# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_131008-jjl
_database_code_depnum_ccdc_archive 'CCDC 1041232'
_audit_update_record             
;
2014-12-24 deposited with the CCDC.
2015-04-06 downloaded from the CCDC.
;
_audit_creation_date             2014-05-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         
'0.18(C57 H42 N3 O3 P3), 0.36(C H2 Cl2), 0.18(H2 O)'
_chemical_formula_sum            'C11 H10 Cl0.05 N2 O2 P2'
_chemical_formula_weight         265.76
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   11.5630(4)
_cell_length_b                   25.5200(7)
_cell_length_c                   18.8834(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.770(3)
_cell_angle_gamma                90.00
_cell_volume                     5474.1(3)
_cell_formula_units_Z            22
_cell_measurement_reflns_used    5791
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8089
_cell_measurement_theta_min      3.1793
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             3009
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23584
_diffrn_reflns_theta_full        28.87
_diffrn_reflns_theta_max         28.87
_diffrn_reflns_theta_min         3.19
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1954
_diffrn_measured_fraction_theta_full 0.858
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0106101000
_diffrn_orient_matrix_UB_12      0.0247378000
_diffrn_orient_matrix_UB_13      0.0146648000
_diffrn_orient_matrix_UB_21      0.0599168000
_diffrn_orient_matrix_UB_22      0.0014305000
_diffrn_orient_matrix_UB_23      0.0172516000
_diffrn_orient_matrix_UB_31      0.0140066000
_diffrn_orient_matrix_UB_32      0.0125730000
_diffrn_orient_matrix_UB_33      -0.0308248000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                8536
_reflns_number_total             12350
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.255
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         12350
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0654
_refine_ls_restrained_S_all      1.255
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1858
_refine_ls_wR_factor_ref         0.2080
_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. 
;
_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 O(H,H) groups
2.a Free rotating group:
 O40(H40A,H40B)
2.b Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B), C69(H69A,H69B)
2.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
  C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63),
 C64(H64), C65(H65), C66(H66), C67(H67), C68(H68)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
P1 P 0.23360(6) 0.40982(3) 0.67577(4) 0.03477(18) Uani 1 d . . .
P2 P 0.12831(6) 0.16360(3) 0.52532(4) 0.03726(19) Uani 1 d . . .
P3 P 0.60303(6) 0.33796(3) 0.46369(4) 0.03680(19) Uani 1 d . . .
N1 N 0.23890(19) 0.31606(8) 0.58232(11) 0.0334(5) Uani 1 d . . .
N2 N 0.3457(2) 0.32684(9) 0.48744(12) 0.0373(5) Uani 1 d . . .
O3 O 0.34696(17) 0.38232(8) 0.70056(10) 0.0434(5) Uani 1 d . . .
O5 O 0.11118(18) 0.20738(8) 0.47312(10) 0.0455(5) Uani 1 d . . .
N6 N 0.3409(2) 0.24404(9) 0.54323(12) 0.0363(5) Uani 1 d . . .
C7 C 0.5397(2) 0.27793(10) 0.42205(14) 0.0350(6) Uani 1 d . . .
C9 C 0.2075(2) 0.43030(10) 0.58101(14) 0.0343(6) Uani 1 d . . .
O10 O 0.60583(19) 0.33973(9) 0.54301(10) 0.0500(5) Uani 1 d . . .
C11 C 0.4435(2) 0.25255(10) 0.44417(13) 0.0345(6) Uani 1 d . . .
C12 C 0.2407(2) 0.40028(10) 0.52496(14) 0.0343(6) Uani 1 d . . .
C13 C 0.2793(2) 0.34501(10) 0.53310(13) 0.0325(5) Uani 1 d . . .
C14 C 0.2291(2) 0.23170(10) 0.63824(14) 0.0345(6) Uani 1 d . . .
C15 C 0.1693(2) 0.18451(10) 0.61881(14) 0.0364(6) Uani 1 d . . .
C16 C 0.2722(2) 0.26576(10) 0.58463(13) 0.0332(6) Uani 1 d . . .
C17 C 0.3741(2) 0.27637(10) 0.49507(13) 0.0334(6) Uani 1 d . . .
C18 C 0.7509(2) 0.33924(12) 0.44474(16) 0.0426(7) Uani 1 d . . .
C19 C 0.2329(3) 0.47106(11) 0.72455(15) 0.0419(6) Uani 1 d . . .
