uiso 1 1 calc R U . . .
C25 C -0.08480(11) 0.66670(5) 0.53841(10) 0.0278(3) Uani 1 1 d . . . . .
H25 H -0.1254 0.6885 0.5658 0.033 Uiso 1 1 calc R U . . .
C29 C 0.12361(11) 0.78424(5) 0.34085(12) 0.0308(3) Uani 1 1 d . . . . .
H29 H 0.1425 0.8064 0.3861 0.037 Uiso 1 1 calc R U . . .
C30 C 0.11794(12) 0.79647(5) 0.25048(13) 0.0361(4) Uani 1 1 d . . . . .
H30 H 0.1337 0.8268 0.2334 0.043 Uiso 1 1 calc R U . . .
C31 C 0.08913(12) 0.76413(5) 0.18482(11) 0.0332(3) Uani 1 1 d . . . . .
H31 H 0.0845 0.7724 0.1225 0.040 Uiso 1 1 calc R U . . .
C32 C 0.06693(10) 0.71950(5) 0.20978(10) 0.0248(3) Uani 1 1 d . . . . .
H32 H 0.0475 0.6976 0.1641 0.030 Uiso 1 1 calc R U . . .
C33 C -0.01426(9) 0.63145(4) 0.25742(8) 0.0182(2) Uani 1 1 d . . . . .
C34 C -0.10649(10) 0.65211(5) 0.23221(10) 0.0266(3) Uani 1 1 d . . . . .
H34 H -0.1203 0.6818 0.2546 0.032 Uiso 1 1 calc R U . . .
C35 C -0.17820(11) 0.62993(6) 0.17488(11) 0.0328(3) Uani 1 1 d . . . . .
H35 H -0.2405 0.6444 0.1583 0.039 Uiso 1 1 calc R U . . .
C36 C -0.15923(11) 0.58671(6) 0.14169(10) 0.0311(3) Uani 1 1 d . . . . .
H36 H -0.2079 0.5716 0.1017 0.037 Uiso 1 1 calc R U . . .
C37 C -0.06876(11) 0.56571(5) 0.16727(10) 0.0272(3) Uani 1 1 d . . . . .
H37 H -0.0554 0.5360 0.1451 0.033 Uiso 1 1 calc R U . . .
C38 C 0.00292(10) 0.58794(4) 0.22540(9) 0.0214(3) Uani 1 1 d . . . . .
H38 H 0.0644 0.5730 0.2432 0.026 Uiso 1 1 calc R U . . .
C39 C 0.32616(9) 0.60711(4) 0.56580(8) 0.0184(2) Uani 1 1 d . . . . .
C40 C 0.25689(10) 0.56677(4) 0.58503(9) 0.0211(3) Uani 1 1 d . . . . .
C41 C 0.22210(12) 0.56104(5) 0.67035(10) 0.0291(3) Uani 1 1 d . . . . .
H41 H 0.2340 0.5843 0.7148 0.035 Uiso 1 1 calc R U . . .
C42 C 0.17044(13) 0.52192(6) 0.69142(12) 0.0370(4) Uani 1 1 d . . . . .
H42 H 0.1477 0.5185 0.7501 0.044 Uiso 1 1 calc R U . . .
C43 C 0.15174(14) 0.48753(5) 0.62689(13) 0.0401(4) Uani 1 1 d . . . . .
H43 H 0.1162 0.4607 0.6410 0.048 Uiso 1 1 calc R U . . .
C44 C 0.18566(14) 0.49313(5) 0.54220(12) 0.0397(4) Uani 1 1 d . . . . .
H44 H 0.1736 0.4698 0.4977 0.048 Uiso 1 1 calc R U . . .
C45 C 0.23714(12) 0.53239(5) 0.52128(10) 0.0298(3) Uani 1 1 d . . . . .
H45 H 0.2593 0.5358 0.4623 0.036 Uiso 1 1 calc R U . . .
C46 C 0.29863(10) 0.64973(4) 0.62062(8) 0.0194(2) Uani 1 1 d . . . . .
C47 C 0.36701(11) 0.67252(5) 0.68033(9) 0.0252(3) Uani 1 1 d . . . . .
H47 H 0.4335 0.6612 0.6900 0.030 Uiso 1 1 calc R U . . .
C48 C 0.33993(12) 0.71157(5) 0.72634(10) 0.0324(3) Uani 1 1 d . . . . .
H48 H 0.3880 0.7266 0.7669 0.039 Uiso 1 1 calc R U . . .
C49 C 0.24356(13) 0.72859(5) 0.71339(11) 0.0332(3) Uani 1 1 d . . . . .
H49 H 0.2257 0.7558 0.7435 0.040 Uiso 1 1 calc R U . . .
C50 C 0.17332(12) 0.70570(5) 0.65634(10) 0.0303(3) Uani 1 1 d . . . . .
H50 H 0.1065 0.7168 0.6481 0.036 Uiso 1 1 calc R U . . .
C51 C 0.20045(10) 0.66639(5) 0.61102(9) 0.0239(3) Uani 1 1 d . . . . .
H51 H 0.1513 0.6506 0.5728 0.029 Uiso 1 1 calc R U . . .
C52 C 0.43609(10) 0.59189(5) 0.59019(9) 0.0229(3) Uani 1 1 d . . . . .
C53 C 0.51450(11) 0.61969(5) 0.56687(10) 0.0276(3) Uani 1 1 d . . . . .
H53 H 0.4998 0.6475 0.5350 0.033 Uiso 1 1 calc R U . . .
C54 C 0.61376(12) 0.60758(7) 0.58924(11) 0.0378(4) Uani 1 1 d . . . . .
H54 H 0.6658 0.6275 0.5740 0.045 Uiso 1 1 calc R U . . .
C55 C 0.63715(13) 0.56708(8) 0.63323(13) 0.0480(5) Uani 1 1 d . . . . .
H55 H 0.7050 0.5588 0.6485 0.058 Uiso 1 1 calc R U . . .
C56 C 0.56031(15) 0.53845(8) 0.65504(15) 0.0548(5) Uani 1 1 d . . . . .
H56 H 0.5758 0.5101 0.6844 0.066 Uiso 1 1 calc R U . . .
C57 C 0.46055(13) 0.55085(6) 0.63439(12) 0.0398(4) Uani 1 1 d . . . . .
H57 H 0.4088 0.5310 0.6507 0.048 Uiso 1 1 calc R U . . .
C58 C 0.40891(9) 0.69224(4) 0.30012(8) 0.0178(2) Uani 1 1 d . . . . .
C59 C 0.39577(9) 0.73895(4) 0.34710(9) 0.0208(3) Uani 1 1 d . . . . .
C60 C 0.38931(11) 0.78062(5) 0.30122(11) 0.0292(3) Uani 1 1 d . . . . .
H60 H 0.3946 0.7812 0.2376 0.035 Uiso 1 1 calc R U . . .
C61 C 0.37522(13) 0.82147(5) 0.34699(13) 0.0381(4) Uani 1 1 d . . . . .
H61 H 0.3706 0.8495 0.3143 0.046 Uiso 1 1 calc R U . . .
C62 C 0.36788(13) 0.82162(5) 0.43951(13) 0.0391(4) Uani 1 1 d . . . . .
H62 H 0.3566 0.8495 0.4703 0.047 Uiso 1 1 calc R U . . .
C63 C 0.37707(12) 0.78065(6) 0.48692(11) 0.0338(3) Uani 1 1 d . . . . .
H63 H 0.3730 0.7804 0.5507 0.041 Uiso 1 1 calc R U . . .
C64 C 0.39226(10) 0.73999(5) 0.44113(10) 0.0255(3) Uani 1 1 d . . . . .
H64 H 0.4004 0.7122 0.4746 0.031 Uiso 1 1 calc R U . . .
C65 C 0.50708(9) 0.66986(5) 0.33992(9) 0.0209(3) Uani 1 1 d . . . . .
C66 C 0.52056(10) 0.62271(5) 0.33713(9) 0.0245(3) Uani 1 1 d . . . . .
H66 H 0.4649 0.6036 0.3196 0.029 Uiso 1 1 calc R U . . .
C67 C 0.61395(11) 0.60291(5) 0.35944(11) 0.0315(3) Uani 1 1 d . . . . .
H67 H 0.6216 0.5706 0.3567 0.038 Uiso 1 1 calc R U . . .
C68 C 0.69595(11) 0.63035(6) 0.38573(11) 0.0345(3) Uani 1 1 d . . . . .
H68 H 0.7600 0.6171 0.4000 0.041 Uiso 1 1 calc R U . . .
C69 C 0.68311(11) 0.67722(6) 0.39081(11) 0.0345(3) Uani 1 1 d . . . . .
H69 H 0.7385 0.6962 0.4100 0.041 Uiso 1 1 calc R U . . .
C70 C 0.58989(10) 0.69703(5) 0.36812(10) 0.0285(3) Uani 1 1 d . . . . .
H70 H 0.5824 0.7293 0.3718 0.034 Uiso 1 1 calc R U . . .
C71 C 0.41449(10) 0.69763(4) 0.19669(9) 0.0228(3) Uani 1 1 d . . . . .
C72 C 0.33142(12) 0.71421(5) 0.14314(10) 0.0281(3) Uani 1 1 d . . . . .
H72 H 0.2738 0.7239 0.1711 0.034 Uiso 1 1 calc R U . . .
C73 C 0.33236(15) 0.71664(6) 0.04923(11) 0.0397(4) Uani 1 1 d . . . . .
H73 H 0.2748 0.7272 0.0133 0.048 Uiso 1 1 calc R U . . .
C74 C 0.41675(17) 0.70378(6) 0.00814(11) 0.0464(5) Uani 1 1 d . . . . .
H74 H 0.4169 0.7051 -0.0560 0.056 Uiso 1 1 calc R U . . .
C75 C 0.50055(16) 0.68908(6) 0.06019(12) 0.0445(4) Uani 1 1 d . . . . .
H75 H 0.5593 0.6812 0.0320 0.053 Uiso 1 1 calc R U . . .
C76 C 0.49972(12) 0.68566(5) 0.15416(10) 0.0322(3) Uani 1 1 d . . . . .
H76 H 0.5577 0.6751 0.1895 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
P1 N1 1.6966(12) . ?
P1 N4 1.7404(11) . ?
P1 N3 1.7605(11) . ?
P1 P2 2.6343(8) . ?
C1 N1 1.4839(16) . ?
C1 C8 1.5412(18) . ?
C1 C2 1.5459(18) . ?
C1 C14 1.5485(18) . ?
N1 H1 0.8800 . ?
P2 N2 1.6920(11) . ?
P2 N4 1.7305(11) . ?
P2 N3 1.7724(11) . ?
N2 C39 1.4863(16) . ?
N2 H2 0.8800 . ?
C2 C3 1.3914(19) . ?
C2 C7 1.3932(19) . ?
N3 C20 1.5169(15) . ?
C3 C4 1.391(2) . ?
C3 H3 0.9500 . ?
N4 C58 1.5035(15) . ?
C4 C5 1.386(2) . ?
C4 H4 0.9500 . ?
C8 C13 1.3903(19) . ?
C8 C9 1.397(2) . ?
C7 C6 1.401(2) . ?
C7 H7 0.9500 . ?
C6 C5 1.379(2) . ?
C6 H6 0.9500 . ?
C5 H5 0.9500 . ?
C9 C10 1.384(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.392(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.374(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.393(2) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C16 C17 1.385(3) . ?
C16 C15 1.393(2) . ?
C16 H16 0.9500 . ?
C15 C14 1.388(2) . ?
C15 H15 0.9500 . ?
C14 C19 1.394(2) . ?
C17 C18 1.368(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.393(2) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C33 1.5389(17) . ?
C20 C21 1.5418(17) . ?
C20 C27 1.5451(17) . ?
C21 C26 1.3915(18) . ?
C21 C22 1.3952(18) . ?
C22 C23 1.3874(19) . ?
C22 H22 0.9500 . ?
C23 C24 1.394(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.377(2) . ?
C24 H24 0.9500 . ?
C28 C29 1.3916(19) . ?
C28 C27 1.3993(19) . ?
C28 H28 0.9500 . ?
C27 C32 1.3991(19) . ?
C26 C25 1.3907(19) . ?
C26 H26 0.9500 . ?
C25 H25 0.9500 . ?
C29 C30 1.380(2) . ?
C29 H29 0.9500 . ?
C30 C31 1.385(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.392(2) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.3808(18) . ?
C33 C34 1.3976(18) . ?
C34 C35 1.387(2) . ?
C34 H34 0.9500 . ?
C35 C36 1.384(2) . ?
C35 H35 0.9500 . ?
C36 C37 1.383(2) . ?
C36 H36 0.9500 . ?
C37 C38 1.3940(19) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.5403(18) . ?
C39 C46 1.5461(18) . ?
C39 C52 1.5522(18) . ?
C40 C45 1.387(2) . ?
C40 C41 1.3923(19) . ?
C41 C42 1.384(2) . ?
C41 H41 0.9500 . ?
C42 C43 1.393(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.378(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.385(2) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.3876(19) . ?