C21 C 0.2197(3) 0.09155(11) 0.44369(16) 0.0465(7) Uani 1 d . . .
H21 H 0.1470 0.0945 0.4130 0.056 Uiso 1 calc . . R
C22 C 0.5294(2) 0.39208(11) 0.41380(15) 0.0410(6) Uani 1 d . . .
C24 C 0.2390(3) 0.11747(10) 0.50905(14) 0.0383(6) Uani 1 d . . .
C25 C 0.5924(3) 0.25318(12) 0.37056(15) 0.0455(7) Uani 1 d . . .
H25 H 0.6570 0.2688 0.3562 0.055 Uiso 1 calc . . R
C26 C 0.1647(3) 0.48073(12) 0.56470(17) 0.0467(7) Uani 1 d . . .
H26 H 0.1435 0.5011 0.6011 0.056 Uiso 1 calc . . R
C27 C 0.4584(3) 0.18097(12) 0.36231(15) 0.0477(7) Uani 1 d . . .
H27 H 0.4314 0.1489 0.3426 0.057 Uiso 1 calc . . R
C28 C 0.2312(3) 0.42261(12) 0.45652(15) 0.0443(7) Uani 1 d . . .
H28 H 0.2549 0.4034 0.4199 0.053 Uiso 1 calc . . R
C29 C -0.0053(3) 0.12623(12) 0.52021(16) 0.0461(7) Uani 1 d . . .
C30 C 0.1527(3) 0.50155(12) 0.49588(17) 0.0522(8) Uani 1 d . . .
H30 H 0.1214 0.5349 0.4862 0.063 Uiso 1 calc . . R
C31 C 0.1055(2) 0.37665(11) 0.69486(15) 0.0404(6) Uani 1 d . . .
C32 C 0.8357(3) 0.31098(14) 0.48965(18) 0.0575(8) Uani 1 d . . .
H32 H 0.8168 0.2938 0.5294 0.069 Uiso 1 calc . . R
C33 C 0.2519(3) 0.24788(12) 0.70938(15) 0.0465(7) Uani 1 d . . .
H33 H 0.2908 0.2794 0.7217 0.056 Uiso 1 calc . . R
C34 C 0.4055(3) 0.20432(11) 0.41447(15) 0.0446(7) Uani 1 d . . .
H34 H 0.3435 0.1874 0.4299 0.053 Uiso 1 calc . . R
C35 C 0.1873(3) 0.47265(13) 0.44208(17) 0.0534(8) Uani 1 d . . .
H35 H 0.1812 0.4867 0.3961 0.064 Uiso 1 calc . . R
C36 C 0.5505(3) 0.20555(12) 0.34010(16) 0.0509(8) Uani 1 d . . .
H36 H 0.5853 0.1904 0.3045 0.061 Uiso 1 calc . . R
C37 C 0.1349(3) 0.15486(12) 0.67361(17) 0.0530(8) Uani 1 d . . .
H37 H 0.0939 0.1237 0.6620 0.064 Uiso 1 calc . . R
C38 C 0.2170(3) 0.21728(13) 0.76264(16) 0.0577(9) Uani 1 d . . .
H38 H 0.2322 0.2285 0.8103 0.069 Uiso 1 calc . . R
C39 C -0.0036(3) 0.37784(15) 0.64954(19) 0.0595(9) Uani 1 d . . .
H39 H -0.0114 0.3928 0.6040 0.071 Uiso 1 calc . . R
C41 C 0.4522(3) 0.38636(13) 0.34786(16) 0.0496(7) Uani 1 d . . .
H41 H 0.4359 0.3532 0.3279 0.060 Uiso 1 calc . . R
C42 C 0.1158(3) 0.35313(13) 0.76262(17) 0.0521(8) Uani 1 d . . .
H42 H 0.1884 0.3521 0.7937 0.063 Uiso 1 calc . . R
C43 C 0.3399(3) 0.49740(13) 0.74431(16) 0.0517(8) Uani 1 d . . .
H43 H 0.4081 0.4829 0.7333 0.062 Uiso 1 calc . . R
C44 C 0.3461(3) 0.11188(13) 0.55454(17) 0.0533(8) Uani 1 d . . .
H44 H 0.3591 0.1282 0.5993 0.064 Uiso 1 calc . . R
C45 C 0.1607(3) 0.17092(13) 0.74491(17) 0.0597(9) Uani 1 d . . .