C46 C51 1.3990(19) . ?
C47 C48 1.391(2) . ?
C47 H47 0.9500 . ?
C48 C49 1.382(2) . ?
C48 H48 0.9500 . ?
C49 C50 1.382(2) . ?
C49 H49 0.9500 . ?
C50 C51 1.392(2) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 C57 1.390(2) . ?
C52 C53 1.394(2) . ?
C53 C54 1.389(2) . ?
C53 H53 0.9500 . ?
C54 C55 1.372(3) . ?
C54 H54 0.9500 . ?
C55 C56 1.385(3) . ?
C55 H55 0.9500 . ?
C56 C57 1.394(2) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
C58 C65 1.5408(18) . ?
C58 C59 1.5462(18) . ?
C58 C71 1.5462(18) . ?
C59 C60 1.3914(19) . ?
C59 C64 1.3963(19) . ?
C60 C61 1.391(2) . ?
C60 H60 0.9500 . ?
C61 C62 1.381(3) . ?
C61 H61 0.9500 . ?
C62 C63 1.386(2) . ?
C62 H62 0.9500 . ?
C63 C64 1.389(2) . ?
C63 H63 0.9500 . ?
C64 H64 0.9500 . ?
C65 C66 1.388(2) . ?
C65 C70 1.3987(19) . ?
C66 C67 1.393(2) . ?
C66 H66 0.9500 . ?
C67 C68 1.389(2) . ?
C67 H67 0.9500 . ?
C68 C69 1.381(2) . ?
C68 H68 0.9500 . ?
C69 C70 1.392(2) . ?
C69 H69 0.9500 . ?
C70 H70 0.9500 . ?
C71 C76 1.395(2) . ?
C71 C72 1.397(2) . ?
C72 C73 1.392(2) . ?
C72 H72 0.9500 . ?
C73 C74 1.381(3) . ?
C73 H73 0.9500 . ?
C74 C75 1.376(3) . ?
C74 H74 0.9500 . ?
C75 C76 1.395(2) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 N4 101.92(5) . . ?
N1 P1 N3 104.70(5) . . ?
N4 P1 N3 82.37(5) . . ?
N1 P1 P2 109.72(4) . . ?
N4 P1 P2 40.49(3) . . ?
N3 P1 P2 41.96(4) . . ?
N1 C1 C8 110.06(10) . . ?
N1 C1 C2 110.45(10) . . ?
C8 C1 C2 110.25(10) . . ?
N1 C1 C14 105.81(10) . . ?
C8 C1 C14 111.37(10) . . ?
C2 C1 C14 108.81(11) . . ?
C1 N1 P1 130.79(9) . . ?
C1 N1 H1 114.6 . . ?
P1 N1 H1 114.6 . . ?
N2 P2 N4 99.57(5) . . ?
N2 P2 N3 109.18(5) . . ?
N4 P2 N3 82.31(5) . . ?
N2 P2 P1 111.05(4) . . ?
N4 P2 P1 40.77(4) . . ?
N3 P2 P1 41.61(3) . . ?
C39 N2 P2 130.48(8) . . ?
C39 N2 H2 114.8 . . ?
P2 N2 H2 114.8 . . ?
C3 C2 C7 117.80(13) . . ?
C3 C2 C1 120.61(12) . . ?
C7 C2 C1 121.47(12) . . ?
C20 N3 P1 116.68(8) . . ?
C20 N3 P2 112.72(8) . . ?
P1 N3 P2 96.43(5) . . ?
C4 C3 C2 121.43(14) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C58 N4 P2 128.06(8) . . ?
C58 N4 P1 129.66(8) . . ?
P2 N4 P1 98.74(5) . . ?
C5 C4 C3 120.06(14) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C13 C8 C9 117.90(13) . . ?
C13 C8 C1 121.97(12) . . ?
C9 C8 C1 120.12(12) . . ?
C2 C7 C6 120.92(14) . . ?
C2 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C5 C6 C7 120.24(14) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C6 C5 C4 119.52(14) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C10 C9 C8 121.03(14) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C9 C10 C11 120.44(15) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C12 C11 C10 118.95(14) . . ?
C12 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
C11 C12 C13 120.85(15) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C8 C13 C12 120.81(15) . . ?
C8 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C17 C16 C15 120.75(16) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C14 C15 C16 120.43(16) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C14 C19 118.08(13) . . ?
C15 C14 C1 122.96(13) . . ?
C19 C14 C1 118.96(12) . . ?
C18 C17 C16 119.23(15) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C19 120.46(16) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C14 121.00(15) . . ?
C18 C19 H19 119.5 . . ?
C14 C19 H19 119.5 . . ?
N3 C20 C33 111.42(10) . . ?
N3 C20 C21 107.44(9) . . ?
C33 C20 C21 103.20(9) . . ?
N3 C20 C27 108.86(9) . . ?
C33 C20 C27 110.70(10) . . ?
C21 C20 C27 115.13(10) . . ?
C26 C21 C22 118.26(12) . . ?
C26 C21 C20 123.28(11) . . ?
C22 C21 C20 118.16(11) . . ?
C23 C22 C21 121.01(12) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C22 C23 C24 119.93(13) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 119.46(13) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C29 C28 C27 120.88(14) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C32 C27 C28 117.80(12) . . ?
C32 C27 C20 119.65(12) . . ?
C28 C27 C20 122.05(11) . . ?
C25 C26 C21 120.72(13) . . ?
C25 C26 H26 119.6 . . ?
C21 C26 H26 119.6 . . ?
C24 C25 C26 120.55(13) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C30 C29 C28 120.55(14) . . ?
C30 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
C29 C30 C31 119.50(14) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C30 C31 C32 120.26(14) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C31 C32 C27 121.00(14) . . ?
C31 C32 H32 119.5 . . ?
C27 C32 H32 119.5 . . ?
C38 C33 C34 118.32(12) . . ?
C38 C33 C20 121.57(11) . . ?
C34 C33 C20 119.87(12) . . ?
C35 C34 C33 120.90(14) . . ?
C35 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C36 C35 C34 120.21(14) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C37 C36 C35 119.31(13) . . ?
C37 C36 H36 120.3 . . ?
C35 C36 H36 120.3 . . ?
C36 C37 C38 120.37(14) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C33 C38 C37 120.85(13) . . ?
C33 C38 H38 119.6 . . ?
C37 C38 H38 119.6 . . ?
N2 C39 C40 111.12(10) . . ?
N2 C39 C46 109.77(10) . . ?
C40 C39 C46 110.06(10) . . ?
N2 C39 C52 105.67(10) . . ?
C40 C39 C52 108.30(10) . . ?
C46 C39 C52 111.85(10) . . ?
C45 C40 C41 118.05(13) . . ?
C45 C40 C39 120.68(12) . . ?
C41 C40 C39 120.85(12) . . ?
C42 C41 C40 121.04(14) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C41 C42 C43 120.26(15) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C44 C43 C42 118.92(14) . . ?
C44 C43 H43 120.5 . . ?
C42 C43 H43 120.5 . . ?
C43 C44 C45 120.66(15) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 H44 119.7 . . ?
C44 C45 C40 121.06(14) . . ?
C44 C45 H45 119.5 . . ?
C40 C45 H45 119.5 . . ?
C47 C46 C51 117.60(12) . . ?
C47 C46 C39 123.02(12) . . ?
C51 C46 C39 119.37(11) . . ?
C46 C47 C48 121.21(14) . . ?
C46 C47 H47 119.4 . . ?
C48 C47 H47 119.4 . . ?
C49 C48 C47 120.40(14) . . ?
C49 C48 H48 119.8 . . ?
C47 C48 H48 119.8 . . ?
C50 C49 C48 119.45(14) . . ?
C50 C49 H49 120.3 . . ?
C48 C49 H49 120.3 . . ?
C49 C50 C51 119.98(14) . . ?
C49 C50 H50 120.0 . . ?
C51 C50 H50 120.0 . . ?
C50 C51 C46 121.28(13) . . ?
C50 C51 H51 119.4 . . ?
C46 C51 H51 119.4 . . ?
C57 C52 C53 117.70(14) . . ?
C57 C52 C39 122.50(13) . . ?
C53 C52 C39 119.80(12) . . ?
C54 C53 C52 121.34(15) . . ?
C54 C53 H53 119.3 . . ?
C52 C53 H53 119.3 . . ?
C55 C54 C53 120.51(17) . . ?
C55 C54 H54 119.7 . . ?
C53 C54 H54 119.7 . . ?
C54 C55 C56 119.00(16) . . ?
C54 C55 H55 120.5 . . ?
C56 C55 H55 120.5 . . ?
C55 C56 C57 120.73(17) . . ?
C55 C56 H56 119.6 . . ?
C57 C56 H56 119.6 . . ?
C52 C57 C56 120.68(17) . . ?
C52 C57 H57 119.7 . . ?
C56 C57 H57 119.7 . . ?
N4 C58 C65 111.48(10) . . ?
N4 C58 C59 109.05(10) . . ?
C65 C58 C59 109.13(10) . . ?
N4 C58 C71 107.29(10) . . ?
C65 C58 C71 108.05(10) . . ?
C59 C58 C71 111.85(10) . . ?
C60 C59 C64 117.46(13) . . ?
C60 C59 C58 123.73(12) . . ?
C64 C59 C58 118.80(12) . . ?
C61 C60 C59 121.08(15) . . ?
C61 C60 H60 119.5 . . ?
C59 C60 H60 119.5 . . ?
C62 C61 C60 120.61(15) . . ?
C62 C61 H61 119.7 . . ?
C60 C61 H61 119.7 . . ?
C61 C62 C63 119.23(14) . . ?
C61 C62 H62 120.4 . . ?
C63 C62 H62 120.4 . . ?
C62 C63 C64 119.99(15) . . ?
C62 C63 H63 120.0 . . ?
C64 C63 H63 120.0 . . ?
C63 C64 C59 121.53(14) . . ?
C63 C64 H64 119.2 . . ?
C59 C64 H64 119.2 . . ?
C66 C65 C70 117.92(13) . . ?
C66 C65 C58 121.18(11) . . ?
C70 C65 C58 120.30(12) . . ?
C65 C66 C67 121.37(13) . . ?
C65 C66 H66 119.3 . . ?
C67 C66 H66 119.3 . . ?
C68 C67 C66 120.11(15) . . ?
C68 C67 H67 119.9 . . ?
C66 C67 H67 119.9 . . ?
C69 C68 C67 119.12(14) . . ?
C69 C68 H68 120.4 . . ?
C67 C68 H68 120.4 . . ?
C68 C69 C70 120.76(14) . . ?
C68 C69 H69 119.6 . . ?
C70 C69 H69 119.6 . . ?
C69 C70 C65 120.70(14) . . ?
C69 C70 H70 119.7 . . ?
C65 C70 H70 119.7 . . ?
C76 C71 C72 118.36(13) . . ?
C76 C71 C58 122.08(13) . . ?
C72 C71 C58 119.55(12) . . ?
C73 C72 C71 120.61(16) . . ?
C73 C72 H72 119.7 . . ?
C71 C72 H72 119.7 . . ?
C74 C73 C72 120.16(17) . . ?
C74 C73 H73 119.9 . . ?
C72 C73 H73 119.9 . . ?
C75 C74 C73 119.93(15) . . ?
C75 C74 H74 120.0 . . ?
C73 C74 H74 120.0 . . ?
C74 C75 C76 120.34(17) . . ?
C74 C75 H75 119.8 . . ?
C76 C75 H75 119.8 . . ?
C75 C76 C71 120.52(17) . . ?
C75 C76 H76 119.7 . . ?
C71 C76 H76 119.7 . . ?