H45 H 0.1394 0.1500 0.7807 0.072 Uiso 1 calc . . R
C46 C 0.5529(3) 0.44236(13) 0.44168(19) 0.0557(8) Uani 1 d . . .
H46 H 0.6039 0.4468 0.4856 0.067 Uiso 1 calc . . R
C47 C 0.4146(4) 0.05711(13) 0.4689(2) 0.0636(10) Uani 1 d . . .
H47 H 0.4740 0.0371 0.4553 0.076 Uiso 1 calc . . R
C48 C 0.1328(3) 0.49230(13) 0.74305(19) 0.0578(8) Uani 1 d . . .
H48 H 0.0608 0.4752 0.7308 0.069 Uiso 1 calc . . R
C49 C 0.3070(3) 0.06137(12) 0.42346(19) 0.0581(9) Uani 1 d . . .
H49 H 0.2934 0.0440 0.3794 0.070 Uiso 1 calc . . R
C50 C -0.0065(3) 0.07332(13) 0.53914(19) 0.0595(9) Uani 1 d . . .
H50 H 0.0640 0.0554 0.5537 0.071 Uiso 1 calc . . R
C51 C -0.1123(4) 0.04781(17) 0.5362(2) 0.0757(12) Uani 1 d . . .
H51 H -0.1128 0.0127 0.5492 0.091 Uiso 1 calc . . R
C52 C 0.4001(3) 0.43039(16) 0.31223(19) 0.0643(10) Uani 1 d . . .
H52 H 0.3483 0.4266 0.2685 0.077 Uiso 1 calc . . R
C53 C 0.5014(4) 0.48533(14) 0.4051(2) 0.0664(10) Uani 1 d . . .
H53 H 0.5189 0.5187 0.4238 0.080 Uiso 1 calc . . R
C54 C -0.0906(4) 0.33358(17) 0.7379(2) 0.0793(13) Uani 1 d . . .
H54 H -0.1562 0.3192 0.7524 0.095 Uiso 1 calc . . R
C55 C 0.9497(3) 0.30797(16) 0.4759(2) 0.0716(10) Uani 1 d . . .
H55 H 1.0066 0.2886 0.5063 0.086 Uiso 1 calc . . R
C56 C -0.1118(3) 0.15184(16) 0.49702(19) 0.0653(9) Uani 1 d . . .
H56 H -0.1126 0.1868 0.4828 0.078 Uiso 1 calc . . R
C57 C 0.3454(4) 0.54418(14) 0.77964(18) 0.0676(10) Uani 1 d . . .
H57 H 0.4168 0.5619 0.7913 0.081 Uiso 1 calc . . R
C58 C 0.2459(5) 0.56525(14) 0.7981(2) 0.0762(12) Uani 1 d . . .
H58 H 0.2501 0.5970 0.8226 0.091 Uiso 1 calc . . R
C59 C 0.8947(4) 0.3615(2) 0.3736(3) 0.0956(16) Uani 1 d . . .
H59 H 0.9149 0.3782 0.3339 0.115 Uiso 1 calc . . R
C60 C 0.4241(4) 0.47920(15) 0.3409(2) 0.0688(11) Uani 1 d . . .
H60 H 0.3880 0.5084 0.3168 0.083 Uiso 1 calc . . R
C61 C 0.9775(3) 0.33283(17) 0.4191(2) 0.0771(12) Uani 1 d . . .
H61 H 1.0539 0.3307 0.4104 0.092 Uiso 1 calc . . R
C62 C 0.0175(4) 0.33139(15) 0.7833(2) 0.0718(11) Uani 1 d . . .
H62 H 0.0244 0.3152 0.8280 0.086 Uiso 1 calc . . R
C63 C 0.4343(3) 0.08221(15) 0.53434(19) 0.0663(10) Uani 1 d . . .
H63 H 0.5069 0.0792 0.5650 0.080 Uiso 1 calc . . R
C64 C 0.1412(4) 0.53988(14) 0.7805(2) 0.0701(11) Uani 1 d . . .
H64 H 0.0743 0.5543 0.7935 0.084 Uiso 1 calc . . R
C65 C -0.1018(3) 0.35658(19) 0.6723(2) 0.0814(13) Uani 1 d . . .
H65 H -0.1753 0.3582 0.6423 0.098 Uiso 1 calc . . R
C66 C -0.2159(4) 0.0734(2) 0.5146(2) 0.0856(15) Uani 1 d . . .