_refine_diff_density_max         0.646
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.060
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1821183'
_audit_update_record             
;
2018-02-01 deposited with the CCDC.
2018-05-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H54 Li6 N6 P2, C6 H6'
_chemical_formula_sum            'C30 H60 Li6 N6 P2'
_chemical_formula_weight         608.42

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.6711(6)
_cell_length_b                   9.9510(4)
_cell_length_c                   10.2311(7)
_cell_angle_alpha                106.972(5)
_cell_angle_beta                 90.419(6)
_cell_angle_gamma                93.980(5)
_cell_volume                     939.07(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    18894
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             330
_exptl_absorpt_coefficient_mu    0.142
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.288
0 -1 0 0.246
0 0 -1 0.119
0 0 1 0.147
1 0 0 0.169
-1 0 0 0.104
0 -1 1 0.220
0 1 -1 0.213
-1 -1 0 0.217


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18804
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4283
_reflns_number_gt                3779
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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 > 2sigma(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)+(0.0420P)²+0.3683P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4283
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0968
_refine_ls_wR_factor_gt          0.0872
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.11765(3) 0.66778(3) 0.66307(3) 0.01703(9) Uani 1 1 d . . .
N1 N -0.06206(10) 0.66745(10) 0.65984(10) 0.0211(2) Uani 1 1 d . . .
N2 N 0.13702(11) 0.49289(10) 0.65743(11) 0.0218(2) Uani 1 1 d . . .
N3 N 0.15096(11) 0.66005(11) 0.49382(10) 0.0215(2) Uani 1 1 d . . .
C5 C 0.23331(14) 0.46829(13) 0.76001(13) 0.0252(3) Uani 1 1 d . . .
C9 C 0.25177(13) 0.76900(13) 0.47023(13) 0.0252(3) Uani 1 1 d . . .
C1 C -0.12756(12) 0.77545(13) 0.76850(12) 0.0222(2) Uani 1 1 d . . .
C10 C 0.39731(14) 0.76363(16) 0.52762(16) 0.0354(3) Uani 1 1 d . . .
H10A H 0.3944 0.7831 0.6251 0.043 Uiso 1 1 d R . .
H10B H 0.4596 0.8328 0.5056 0.043 Uiso 1 1 d R . .
H10C H 0.4292 0.6716 0.4882 0.043 Uiso 1 1 d R . .
C6 C 0.18962(16) 0.53331(16) 0.90693(14) 0.0330(3) Uani 1 1 d . . .
H6A H 0.1857 0.6331 0.9246 0.040 Uiso 1 1 d R . .
H6B H 0.2560 0.5153 0.9689 0.040 Uiso 1 1 d R . .
H6C H 0.0999 0.4921 0.9196 0.040 Uiso 1 1 d R . .
C12 C 0.20725(16) 0.91878(15) 0.53119(16) 0.0354(3) Uani 1 1 d . . .
H12A H 0.1177 0.9261 0.4938 0.042 Uiso 1 1 d R . .
H12B H 0.2736 0.9848 0.5094 0.042 Uiso 1 1 d R . .
H12C H 0.2025 0.9393 0.6287 0.042 Uiso 1 1 d R . .
C14 C 0.61886(15) 0.06903(16) 0.07092(15) 0.0358(3) Uani 1 1 d . . .
H14 H 0.6990 0.1155 0.1187 0.043 Uiso 1 1 d R . .
C11 C 0.26003(19) 0.74012(18) 0.31562(15) 0.0432(4) Uani 1 1 d . . .
H11A H 0.2925 0.6484 0.2760 0.052 Uiso 1 1 d R . .
H11B H 0.3230 0.8100 0.2957 0.052 Uiso 1 1 d R . .
H11C H 0.1696 0.7437 0.2779 0.052 Uiso 1 1 d R . .
C13 C 0.56424(18) 0.11291(16) -0.03257(15) 0.0400(4) Uani 1 1 d . . .
H13 H 0.6072 0.1895 -0.0549 0.048 Uiso 1 1 d R . .
C8 C 0.38243(14) 0.52390(17) 0.74801(16) 0.0349(3) Uani 1 1 d . . .
H8A H 0.4142 0.4799 0.6580 0.042 Uiso 1 1 d R . .
H8B H 0.4407 0.5026 0.8146 0.042 Uiso 1 1 d R . .
H8C H 0.3862 0.6241 0.7639 0.042 Uiso 1 1 d R . .
Li1 Li -0.0651(2) 0.4768(2) 0.6850(2) 0.0270(4) Uani 1 1 d . . .
C15 C 0.55431(18) -0.04362(16) 0.10358(15) 0.0392(4) Uani 1 1 d . . .
H15 H 0.5907 -0.0736 0.1738 0.047 Uiso 1 1 d R . .
C3 C -0.28302(16) 0.7535(2) 0.7368(2) 0.0555(5) Uani 1 1 d . . .
H3A H -0.3019 0.7674 0.6496 0.067 Uiso 1 1 d R . .
H3B H -0.3300 0.8199 0.8064 0.067 Uiso 1 1 d R . .
H3C H -0.3152 0.6594 0.7347 0.067 Uiso 1 1 d R . .
Li2 Li 0.2074(2) 0.4668(2) 0.4703(2) 0.0266(4) Uani 1 1 d . . .
C2 C -0.08070(19) 0.92578(15) 0.77234(19) 0.0445(4) Uani 1 1 d . . .
H2A H 0.0172 0.9425 0.7925 0.053 Uiso 1 1 d R . .
H2B H -0.1295 0.9902 0.8420 0.053 Uiso 1 1 d R . .
H2C H -0.1005 0.9396 0.6853 0.053 Uiso 1 1 d R . .
C4 C -0.1014(2) 0.7618(2) 0.91057(16) 0.0491(5) Uani 1 1 d . . .
H4A H -0.1304 0.6679 0.9116 0.059 Uiso 1 1 d R . .
H4B H -0.1532 0.8281 0.9754 0.059 Uiso 1 1 d R . .
H4C H -0.0043 0.7809 0.9345 0.059 Uiso 1 1 d R . .
C7 C 0.2305(2) 0.30818(16) 0.73309(19) 0.0462(4) Uani 1 1 d . . .
H7A H 0.1376 0.2715 0.7413 0.055 Uiso 1 1 d R . .
H7B H 0.2905 0.2873 0.7986 0.055 Uiso 1 1 d R . .
H7C H 0.2616 0.2656 0.6425 0.055 Uiso 1 1 d R . .
Li3 Li -0.0484(2) 0.6906(2) 0.4751(2) 0.0266(4) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N1 1.7379(10) . ?
P1 N3 1.7441(10) . ?
P1 N2 1.7475(10) . ?
P1 Li1 2.564(2) . ?
P1 Li3 2.567(2) . ?
P1 Li2 2.570(2) . ?
N1 C1 1.4830(14) . ?
N1 Li3 1.974(2) . ?
N1 Li1 1.986(2) . ?
N1 Li2 2.051(2) 2_566 ?
N2 C5 1.4818(15) . ?
N2 Li1 1.979(2) . ?
N2 Li2 1.987(2) . ?
N2 Li3 2.056(2) 2_566 ?
N3 C9 1.4810(15) . ?
N3 Li2 1.983(2) . ?
N3 Li3 1.989(2) . ?
N3 Li1 2.064(2) 2_566 ?
C5 C8 1.5273(19) . ?
C5 C6 1.5283(19) . ?
C5 C7 1.5339(19) . ?
C9 C11 1.5267(19) . ?
C9 C10 1.532(2) . ?
C9 C12 1.5317(19) . ?
C1 C4 1.5197(19) . ?
C1 C2 1.5219(19) . ?
C1 C3 1.5230(19) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9601 . ?
C6 H6C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C14 C15 1.372(2) . ?
C14 C13 1.373(2) . ?
C14 H14 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9601 . ?
C11 H11C 0.9600 . ?
C13 C15 1.380(2) 2_655 ?
C13 H13 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9601 . ?
C8 H8C 0.9600 . ?
Li1 N3 2.064(2) 2_566 ?
Li1 Li2 2.309(3) 2_566 ?
Li1 Li3 2.313(3) 2_566 ?
Li1 C11 2.764(3) 2_566 ?
Li1 Li2 3.431(3) . ?
Li1 Li3 3.434(3) . ?
C15 C13 1.380(2) 2_655 ?
C15 H15 0.9300 . ?
C3 H3A 0.9601 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
Li2 N1 2.051(2) 2_566 ?
Li2 Li3 2.306(3) 2_566 ?
Li2 Li1 2.309(3) 2_566 ?
Li2 C3 2.713(3) 2_566 ?
Li2 Li3 3.433(3) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9599 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9599 . ?
C7 H7C 0.9600 . ?
Li3 N2 2.056(2) 2_566 ?
Li3 Li2 2.306(3) 2_566 ?
Li3 Li1 2.313(3) 2_566 ?
Li3 C7 2.757(3) 2_566 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 N3 100.19(5) . . ?
N1 P1 N2 100.35(5) . . ?