H66 H -0.2866 0.0557 0.5130 0.103 Uiso 1 calc . . R
C67 C -0.2171(4) 0.1250(2) 0.4951(2) 0.0834(13) Uani 1 d . . .
H67 H -0.2884 0.1422 0.4806 0.100 Uiso 1 calc . . R
C68 C 0.7809(3) 0.36562(16) 0.3868(2) 0.0684(11) Uani 1 d . . .
H68 H 0.7254 0.3859 0.3569 0.082 Uiso 1 calc . . R
Cl4 Cl 0.44335(15) 0.68968(7) 0.80468(8) 0.1246(5) Uani 1 d . . .
Cl23 Cl 0.2254(2) 0.71498(7) 0.85001(14) 0.1778(9) Uani 1 d . . .
C74 C 0.3805(6) 0.7250(3) 0.8601(4) 0.153(3) Uani 1 d . . .
H74A H 0.3951 0.7617 0.8522 0.184 Uiso 1 calc . . R
H74B H 0.4172 0.7166 0.9093 0.184 Uiso 1 calc . . R
Cl8 Cl 0.36199(15) 0.53222(10) 0.15506(8) 0.1661(9) Uani 1 d . . .
Cl20 Cl 0.13707(18) 0.52354(10) 0.19329(13) 0.1793(10) Uani 1 d . . .
C69 C 0.2487(4) 0.56425(19) 0.1831(2) 0.0874(13) Uani 1 d . . .
H69A H 0.2783 0.5814 0.2287 0.105 Uiso 1 calc . . R
H69B H 0.2185 0.5911 0.1481 0.105 Uiso 1 calc . . R
O40 O 0.4158(2) 0.62671(17) 0.31821(15) 0.0939(10) Uani 1 d . . .
H40A H 0.4887 0.6307 0.3179 0.141 Uiso 1 d . . G
H40B H 0.4053 0.6252 0.3615 0.141 Uiso 1 d . . G


_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 O3 1.484(2) . ?
P1 C9 1.834(3) . ?
P1 C19 1.815(3) . ?
P1 C31 1.800(3) . ?
P2 O5 1.479(2) . ?
P2 C15 1.820(3) . ?
P2 C24 1.807(3) . ?
P2 C29 1.803(3) . ?
P3 C7 1.813(3) . ?
P3 O10 1.493(2) . ?
P3 C18 1.811(3) . ?
P3 C22 1.794(3) . ?
N1 C13 1.338(3) . ?
N1 C16 1.339(3) . ?
N2 C13 1.340(3) . ?
N2 C17 1.330(3) . ?
N6 C16 1.335(3) . ?
N6 C17 1.336(3) . ?
C7 C11 1.416(3) . ?
C7 C25 1.392(4) . ?
C9 C12 1.417(4) . ?
C9 C26 1.392(4) . ?
C11 C17 1.492(3) . ?
C11 C34 1.389(4) . ?
C12 C13 1.479(4) . ?
C12 C28 1.398(4) . ?
C14 C15 1.403(4) . ?
C14 C16 1.489(3) . ?
C14 C33 1.383(4) . ?
C15 C37 1.398(4) . ?
C18 C32 1.375(4) . ?
C18 C68 1.384(4) . ?
C19 C43 1.396(4) . ?
C19 C48 1.381(4) . ?
C21 C24 1.381(4) . ?
C21 C49 1.380(4) . ?
C22 C41 1.397(4) . ?
C22 C46 1.394(4) . ?
C24 C44 1.376(4) . ?
C25 C36 1.393(4) . ?
C26 C30 1.387(4) . ?
C27 C34 1.387(4) . ?
C27 C36 1.368(4) . ?
C28 C35 1.382(4) . ?
C29 C50 1.397(4) . ?
C29 C56 1.390(5) . ?
C30 C35 1.374(4) . ?
C31 C39 1.386(4) . ?
C31 C42 1.398(4) . ?
C32 C55 1.393(5) . ?
C33 C38 1.391(4) . ?
C37 C45 1.385(4) . ?
C38 C45 1.362(5) . ?
C39 C65 1.397(5) . ?
C41 C52 1.388(5) . ?
C42 C62 1.385(4) . ?
C43 C57 1.363(5) . ?
C44 C63 1.380(4) . ?
C46 C53 1.371(5) . ?
C47 C49 1.377(5) . ?
C47 C63 1.372(5) . ?
C48 C64 1.399(5) . ?