N3 P1 N2 100.29(5) . . ?
N1 P1 Li1 50.66(6) . . ?
N3 P1 Li1 113.15(6) . . ?
N2 P1 Li1 50.41(6) . . ?
N1 P1 Li3 50.19(6) . . ?
N3 P1 Li3 50.67(6) . . ?
N2 P1 Li3 113.00(6) . . ?
Li1 P1 Li3 84.02(7) . . ?
N1 P1 Li2 112.70(6) . . ?
N3 P1 Li2 50.40(6) . . ?
N2 P1 Li2 50.52(6) . . ?
Li1 P1 Li2 83.87(7) . . ?
Li3 P1 Li2 83.86(7) . . ?
C1 N1 P1 118.14(8) . . ?
C1 N1 Li3 119.22(10) . . ?
P1 N1 Li3 87.26(8) . . ?
C1 N1 Li1 115.73(10) . . ?
P1 N1 Li1 86.76(8) . . ?
Li3 N1 Li1 120.25(10) . . ?
C1 N1 Li2 111.68(9) . 2_566 ?
P1 N1 Li2 130.14(8) . 2_566 ?
Li3 N1 Li2 69.87(10) . 2_566 ?
Li1 N1 Li2 69.76(10) . 2_566 ?
C5 N2 P1 117.19(8) . . ?
C5 N2 Li1 119.07(10) . . ?
P1 N2 Li1 86.72(8) . . ?
C5 N2 Li2 116.92(10) . . ?
P1 N2 Li2 86.73(8) . . ?
Li1 N2 Li2 119.79(10) . . ?
C5 N2 Li3 113.04(10) . 2_566 ?
P1 N2 Li3 129.75(8) . 2_566 ?
Li1 N2 Li3 69.92(10) . 2_566 ?
Li2 N2 Li3 69.52(10) . 2_566 ?
C9 N3 P1 117.31(8) . . ?
C9 N3 Li2 119.88(10) . . ?
P1 N3 Li2 86.94(8) . . ?
C9 N3 Li3 116.17(10) . . ?
P1 N3 Li3 86.62(8) . . ?
Li2 N3 Li3 119.59(10) . . ?
C9 N3 Li1 113.01(10) . 2_566 ?
P1 N3 Li1 129.64(8) . 2_566 ?
Li2 N3 Li1 69.56(10) . 2_566 ?
Li3 N3 Li1 69.57(10) . 2_566 ?
N2 C5 C8 112.85(11) . . ?
N2 C5 C6 112.84(11) . . ?
C8 C5 C6 107.97(11) . . ?
N2 C5 C7 106.57(11) . . ?
C8 C5 C7 108.33(12) . . ?
C6 C5 C7 108.09(12) . . ?
N3 C9 C11 106.80(10) . . ?
N3 C9 C10 112.80(11) . . ?
C11 C9 C10 108.24(12) . . ?
N3 C9 C12 112.81(11) . . ?
C11 C9 C12 108.21(12) . . ?
C10 C9 C12 107.80(11) . . ?
N1 C1 C4 112.92(11) . . ?
N1 C1 C2 113.37(11) . . ?
C4 C1 C2 107.38(13) . . ?
N1 C1 C3 106.53(10) . . ?
C4 C1 C3 108.57(14) . . ?
C2 C1 C3 107.90(13) . . ?
C9 C10 H10A 109.4 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C5 C6 H6A 109.6 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.4 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C15 C14 C13 119.53(14) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.4 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C13 C15 120.15(15) . 2_655 ?
C14 C13 H13 120.0 . . ?
C15 C13 H13 119.9 2_655 . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.4 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 Li1 N1 84.91(9) . . ?
N2 Li1 N3 106.10(11) . 2_566 ?
N1 Li1 N3 105.77(11) . 2_566 ?
N2 Li1 Li2 116.94(12) . 2_566 ?
N1 Li1 Li2 56.44(9) . 2_566 ?
N3 Li1 Li2 53.58(8) 2_566 2_566 ?
N2 Li1 Li3 56.60(9) . 2_566 ?
N1 Li1 Li3 116.67(12) . 2_566 ?
N3 Li1 Li3 53.70(8) 2_566 2_566 ?
Li2 Li1 Li3 95.92(11) 2_566 2_566 ?
N2 Li1 P1 42.87(5) . . ?
N1 Li1 P1 42.58(5) . . ?
N3 Li1 P1 117.20(10) 2_566 . ?
Li2 Li1 P1 89.58(9) 2_566 . ?
Li3 Li1 P1 89.76(9) 2_566 . ?
N2 Li1 C11 135.43(12) . 2_566 ?
N1 Li1 C11 137.66(12) . 2_566 ?
N3 Li1 C11 57.87(7) 2_566 2_566 ?
Li2 Li1 C11 87.87(10) 2_566 2_566 ?
Li3 Li1 C11 86.19(10) 2_566 2_566 ?
P1 Li1 C11 174.96(10) . 2_566 ?
N2 Li1 Li2 30.17(6) . . ?
N1 Li1 Li2 78.81(8) . . ?
N3 Li1 Li2 79.37(8) 2_566 . ?
Li2 Li1 Li2 89.85(9) 2_566 . ?
Li3 Li1 Li2 41.94(8) 2_566 . ?
P1 Li1 Li2 48.14(5) . . ?
C11 Li1 Li2 127.48(9) 2_566 . ?
N2 Li1 Li3 79.14(8) . . ?
N1 Li1 Li3 29.78(6) . . ?
N3 Li1 Li3 79.35(8) 2_566 . ?
Li2 Li1 Li3 41.88(8) 2_566 . ?
Li3 Li1 Li3 89.98(9) 2_566 . ?
P1 Li1 Li3 48.03(5) . . ?
C11 Li1 Li3 128.88(9) 2_566 . ?
Li2 Li1 Li3 60.00(7) . . ?
C14 C15 C13 120.32(14) . 2_655 ?
C14 C15 H15 119.9 . . ?
C13 C15 H15 119.8 2_655 . ?
C1 C3 H3A 109.6 . . ?
C1 C3 H3B 109.3 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.4 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N3 Li2 N2 84.94(9) . . ?
N3 Li2 N1 106.38(11) . 2_566 ?
N2 Li2 N1 105.92(11) . 2_566 ?
N3 Li2 Li3 117.22(11) . 2_566 ?
N2 Li2 Li3 56.65(9) . 2_566 ?
N1 Li2 Li3 53.50(8) 2_566 2_566 ?
N3 Li2 Li1 56.86(9) . 2_566 ?
N2 Li2 Li1 117.12(11) . 2_566 ?
N1 Li2 Li1 53.81(8) 2_566 2_566 ?
Li3 Li2 Li1 96.17(11) 2_566 2_566 ?
N3 Li2 P1 42.66(5) . . ?
N2 Li2 P1 42.75(5) . . ?
N1 Li2 P1 117.15(9) 2_566 . ?
Li3 Li2 P1 89.77(9) 2_566 . ?
Li1 Li2 P1 89.79(9) 2_566 . ?
N3 Li2 C3 137.56(12) . 2_566 ?
N2 Li2 C3 135.96(12) . 2_566 ?
N1 Li2 C3 58.80(7) 2_566 2_566 ?
Li3 Li2 C3 86.96(10) 2_566 2_566 ?
Li1 Li2 C3 88.07(10) 2_566 2_566 ?
P1 Li2 C3 175.89(10) . 2_566 ?
N3 Li2 Li1 79.11(8) . . ?
N2 Li2 Li1 30.04(6) . . ?
N1 Li2 Li1 79.34(8) 2_566 . ?
Li3 Li2 Li1 42.10(7) 2_566 . ?
Li1 Li2 Li1 90.15(9) 2_566 . ?
P1 Li2 Li1 47.99(5) . . ?
C3 Li2 Li1 128.47(9) 2_566 . ?
N3 Li2 Li3 30.25(6) . . ?
N2 Li2 Li3 79.09(8) . . ?
N1 Li2 Li3 79.48(8) 2_566 . ?
Li3 Li2 Li3 90.14(9) 2_566 . ?
Li1 Li2 Li3 42.08(8) 2_566 . ?
P1 Li2 Li3 48.03(5) . . ?
C3 Li2 Li3 129.41(10) 2_566 . ?
Li1 Li2 Li3 60.04(6) . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.6 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C4 H4A 109.4 . . ?
C1 C4 H4B 109.3 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.7 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.4 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 Li3 N3 84.75(9) . . ?
N1 Li3 N2 106.21(11) . 2_566 ?
N3 Li3 N2 106.03(11) . 2_566 ?
N1 Li3 Li2 56.63(9) . 2_566 ?
N3 Li3 Li2 116.87(11) . 2_566 ?
N2 Li3 Li2 53.83(8) 2_566 2_566 ?
N1 Li3 Li1 116.88(12) . 2_566 ?
N3 Li3 Li1 56.73(9) . 2_566 ?
N2 Li3 Li1 53.49(8) 2_566 2_566 ?
Li2 Li3 Li1 95.96(11) 2_566 2_566 ?
N1 Li3 P1 42.55(5) . . ?
N3 Li3 P1 42.71(5) . . ?
N2 Li3 P1 117.25(10) 2_566 . ?
Li2 Li3 P1 89.59(9) 2_566 . ?
Li1 Li3 P1 89.78(9) 2_566 . ?
N1 Li3 C7 136.56(12) . 2_566 ?
N3 Li3 C7 136.88(12) . 2_566 ?
N2 Li3 C7 58.15(7) 2_566 2_566 ?
Li2 Li3 C7 87.15(10) 2_566 2_566 ?
Li1 Li3 C7 87.32(10) 2_566 2_566 ?
P1 Li3 C7 175.39(10) . 2_566 ?
N1 Li3 Li2 78.90(8) . . ?
N3 Li3 Li2 30.15(6) . . ?
N2 Li3 Li2 79.30(8) 2_566 . ?
Li2 Li3 Li2 89.86(9) 2_566 . ?
Li1 Li3 Li2 42.00(8) 2_566 . ?
P1 Li3 Li2 48.11(5) . . ?
C7 Li3 Li2 128.57(9) 2_566 . ?
N1 Li3 Li1 29.98(6) . . ?
N3 Li3 Li1 78.96(8) . . ?
N2 Li3 Li1 79.57(8) 2_566 . ?
Li2 Li3 Li1 41.96(8) 2_566 . ?
Li1 Li3 Li1 90.02(9) 2_566 . ?
P1 Li3 Li1 47.96(5) . . ?
C7 Li3 Li1 128.41(9) 2_566 . ?
Li2 Li3 Li1 59.95(7) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.042
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1821184'
_audit_update_record             
;
2018-02-01 deposited with the CCDC.
2018-05-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H29 Li N3 P'
_chemical_formula_sum            'C11 H29 Li N3 P'
_chemical_formula_weight         241.28