C50 C51 1.378(5) . ?
C51 C66 1.359(6) . ?
C52 C60 1.365(5) . ?
C53 C60 1.375(6) . ?
C54 C62 1.378(6) . ?
C54 C65 1.355(6) . ?
C55 C61 1.335(5) . ?
C56 C67 1.392(5) . ?
C57 C58 1.373(6) . ?
C58 C64 1.358(6) . ?
C59 C61 1.372(6) . ?
C59 C68 1.388(5) . ?
C66 C67 1.366(7) . ?
Cl4 C74 1.648(6) . ?
Cl23 C74 1.786(7) . ?
Cl8 C69 1.710(4) . ?
Cl20 C69 1.696(5) . ?

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 P1 C9 114.66(11) . . ?
O3 P1 C19 109.55(13) . . ?
O3 P1 C31 115.21(13) . . ?
C19 P1 C9 103.54(13) . . ?
C31 P1 C9 109.75(13) . . ?
C31 P1 C19 102.80(13) . . ?
O5 P2 C15 113.77(12) . . ?
O5 P2 C24 112.94(11) . . ?
O5 P2 C29 110.93(14) . . ?
C24 P2 C15 106.96(13) . . ?
C29 P2 C15 105.78(12) . . ?
C29 P2 C24 105.88(14) . . ?
O10 P3 C7 113.07(12) . . ?
O10 P3 C18 110.69(13) . . ?
O10 P3 C22 115.02(13) . . ?
C18 P3 C7 104.44(12) . . ?
C22 P3 C7 108.01(13) . . ?
C22 P3 C18 104.78(13) . . ?
C13 N1 C16 114.6(2) . . ?
C17 N2 C13 115.1(2) . . ?
C16 N6 C17 114.8(2) . . ?
C11 C7 P3 122.32(19) . . ?
C25 C7 P3 119.5(2) . . ?
C25 C7 C11 118.0(2) . . ?
C12 C9 P1 123.8(2) . . ?
C26 C9 P1 117.8(2) . . ?
C26 C9 C12 118.0(2) . . ?
C7 C11 C17 123.4(2) . . ?
C34 C11 C7 119.5(2) . . ?
C34 C11 C17 117.0(2) . . ?
C9 C12 C13 123.9(2) . . ?
C28 C12 C9 119.0(2) . . ?
C28 C12 C13 117.1(2) . . ?
N1 C13 N2 124.9(2) . . ?
N1 C13 C12 117.4(2) . . ?
N2 C13 C12 117.5(2) . . ?
C15 C14 C16 122.3(2) . . ?
C33 C14 C15 120.4(2) . . ?
C33 C14 C16 117.3(2) . . ?
C14 C15 P2 122.10(19) . . ?
C37 C15 P2 120.0(2) . . ?
C37 C15 C14 117.7(2) . . ?
N1 C16 C14 116.8(2) . . ?
N6 C16 N1 125.3(2) . . ?
N6 C16 C14 117.9(2) . . ?
N2 C17 N6 125.1(2) . . ?
N2 C17 C11 118.4(2) . . ?
N6 C17 C11 116.4(2) . . ?
C32 C18 P3 117.4(2) . . ?
C32 C18 C68 119.2(3) . . ?
C68 C18 P3 123.4(2) . . ?
C43 C19 P1 117.6(2) . . ?
C48 C19 P1 123.4(2) . . ?
C48 C19 C43 119.1(3) . . ?
C49 C21 C24 120.7(3) . . ?
C41 C22 P3 123.3(2) . . ?
C46 C22 P3 118.1(2) . . ?
C46 C22 C41 118.6(3) . . ?
C21 C24 P2 117.5(2) . . ?
C44 C24 P2 123.0(2) . . ?
C44 C24 C21 119.0(3) . . ?
C7 C25 C36 121.4(3) . . ?
C30 C26 C9 122.0(3) . . ?
C36 C27 C34 119.5(3) . . ?
C35 C28 C12 121.4(3) . . ?
C50 C29 P2 123.1(3) . . ?
C56 C29 P2 117.9(2) . . ?
C56 C29 C50 119.0(3) . . ?
C35 C30 C26 119.7(3) . . ?
C39 C31 P1 123.7(2) . . ?
C39 C31 C42 119.1(3) . . ?
C42 C31 P1 116.9(2) . . ?
C18 C32 C55 120.3(3) . . ?