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'
Li Li -0.0003 0.0001 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

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

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

_cell_length_a                   9.6620(7)
_cell_length_b                   16.2120(16)
_cell_length_c                   9.8750(4)
_cell_angle_alpha                90.000(7)
_cell_angle_beta                 104.960(6)
_cell_angle_gamma                90.000(6)
_cell_volume                     1494.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    22564
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_F_000             536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.593
_exptl_crystal_size_mid          0.492
_exptl_crystal_size_min          0.424
_exptl_absorpt_coefficient_mu    0.165
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.250
0 0 1 0.229
1 0 0 0.246
-1 0 0 0.205
0 -1 0 0.212
0 1 0 0.198
-1 -1 0 0.236
-1 1 0 0.218
1 1 0 0.242
1 -1 0 0.252
-1 0 1 0.252
1 0 -1 0.321


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_process_details   
;
Gaussian integration (Coppens, 1970)
;

_diffrn_ambient_temperature      150(1)
_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 Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_reflns_number            22438
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.182
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             3492
_reflns_number_gt                2955
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'


_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0575P)²+1.0132P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3492
_refine_ls_number_parameters     157
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.1215
_refine_ls_wR_factor_gt          0.1084
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.69845(6) 0.2500 0.09565(5) 0.01483(14) Uani 1 2 d S T P . .
P2 P 0.86352(6) 0.2500 0.35657(5) 0.01537(14) Uani 1 2 d S T P . .
N1 N 0.78361(13) 0.17776(8) 0.22542(12) 0.0157(3) Uani 1 1 d . . . . .
N4 N 0.46197(15) 0.08334(8) 0.35597(14) 0.0231(3) Uani 1 1 d . . . . .
N2 N 0.53472(18) 0.2500 0.11881(18) 0.0162(4) Uani 1 2 d S T P . .
N3 N 0.74389(19) 0.2500 0.45019(18) 0.0168(4) Uani 1 2 d S T P . .
C5 C 0.8027(2) 0.2500 0.6050(2) 0.0204(4) Uani 1 2 d S T P . .
C1 C 0.86348(17) 0.10600(10) 0.19111(17) 0.0219(3) Uani 1 1 d . . . . .
C11 C 0.54421(17) 0.03119(10) 0.47066(18) 0.0245(4) Uani 1 1 d . . . . .
H11A H 0.5950 0.0667 0.5464 0.029 Uiso 1 1 d R U . . .
H11B H 0.6155 0.0011 0.4370 0.029 Uiso 1 1 d R U . . .
C12 C 0.3927(2) 0.03428(12) 0.23285(19) 0.0344(4) Uani 1 1 d . . . . .
H12A H 0.3193 0.0006 0.2540 0.041 Uiso 1 1 d R U . . .
H12B H 0.4627 -0.0003 0.2076 0.041 Uiso 1 1 d R U . . .
H12C H 0.3507 0.0703 0.1561 0.041 Uiso 1 1 d R U . . .
C2 C 0.9212(2) 0.05612(11) 0.3248(2) 0.0327(4) Uani 1 1 d . . . . .
H2A H 0.9901 0.0885 0.3910 0.039 Uiso 1 1 d R U . . .
H2B H 0.9661 0.0068 0.3031 0.039 Uiso 1 1 d R U . . .
H2C H 0.8435 0.0417 0.3643 0.039 Uiso 1 1 d R U . . .
C3 C 0.98809(19) 0.13293(12) 0.1324(2) 0.0307(4) Uani 1 1 d . . . . .
H3A H 0.9517 0.1638 0.0477 0.037 Uiso 1 1 d R U . . .
H3B H 1.0382 0.0851 0.1125 0.037 Uiso 1 1 d R U . . .
H3C H 1.0525 0.1668 0.2000 0.037 Uiso 1 1 d R U . . .
C9 C 0.2748(2) 0.2500 0.0291(2) 0.0255(5) Uani 1 2 d S T P . .
H9A H 0.2703 0.2024 0.0857 0.038 Uiso 0.5 1 calc R U P . .
H9B H 0.1967 0.2485 -0.0539 0.038 Uiso 1 2 calc R U P . .
H9C H 0.2680 0.2991 0.0814 0.038 Uiso 0.5 1 calc R U P . .
H9D H 0.2197 0.2976 -0.0102 0.038 Uiso 0.5 1 calc R U P . .
H9E H 0.2933 0.2515 0.1294 0.038 Uiso 1 2 calc R U P . .
H9F H 0.2220 0.2009 -0.0059 0.038 Uiso 0.5 1 calc R U P . .
C10 C 0.41959(18) 0.17326(11) -0.10233(17) 0.0256(4) Uani 1 1 d . . . . .
H10A H 0.5060 0.1736 -0.1332 0.031 Uiso 1 1 d R U . . .
H10B H 0.3382 0.1739 -0.1823 0.031 Uiso 1 1 d R U . . .
H10C H 0.4169 0.1245 -0.0480 0.031 Uiso 1 1 d R U . . .
C7 C 0.8938(2) 0.17326(12) 0.65680(18) 0.0298(4) Uani 1 1 d . . . . .
H7A H 0.8381 0.1246 0.6257 0.036 Uiso 1 1 d R U . . .
H7B H 0.9240 0.1737 0.7574 0.036 Uiso 1 1 d R U . . .
H7C H 0.9764 0.1735 0.6198 0.036 Uiso 1 1 d R U . . .
C13 C 0.3548(2) 0.13312(11) 0.4005(2) 0.0303(4) Uani 1 1 d . . . . .
H13A H 0.3124 0.1718 0.3280 0.036 Uiso 1 1 d R U . . .
H13B H 0.4002 0.1625 0.4847 0.036 Uiso 1 1 d R U . . .
H13C H 0.2818 0.0976 0.4180 0.036 Uiso 1 1 d R U . . .
C8 C 0.4159(2) 0.2500 -0.0119(2) 0.0186(4) Uani 1 2 d S T P . .
C6 C 0.6768(3) 0.2500 0.6718(2) 0.0270(5) Uani 1 2 d S T P . .
H6A H 0.6181 0.2024 0.6408 0.041 Uiso 0.5 1 calc R U P . .
H6B H 0.6209 0.2991 0.6446 0.041 Uiso 0.5 1 calc R U P . .
H6C H 0.7123 0.2486 0.7720 0.041 Uiso 1 2 calc R U P . .
H6D H 0.6827 0.2976 0.7308 0.041 Uiso 0.5 1 calc R U P . .
H6E H 0.6800 0.2009 0.7269 0.041 Uiso 0.5 1 calc R U P . .
H6F H 0.5886 0.2514 0.5996 0.041 Uiso 1 2 calc R U P . .
C4 C 0.7612(2) 0.05347(12) 0.0826(2) 0.0371(5) Uani 1 1 d . . . . .
H4A H 0.6828 0.0359 0.1188 0.044 Uiso 1 1 d R U . . .
H4B H 0.8110 0.0060 0.0611 0.044 Uiso 1 1 d R U . . .
H4C H 0.7250 0.0853 -0.0011 0.044 Uiso 1 1 d R U . . .
Li1 Li 0.6012(3) 0.17155(17) 0.3011(3) 0.0209(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N2 1.6558(18) . ?
P1 N1 1.7738(13) 4_565 ?
P1 N1 1.7738(13) . ?
P1 P2 2.6572(8) . ?
P1 Li1 2.757(3) 4_565 ?
P1 Li1 2.757(3) . ?
P2 N3 1.6560(18) . ?
P2 N1 1.7688(13) . ?
P2 N1 1.7688(13) 4_565 ?
P2 Li1 2.761(3) 4_565 ?
P2 Li1 2.761(3) . ?
N1 C1 1.4828(19) . ?
N1 Li1 2.087(3) . ?
N4 C12 1.463(2) . ?
N4 C13 1.467(2) . ?
N4 C11 1.471(2) . ?
N4 Li1 2.127(3) . ?
N2 C8 1.490(3) . ?
N2 Li1 2.161(3) 4_565 ?
N2 Li1 2.161(3) . ?
N3 C5 1.487(3) . ?
N3 Li1 2.154(3) . ?
N3 Li1 2.154(3) 4_565 ?
C5 C6 1.526(3) . ?
C5 C7 1.534(2) . ?
C5 C7 1.534(2) 4_565 ?
C1 C4 1.518(2) . ?
C1 C2 1.525(2) . ?
C1 C3 1.529(2) . ?
C11 C11 1.531(3) 3_656 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9699 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9599 . ?
C2 H2C 0.9601 . ?
C3 H3A 0.9599 . ?
C3 H3B 0.9601 . ?
C3 H3C 0.9599 . ?
C9 C8 1.519(3) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9 H9D 0.9600 . ?
C9 H9E 0.9600 . ?
C9 H9F 0.9600 . ?
C10 C8 1.537(2) . ?
C10 H10A 0.9599 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9599 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9601 . ?
C7 H7C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C8 C10 1.537(2) 4_565 ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C6 H6D 0.9600 . ?
C6 H6E 0.9600 . ?
C6 H6F 0.9600 . ?
C4 H4A 0.9601 . ?
C4 H4B 0.9599 . ?
C4 H4C 0.9600 . ?
Li1 Li1 2.544(5) 4_565 ?

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
N2 P1 N1 100.47(6) . 4_565 ?
N2 P1 N1 100.47(6) . . ?
N1 P1 N1 82.64(8) 4_565 . ?
N2 P1 P2 102.81(6) . . ?
N1 P1 P2 41.33(4) 4_565 . ?
N1 P1 P2 41.33(4) . . ?
N2 P1 Li1 51.61(7) . 4_565 ?
N1 P1 Li1 49.19(7) 4_565 4_565 ?
N1 P1 Li1 87.46(7) . 4_565 ?
P2 P1 Li1 61.30(6) . 4_565 ?
N2 P1 Li1 51.61(7) . . ?
N1 P1 Li1 87.46(7) 4_565 . ?
N1 P1 Li1 49.19(7) . . ?
P2 P1 Li1 61.30(6) . . ?
Li1 P1 Li1 54.95(11) 4_565 . ?
N3 P2 N1 99.97(6) . . ?
N3 P2 N1 99.97(6) . 4_565 ?
N1 P2 N1 82.92(8) . 4_565 ?
N3 P2 P1 102.16(6) . . ?
N1 P2 P1 41.47(4) . . ?
N1 P2 P1 41.47(4) 4_565 . ?
N3 P2 Li1 51.22(7) . 4_565 ?
N1 P2 Li1 87.41(7) . 4_565 ?
N1 P2 Li1 49.07(7) 4_565 4_565 ?
P1 P2 Li1 61.12(6) . 4_565 ?
N3 P2 Li1 51.22(7) . . ?
N1 P2 Li1 49.07(7) . . ?
N1 P2 Li1 87.40(7) 4_565 . ?
P1 P2 Li1 61.12(6) . . ?
Li1 P2 Li1 54.84(11) 4_565 . ?
C1 N1 P2 122.15(10) . . ?
C1 N1 P1 121.64(10) . . ?
P2 N1 P1 97.19(6) . . ?
C1 N1 Li1 125.55(12) . . ?
P2 N1 Li1 91.10(9) . . ?
P1 N1 Li1 90.76(9) . . ?
C12 N4 C13 109.95(14) . . ?
C12 N4 C11 111.58(14) . . ?
C13 N4 C11 111.61(13) . . ?
C12 N4 Li1 109.73(13) . . ?
C13 N4 Li1 104.37(13) . . ?
C11 N4 Li1 109.34(12) . . ?
C8 N2 P1 115.51(14) . . ?
C8 N2 Li1 135.91(10) . 4_565 ?
P1 N2 Li1 91.49(10) . 4_565 ?
C8 N2 Li1 135.91(10) . . ?
P1 N2 Li1 91.49(10) . . ?
Li1 N2 Li1 72.08(15) 4_565 . ?
C5 N3 P2 115.94(14) . . ?
C5 N3 Li1 135.25(11) . . ?
P2 N3 Li1 91.96(10) . . ?
C5 N3 Li1 135.25(11) . 4_565 ?
P2 N3 Li1 91.96(10) . 4_565 ?
Li1 N3 Li1 72.38(15) . 4_565 ?
N3 C5 C6 107.99(18) . . ?
N3 C5 C7 112.15(12) . . ?
C6 C5 C7 107.99(13) . . ?
N3 C5 C7 112.14(12) . 4_565 ?
C6 C5 C7 107.99(13) . 4_565 ?
C7 C5 C7 108.42(19) . 4_565 ?
N1 C1 C4 108.61(13) . . ?
N1 C1 C2 108.29(13) . . ?
C4 C1 C2 109.85(15) . . ?
N1 C1 C3 111.71(14) . . ?
C4 C1 C3 108.98(15) . . ?
C2 C1 C3 109.38(14) . . ?
N4 C11 C11 115.33(17) . 3_656 ?
N4 C11 H11A 108.5 . . ?
C11 C11 H11A 108.7 3_656 . ?
N4 C11 H11B 108.4 . . ?
C11 C11 H11B 108.2 3_656 . ?
H11A C11 H11B 107.5 . . ?
N4 C12 H12A 109.5 . . ?
N4 C12 H12B 109.4 . . ?
H12A C12 H12B 109.5 . . ?
N4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.3 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.4 . . ?
C1 C3 H3B 109.6 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.4 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C9 H9D 109.5 . . ?
H9A C9 H9D 141.1 . . ?
H9B C9 H9D 56.3 . . ?
H9C C9 H9D 56.3 . . ?
C8 C9 H9E 109.5 . . ?
H9A C9 H9E 56.3 . . ?
H9B C9 H9E 141.1 . . ?
H9C C9 H9E 56.3 . . ?
H9D C9 H9E 109.5 . . ?
C8 C9 H9F 109.5 . . ?
H9A C9 H9F 56.3 . . ?
H9B C9 H9F 56.3 . . ?
H9C C9 H9F 141.1 . . ?
H9D C9 H9F 109.5 . . ?
H9E C9 H9F 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.4 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.4 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C13 H13A 109.5 . . ?
N4 C13 H13B 109.4 . . ?
H13A C13 H13B 109.5 . . ?
N4 C13 H13C 109.4 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C8 C9 108.25(17) . . ?
N2 C8 C10 112.02(12) . . ?
C9 C8 C10 108.18(12) . . ?
N2 C8 C10 112.02(12) . 4_565 ?
C9 C8 C10 108.18(12) . 4_565 ?
C10 C8 C10 108.06(18) . 4_565 ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C6 H6D 109.5 . . ?
H6A C6 H6D 141.1 . . ?
H6B C6 H6D 56.3 . . ?
H6C C6 H6D 56.3 . . ?
C5 C6 H6E 109.5 . . ?
H6A C6 H6E 56.3 . . ?
H6B C6 H6E 141.1 . . ?
H6C C6 H6E 56.3 . . ?
H6D C6 H6E 109.5 . . ?
C5 C6 H6F 109.5 . . ?
H6A C6 H6F 56.3 . . ?
H6B C6 H6F 56.3 . . ?
H6C C6 H6F 141.1 . . ?
H6D C6 H6F 109.5 . . ?
H6E C6 H6F 109.5 . . ?
C1 C4 H4A 109.6 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.4 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 Li1 N4 140.51(15) . . ?
N1 Li1 N3 76.43(10) . . ?
N4 Li1 N3 123.92(14) . . ?
N1 Li1 N2 76.73(10) . . ?
N4 Li1 N2 122.44(14) . . ?
N3 Li1 N2 102.83(12) . . ?
N1 Li1 Li1 87.23(8) . 4_565 ?
N4 Li1 Li1 132.25(8) . 4_565 ?
N3 Li1 Li1 53.81(8) . 4_565 ?
N2 Li1 Li1 53.96(8) . 4_565 ?
N1 Li1 P1 40.04(6) . . ?
N4 Li1 P1 148.85(13) . . ?
N3 Li1 P1 87.19(9) . . ?
N2 Li1 P1 36.90(6) . . ?
Li1 Li1 P1 62.53(6) 4_565 . ?
N1 Li1 P2 39.82(6) . . ?
N4 Li1 P2 150.16(13) . . ?
N3 Li1 P2 36.82(6) . . ?
N2 Li1 P2 87.39(9) . . ?
Li1 Li1 P2 62.58(6) 4_565 . ?
P1 Li1 P2 57.57(5) . . ?