C14 C33 C38 120.4(3) . . ?
C27 C34 C11 121.3(3) . . ?
C30 C35 C28 119.8(3) . . ?
C27 C36 C25 120.3(3) . . ?
C45 C37 C15 121.3(3) . . ?
C45 C38 C33 120.0(3) . . ?
C31 C39 C65 120.0(3) . . ?
C52 C41 C22 119.6(3) . . ?
C62 C42 C31 119.7(3) . . ?
C57 C43 C19 120.7(3) . . ?
C24 C44 C63 120.6(3) . . ?
C38 C45 C37 120.1(3) . . ?
C53 C46 C22 120.7(3) . . ?
C63 C47 C49 120.2(3) . . ?
C19 C48 C64 119.1(3) . . ?
C47 C49 C21 119.6(3) . . ?
C51 C50 C29 119.8(4) . . ?
C66 C51 C50 120.7(4) . . ?
C60 C52 C41 120.6(4) . . ?
C46 C53 C60 120.2(4) . . ?
C65 C54 C62 120.5(3) . . ?
C61 C55 C32 120.1(4) . . ?
C29 C56 C67 119.7(4) . . ?
C43 C57 C58 120.2(4) . . ?
C64 C58 C57 120.2(3) . . ?
C61 C59 C68 120.2(4) . . ?
C52 C60 C53 120.2(3) . . ?
C55 C61 C59 120.8(3) . . ?
C54 C62 C42 120.4(4) . . ?
C47 C63 C44 119.9(4) . . ?
C58 C64 C48 120.7(3) . . ?
C54 C65 C39 120.4(4) . . ?
C51 C66 C67 120.6(4) . . ?
C66 C67 C56 120.2(4) . . ?
C18 C68 C59 119.4(4) . . ?
Cl4 C74 Cl23 114.0(3) . . ?
Cl20 C69 Cl8 112.7(3) . . ?

####################################################################### 
# 
# 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_xcalibur
_database_code_depnum_ccdc_archive 'CCDC 1041328'
_audit_update_record             
;
2014-12-24 deposited with the CCDC.
2015-04-06 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu May 15 17:56:02 2014'
;
_audit_creation_method           
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_cell_length_a                   33.603(2)
_cell_length_b                   23.3276(9)
_cell_length_c                   33.068(2)
_cell_angle_alpha                90.0
_cell_angle_beta                 121.583(10)
_cell_angle_gamma                90.0
_cell_volume                     22081(2)
_cell_measurement_reflns_used    8650
_cell_measurement_theta_min      3.0155
_cell_measurement_theta_max      28.8441
_cell_oxdiff_length_a            33.6206(15)
_cell_oxdiff_length_b            23.3118(6)
_cell_oxdiff_length_c            33.0577(15)
_cell_oxdiff_angle_alpha         90.033(3)
_cell_oxdiff_angle_beta          121.541(5)
_cell_oxdiff_angle_gamma         90.034(3)
_cell_oxdiff_volume              22081(2)
_cell_oxdiff_measurement_reflns_used 8667
_exptl_absorpt_correction_T_min  0.90450
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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, Eos'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_reflns_number            48697
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.1403
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         3.0155
_diffrn_reflns_theta_max         28.8441
_diffrn_orient_matrix_UB_11      0.0223471000
_diffrn_orient_matrix_UB_12      0.0034026000
_diffrn_orient_matrix_UB_13      0.0029742000
_diffrn_orient_matrix_UB_21      0.0106046000
_diffrn_orient_matrix_UB_22      -0.0043365000
_diffrn_orient_matrix_UB_23      0.0247838000
_diffrn_orient_matrix_UB_31      0.0009784000
_diffrn_orient_matrix_UB_32      -0.0299231000
_diffrn_orient_matrix_UB_33      -0.0032810000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -7.00   45.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.8890   57.0000 -120.0000 52

#__ type_ start__ end____ width___ exp.time_
  2 omega  -80.00   49.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.8890   19.0000 -150.0000 129

#__ type_ start__ end____ width___ exp.time_
  3 omega  -86.00  -30.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.8890  141.0000    3.0000 56

;
_diffrn_measurement_method       'ω scans'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_theta     26.32
_reflns_odcompleteness_iscentric 1
_chemical_name_common            'mTPOTZ and oTPOTZ'
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      298
_exptl_crystal_recrystallization_method 'Vapour Deposition'
_exptl_crystal_preparation       Luminescent