_refine_diff_density_max         0.347
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.061
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1844612'
_audit_update_record             
;
2018-05-22 deposited with the CCDC.
2018-05-30 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT340_shelx               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00789 Ang.
RESPONSE: poorly diffracting, highly sensitive crystal
;
_vrf_PLAT906_shelx               
;
PROBLEM: Large K Value in the Analysis of Variance ......      3.585 Check
RESPONSE: poorly diffracting, highly sensitive crystal
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         12 Report
RESPONSE: poorly diffracting, highly sensitive crystal
;
_vrf_PLAT913_shelx               
;
PROBLEM: Missing # of Very Strong Reflections in FCF ....          5 Note
RESPONSE: poorly diffracting, highly sensitive crystal
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H39 Na O3'
_chemical_formula_sum            'C31 H39 Na O3'
_chemical_formula_weight         482.61

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

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

_cell_length_a                   10.389(4)
_cell_length_b                   15.520(7)
_cell_length_c                   16.805(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2709.7(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    20590
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_F_000             1040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.592
_exptl_crystal_size_mid          0.264
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.088
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5958
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_special_details           
;
The ratio of minimum to maximum
apparent transmission was 0.799
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            20507
_diffrn_reflns_av_unetI/netI     0.0822
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.359
_diffrn_reflns_theta_max         27.461
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5965
_reflns_number_gt                3784
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_max     0.945
_reflns_Friedel_fraction_full    0.996

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

_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0446P)²+2.3712P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.047(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1284 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.2(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5965
_refine_ls_number_parameters     324
_refine_ls_number_restraints     360
_refine_ls_R_factor_all          0.1346
_refine_ls_R_factor_gt           0.0742
_refine_ls_wR_factor_ref         0.1728
_refine_ls_wR_factor_gt          0.1459
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001

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
Na1 Na 0.65366(19) 0.63916(12) 0.25805(11) 0.0393(5) Uani 1 1 d . U . . .
O1 O 0.7218(4) 0.6825(2) 0.3814(2) 0.0468(10) Uani 1 1 d . U . . .
C1 C 0.6561(4) 0.4721(3) 0.2500(3) 0.0284(9) Uani 1 1 d . U . . .
C2 C 0.5814(5) 0.4729(3) 0.1760(3) 0.0329(11) Uani 1 1 d . U . . .
O2 O 0.4582(3) 0.6975(3) 0.2279(2) 0.0451(9) Uani 1 1 d . U . . .
C3 C 0.6254(5) 0.5133(3) 0.1056(3) 0.0387(12) Uani 1 1 d . U . . .
H3 H 0.7070 0.5409 0.1061 0.046 Uiso 1 1 calc R U . . .
O3 O 0.7746(4) 0.7205(3) 0.1746(3) 0.0563(11) Uani 1 1 d . U . . .
C4 C 0.5541(6) 0.5140(4) 0.0362(3) 0.0485(14) Uani 1 1 d . U . . .
H4 H 0.5881 0.5409 -0.0101 0.058 Uiso 1 1 calc R U . . .
C5 C 0.4334(6) 0.4761(4) 0.0335(3) 0.0546(16) Uani 1 1 d . U . . .
H5 H 0.3837 0.4776 -0.0139 0.065 Uiso 1 1 calc R U . . .
C6 C 0.3870(6) 0.4362(4) 0.1003(3) 0.0528(15) Uani 1 1 d . U . . .
H6 H 0.3043 0.4103 0.0991 0.063 Uiso 1 1 calc R U . . .
C8 C 0.7968(4) 0.4708(3) 0.2461(3) 0.0301(10) Uani 1 1 d . U . . .
C7 C 0.4590(5) 0.4333(4) 0.1697(3) 0.0407(13) Uani 1 1 d . U . . .
H7 H 0.4251 0.4037 0.2145 0.049 Uiso 1 1 calc R U . . .
C9 C 0.8757(5) 0.5054(3) 0.3070(3) 0.0334(11) Uani 1 1 d . U . . .
H9 H 0.8359 0.5293 0.3529 0.040 Uiso 1 1 calc R U . . .
C10 C 1.0097(5) 0.5057(4) 0.3020(3) 0.0439(13) Uani 1 1 d . U . . .
H10 H 1.0589 0.5294 0.3443 0.053 Uiso 1 1 calc R U . . .
C11 C 1.0717(6) 0.4721(4) 0.2366(3) 0.0490(14) Uani 1 1 d . U . . .
H11 H 1.1629 0.4731 0.2331 0.059 Uiso 1 1 calc R U . . .
C12 C 0.9987(5) 0.4370(4) 0.1763(3) 0.0445(13) Uani 1 1 d . U . . .
H12 H 1.0402 0.4129 0.1310 0.053 Uiso 1 1 calc R U . . .
C13 C 0.8653(5) 0.4364(3) 0.1809(3) 0.0381(12) Uani 1 1 d . U . . .
H13 H 0.8179 0.4117 0.1382 0.046 Uiso 1 1 calc R U . . .
C14 C 0.5893(5) 0.4686(3) 0.3261(3) 0.0305(11) Uani 1 1 d . U . . .
C15 C 0.4658(5) 0.5056(3) 0.3375(3) 0.0387(12) Uani 1 1 d . U . . .
H15 H 0.4252 0.5332 0.2937 0.046 Uiso 1 1 calc R U . . .
C16 C 0.4023(6) 0.5030(4) 0.4097(3) 0.0503(15) Uani 1 1 d . U . . .
H16 H 0.3195 0.5286 0.4142 0.060 Uiso 1 1 calc R U . . .
C17 C 0.4566(7) 0.4643(4) 0.4751(3) 0.0574(16) Uani 1 1 d . U . . .
H17 H 0.4128 0.4631 0.5247 0.069 Uiso 1 1 calc R U . . .
C18 C 0.5782(7) 0.4266(4) 0.4667(3) 0.0544(16) Uani 1 1 d . U . . .
H18 H 0.6172 0.3994 0.5112 0.065 Uiso 1 1 calc R U . . .
C19 C 0.6430(6) 0.4283(3) 0.3944(3) 0.0411(12) Uani 1 1 d . U . . .
H19 H 0.7252 0.4019 0.3905 0.049 Uiso 1 1 calc R U . . .
C20 C 0.6646(7) 0.6607(4) 0.4566(3) 0.0586(17) Uani 1 1 d . U . . .
H20A H 0.6982 0.6049 0.4763 0.070 Uiso 1 1 calc R U . . .
H20B H 0.5699 0.6566 0.4518 0.070 Uiso 1 1 calc R U . . .
C21 C 0.7013(7) 0.7313(4) 0.5105(4) 0.0608(18) Uani 1 1 d . U . . .
H21A H 0.6981 0.7127 0.5668 0.073 Uiso 1 1 calc R U . . .
H21B H 0.6444 0.7819 0.5034 0.073 Uiso 1 1 calc R U . . .
C22 C 0.8378(7) 0.7512(5) 0.4848(4) 0.072(2) Uani 1 1 d . U . . .
H22A H 0.8572 0.8133 0.4913 0.087 Uiso 1 1 calc R U . . .
H22B H 0.9006 0.7173 0.5162 0.087 Uiso 1 1 calc R U . . .
C23 C 0.8411(7) 0.7257(4) 0.3985(4) 0.0680(19) Uani 1 1 d . U . . .
H23A H 0.8504 0.7774 0.3644 0.082 Uiso 1 1 calc R U . . .
H23B H 0.9147 0.6868 0.3882 0.082 Uiso 1 1 calc R U . . .
C24 C 0.3923(5) 0.6887(5) 0.1537(3) 0.0537(15) Uani 1 1 d . U . . .
H24A H 0.4209 0.6358 0.1259 0.064 Uiso 1 1 calc R U . . .
H24B H 0.4102 0.7389 0.1191 0.064 Uiso 1 1 calc R U . . .
C25 C 0.2525(6) 0.6836(6) 0.1722(4) 0.073(2) Uani 1 1 d . U . . .
H25A H 0.2034 0.7239 0.1381 0.088 Uiso 1 1 calc R U . . .
H25B H 0.2201 0.6245 0.1629 0.088 Uiso 1 1 calc R U . . .
C26 C 0.2382(6) 0.7072(5) 0.2567(4) 0.072(2) Uani 1 1 d . U . . .
H26A H 0.2078 0.6573 0.2881 0.086 Uiso 1 1 calc R U . . .
H26B H 0.1757 0.7549 0.2628 0.086 Uiso 1 1 calc R U . . .
C27 C 0.3687(6) 0.7346(4) 0.2837(4) 0.0567(16) Uani 1 1 d . U . . .
H27A H 0.3757 0.7982 0.2836 0.068 Uiso 1 1 calc R U . . .
H27B H 0.3860 0.7133 0.3382 0.068 Uiso 1 1 calc R U . . .
C28 C 0.9110(5) 0.7196(4) 0.1670(4) 0.0527(16) Uani 1 1 d . U . . .
H28A H 0.9422 0.6602 0.1579 0.063 Uiso 1 1 calc R U . . .
H28B H 0.9518 0.7423 0.2160 0.063 Uiso 1 1 calc R U . . .
C29 C 0.9434(6) 0.7763(4) 0.0966(4) 0.0566(16) Uani 1 1 d . U . . .
H29A H 1.0068 0.8210 0.1121 0.068 Uiso 1 1 calc R U . A 1
H29B H 0.9802 0.7415 0.0528 0.068 Uiso 1 1 calc R U . A 1
C30 C 0.8241(17) 0.8156(14) 0.0722(12) 0.071(5) Uani 0.64(2) 1 d . U P B 1
H30A H 0.7938 0.7902 0.0216 0.085 Uiso 0.64(2) 1 calc R U P B 1
H30B H 0.8355 0.8784 0.0647 0.085 Uiso 0.64(2) 1 calc R U P B 1
C31 C 0.7302(12) 0.7982(9) 0.1373(9) 0.050(3) Uani 0.64(2) 1 d . U P B 1
H31A H 0.7287 0.8464 0.1758 0.060 Uiso 0.64(2) 1 calc R U P B 1
H31B H 0.6425 0.7903 0.1154 0.060 Uiso 0.64(2) 1 calc R U P B 1
C30A C 0.799(3) 0.788(3) 0.059(2) 0.071(5) Uani 0.36(2) 1 d . U P B 2
H30C H 0.7867 0.8486 0.0425 0.085 Uiso 0.36(2) 1 calc R U P B 2
H30D H 0.7900 0.7511 0.0116 0.085 Uiso 0.36(2) 1 calc R U P B 2
C31A C 0.717(2) 0.7692(17) 0.1066(16) 0.050(3) Uani 0.36(2) 1 d . U P B 2
H31C H 0.6504 0.7333 0.0804 0.060 Uiso 0.36(2) 1 calc R U P B 2
H31D H 0.6749 0.8222 0.1267 0.060 Uiso 0.36(2) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 O3 2.267(4) . ?
Na1 O2 2.280(4) . ?
Na1 O1 2.291(4) . ?
Na1 C1 2.596(5) . ?
Na1 C14 2.960(5) . ?
Na1 C8 3.013(5) . ?
Na1 C2 3.021(5) . ?
O1 C20 1.437(6) . ?
O1 C23 1.438(7) . ?
C1 C14 1.457(6) . ?
C1 C8 1.463(6) . ?
C1 C2 1.466(6) . ?
C2 C3 1.414(7) . ?
C2 C7 1.416(7) . ?
O2 C24 1.429(6) . ?
O2 C27 1.440(6) . ?
C3 C4 1.382(7) . ?
C3 H3 0.9500 . ?
O3 C28 1.423(6) . ?
O3 C31 1.436(11) . ?
O3 C31A 1.50(2) . ?
C4 C5 1.386(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.369(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.386(7) . ?
C6 H6 0.9500 . ?
C8 C13 1.412(7) . ?
C8 C9 1.417(6) . ?
C7 H7 0.9500 . ?
C9 C10 1.395(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.376(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.379(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.388(7) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.419(7) . ?
C14 C19 1.420(7) . ?
C15 C16 1.382(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.374(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.399(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(7) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.473(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.515(9) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.505(9) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.488(8) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.473(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.491(8) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.512(8) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.441(19) . ?
C29 C30A 1.64(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.49(2) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C30A C31A 1.20(4) . ?
C30A H30C 0.9900 . ?
C30A H30D 0.9900 . ?
C31A H31C 0.9900 . ?
C31A H31D 0.9900 . ?

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
O3 Na1 O2 97.78(15) . . ?
O3 Na1 O1 102.99(17) . . ?
O2 Na1 O1 111.07(16) . . ?
O3 Na1 C1 121.22(17) . . ?
O2 Na1 C1 113.17(16) . . ?
O1 Na1 C1 109.72(16) . . ?
O3 Na1 C14 149.56(17) . . ?
O2 Na1 C14 103.87(16) . . ?
O1 Na1 C14 89.02(14) . . ?
C1 Na1 C14 29.47(13) . . ?
O3 Na1 C8 99.69(16) . . ?
O2 Na1 C8 140.26(15) . . ?
O1 Na1 C8 99.33(15) . . ?
C1 Na1 C8 29.04(13) . . ?
C14 Na1 C8 50.32(13) . . ?
O3 Na1 C2 109.33(17) . . ?
O2 Na1 C2 90.94(15) . . ?
O1 Na1 C2 137.78(15) . . ?
C1 Na1 C2 29.01(14) . . ?
C14 Na1 C2 49.93(13) . . ?
C8 Na1 C2 49.57(14) . . ?
C20 O1 C23 106.9(4) . . ?
C20 O1 Na1 126.7(3) . . ?
C23 O1 Na1 125.7(3) . . ?
C14 C1 C8 120.9(4) . . ?
C14 C1 C2 119.5(4) . . ?
C8 C1 C2 119.5(4) . . ?
C14 C1 Na1 89.3(3) . . ?
C8 C1 Na1 91.5(3) . . ?
C2 C1 Na1 91.8(3) . . ?
C3 C2 C7 114.8(5) . . ?
C3 C2 C1 122.8(4) . . ?
C7 C2 C1 122.4(4) . . ?
C3 C2 Na1 85.6(3) . . ?
C7 C2 Na1 128.9(3) . . ?
C1 C2 Na1 59.2(2) . . ?
C24 O2 C27 107.3(4) . . ?
C24 O2 Na1 125.6(3) . . ?
C27 O2 Na1 126.1(3) . . ?
C4 C3 C2 122.4(5) . . ?
C4 C3 H3 118.8 . . ?
C2 C3 H3 118.8 . . ?
C28 O3 C31 106.8(6) . . ?
C28 O3 C31A 109.6(9) . . ?
C28 O3 Na1 127.0(4) . . ?
C31 O3 Na1 124.1(5) . . ?
C31A O3 Na1 122.1(9) . . ?
C3 C4 C5 120.6(5) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 118.9(5) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C7 121.0(6) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C13 C8 C9 114.4(4) . . ?
C13 C8 C1 122.9(4) . . ?
C9 C8 C1 122.7(4) . . ?
C13 C8 Na1 128.9(3) . . ?
C9 C8 Na1 84.7(3) . . ?
C1 C8 Na1 59.4(2) . . ?
C6 C7 C2 122.2(5) . . ?
C6 C7 H7 118.9 . . ?
C2 C7 H7 118.9 . . ?
C10 C9 C8 122.3(5) . . ?
C10 C9 H9 118.8 . . ?
C8 C9 H9 118.8 . . ?
C11 C10 C9 121.0(5) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 118.7(5) . . ?
C10 C11 H11 120.7 . . ?
C12 C11 H11 120.7 . . ?
C11 C12 C13 120.7(5) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C8 123.0(5) . . ?
C12 C13 H13 118.5 . . ?
C8 C13 H13 118.5 . . ?
C15 C14 C19 115.1(5) . . ?
C15 C14 C1 122.3(4) . . ?
C19 C14 C1 122.6(5) . . ?
C15 C14 Na1 83.9(3) . . ?
C19 C14 Na1 128.1(3) . . ?
C1 C14 Na1 61.3(2) . . ?
C16 C15 C14 122.6(5) . . ?
C16 C15 H15 118.7 . . ?
C14 C15 H15 118.7 . . ?
C17 C16 C15 121.3(6) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 118.2(5) . . ?
C16 C17 H17 120.9 . . ?
C18 C17 H17 120.9 . . ?
C19 C18 C17 121.2(6) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C18 C19 C14 121.6(6) . . ?
C18 C19 H19 119.2 . . ?
C14 C19 H19 119.2 . . ?
O1 C20 C21 105.0(5) . . ?
O1 C20 H20A 110.8 . . ?
C21 C20 H20A 110.8 . . ?
O1 C20 H20B 110.8 . . ?
C21 C20 H20B 110.8 . . ?
H20A C20 H20B 108.8 . . ?
C20 C21 C22 102.6(6) . . ?
C20 C21 H21A 111.2 . . ?
C22 C21 H21A 111.2 . . ?
C20 C21 H21B 111.2 . . ?
C22 C21 H21B 111.2 . . ?
H21A C21 H21B 109.2 . . ?
C23 C22 C21 104.0(5) . . ?
C23 C22 H22A 111.0 . . ?
C21 C22 H22A 111.0 . . ?
C23 C22 H22B 111.0 . . ?
C21 C22 H22B 111.0 . . ?
H22A C22 H22B 109.0 . . ?
O1 C23 C22 107.2(5) . . ?
O1 C23 H23A 110.3 . . ?
C22 C23 H23A 110.3 . . ?
O1 C23 H23B 110.3 . . ?
C22 C23 H23B 110.3 . . ?
H23A C23 H23B 108.5 . . ?
O2 C24 C25 106.9(5) . . ?
O2 C24 H24A 110.3 . . ?
C25 C24 H24A 110.3 . . ?
O2 C24 H24B 110.3 . . ?
C25 C24 H24B 110.3 . . ?
H24A C24 H24B 108.6 . . ?
C26 C25 C24 106.6(5) . . ?
C26 C25 H25A 110.4 . . ?
C24 C25 H25A 110.4 . . ?
C26 C25 H25B 110.4 . . ?
C24 C25 H25B 110.4 . . ?
H25A C25 H25B 108.6 . . ?
C25 C26 C27 105.8(5) . . ?
C25 C26 H26A 110.6 . . ?
C27 C26 H26A 110.6 . . ?
C25 C26 H26B 110.6 . . ?
C27 C26 H26B 110.6 . . ?
H26A C26 H26B 108.7 . . ?
O2 C27 C26 106.0(5) . . ?
O2 C27 H27A 110.5 . . ?
C26 C27 H27A 110.5 . . ?
O2 C27 H27B 110.5 . . ?
C26 C27 H27B 110.5 . . ?
H27A C27 H27B 108.7 . . ?
O3 C28 C29 106.6(5) . . ?
O3 C28 H28A 110.4 . . ?
C29 C28 H28A 110.4 . . ?
O3 C28 H28B 110.4 . . ?
C29 C28 H28B 110.4 . . ?
H28A C28 H28B 108.6 . . ?
C30 C29 C28 106.1(8) . . ?
C28 C29 C30A 99.2(12) . . ?
C30 C29 H29A 110.5 . . ?
C28 C29 H29A 110.5 . . ?
C30 C29 H29B 110.5 . . ?
C28 C29 H29B 110.5 . . ?
H29A C29 H29B 108.7 . . ?
C29 C30 C31 106.2(12) . . ?
C29 C30 H30A 110.5 . . ?
C31 C30 H30A 110.5 . . ?
C29 C30 H30B 110.5 . . ?
C31 C30 H30B 110.5 . . ?
H30A C30 H30B 108.7 . . ?
O3 C31 C30 105.2(10) . . ?
O3 C31 H31A 110.7 . . ?
C30 C31 H31A 110.7 . . ?
O3 C31 H31B 110.7 . . ?
C30 C31 H31B 110.7 . . ?
H31A C31 H31B 108.8 . . ?
C31A C30A C29 112(3) . . ?
C31A C30A H30C 109.3 . . ?
C29 C30A H30C 109.3 . . ?
C31A C30A H30D 109.3 . . ?
C29 C30A H30D 109.3 . . ?
H30C C30A H30D 108.0 . . ?
C30A C31A O3 110(2) . . ?
C30A C31A H31C 109.6 . . ?
O3 C31A H31C 109.6 . . ?
C30A C31A H31D 109.6 . . ?
O3 C31A H31D 109.6 . . ?
H31C C31A H31D 108.1 . . ?

_refine_diff_density_max         0.254
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.061

_shelxl_version_number           2013-4

