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

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

data_2a
_database_code_depnum_ccdc_archive 'CCDC 1978287'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne
France
;
_audit_update_record             
;
2020-01-16 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_audit_creation_date             2019-10-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H78 N2 O2 P2 Zr'
_chemical_formula_sum            'C68 H78 N2 O2 P2 Zr'
_chemical_formula_weight         1108.48
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   18.8787(11)
_cell_length_b                   15.7181(9)
_cell_length_c                   27.6141(15)
_cell_angle_alpha                90
_cell_angle_beta                 105.6510(10)
_cell_angle_gamma                90
_cell_volume                     7890.3(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    110
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      2.49
_shelx_estimated_absorpt_T_max   0.948
_shelx_estimated_absorpt_T_min   0.948
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.8246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;    
 SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
 wR2(int) was 0.0540 before and 0.0507 after correction. 
 The Ratio of minimum to maximum transmission is 0.9565. 
 The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.933
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            71040
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.735
_diffrn_reflns_theta_min         3.064
_diffrn_ambient_temperature      110
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       "φ and ω scans'"
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8126
_reflns_number_total             10194
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XT (Sheldrick, 2015))'
_refine_diff_density_max         1.739
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         10194
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0514
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0851P)²+10.8607P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1497
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Free rotating group:
 C19(C20,C21,C22)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C13(H13), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.52565(16) 0.75538(14) 0.73337(9) 0.0318(5) Uani 1 1 d . . . . .
H1A H 0.512729 0.802368 0.708682 0.038 Uiso 1 1 calc R . . . .
H1B H 0.576906 0.763937 0.753918 0.038 Uiso 1 1 calc R . . . .
C2 C 0.37712(11) 0.51499(16) 0.72989(8) 0.0252(4) Uani 1 1 d . . . . .
H2A H 0.376332 0.453746 0.721378 0.030 Uiso 1 1 calc R . . . .
H2B H 0.359627 0.520203 0.760480 0.030 Uiso 1 1 calc R . . . .
C3 C 0.32401(12) 0.55879(17) 0.68861(9) 0.0297(5) Uani 1 1 d . . . . .
C4 C 0.28498(19) 0.6291(3) 0.69766(10) 0.0609(11) Uani 1 1 d . . . . .
H4 H 0.295504 0.651354 0.730820 0.073 Uiso 1 1 calc R . . . .
C5 C 0.2312(2) 0.6678(3) 0.65992(13) 0.0905(18) Uani 1 1 d . . . . .
H5 H 0.204949 0.715179 0.667626 0.109 Uiso 1 1 calc R . . . .
C6 C 0.21548(19) 0.6379(3) 0.61096(11) 0.0692(12) Uani 1 1 d . . . . .
H6 H 0.177579 0.663221 0.585183 0.083 Uiso 1 1 calc R . . . .
C7 C 0.25558(15) 0.5711(2) 0.60037(9) 0.0415(7) Uani 1 1 d . . . . .
H7 H 0.246622 0.551164 0.566779 0.050 Uiso 1 1 calc R . . . .
C8 C 0.30888(13) 0.53264(17) 0.63826(9) 0.0293(5) Uani 1 1 d . . . . .
H8 H 0.336306 0.486855 0.629966 0.035 Uiso 1 1 calc R . . . .
C9 C 0.52966(11) 0.49667(14) 0.64769(7) 0.0197(4) Uani 1 1 d . . . . .
C10 C 0.55426(12) 0.57173(14) 0.63038(8) 0.0232(4) Uani 1 1 d . . . . .
C11 C 0.58962(14) 0.57025(17) 0.59139(9) 0.0318(5) Uani 1 1 d . . . . .
H11 H 0.605144 0.622251 0.580009 0.038 Uiso 1 1 calc R . . . .
C12 C 0.60200(13) 0.49535(18) 0.56964(8) 0.0321(5) Uani 1 1 d . . . . .
C13 C 0.57810(13) 0.42109(17) 0.58747(9) 0.0290(5) Uani 1 1 d . . . . .
H13 H 0.587059 0.368764 0.572943 0.035 Uiso 1 1 calc R . . . .
C14 C 0.54190(12) 0.41809(14) 0.62518(8) 0.0232(4) Uani 1 1 d . . . . .
C15 C 0.51731(13) 0.33245(15) 0.64260(9) 0.0290(5) Uani 1 1 d . . . . .
C16 C 0.43490(14) 0.33389(16) 0.63891(11) 0.0361(6) Uani 1 1 d . . . . .
H16A H 0.420375 0.279226 0.650380 0.054 Uiso 1 1 calc GR . . . .
H16B H 0.407022 0.343646 0.603908 0.054 Uiso 1 1 calc GR . . . .
H16C H 0.424570 0.379704 0.660097 0.054 Uiso 1 1 calc GR . . . .
C17 C 0.56089(16) 0.31490(17) 0.69704(10) 0.0376(6) Uani 1 1 d . . . . .
H17A H 0.613667 0.315997 0.699574 0.056 Uiso 1 1 calc GR . . . .
H17B H 0.547422 0.258832 0.707308 0.056 Uiso 1 1 calc GR . . . .
H17C H 0.549456 0.358630 0.719083 0.056 Uiso 1 1 calc GR . . . .
C18 C 0.53038(18) 0.25790(18) 0.61026(12) 0.0446(7) Uani 1 1 d . . . . .
H18A H 0.583168 0.252477 0.613472 0.067 Uiso 1 1 calc GR . . . .
H18B H 0.504159 0.268345 0.574989 0.067 Uiso 1 1 calc GR . . . .
H18C H 0.512185 0.205238 0.621640 0.067 Uiso 1 1 calc GR . . . .
C19 C 0.64254(11) 0.49422(17) 0.52844(7) 0.0407(7) Uani 1 1 d . . . A -1
C20 C 0.6378(3) 0.5798(2) 0.50137(17) 0.179(4) Uani 1 1 d G . . A -1
H20A H 0.585993 0.595191 0.487185 0.269 Uiso 1 1 calc GR . . A -1
H20B H 0.662024 0.575410 0.474252 0.269 Uiso 1 1 calc GR . . A -1
H20C H 0.662194 0.623637 0.525323 0.269 Uiso 1 1 calc GR . . A -1
C21 C 0.72359(14) 0.4739(4) 0.55299(12) 0.139(3) Uani 1 1 d G . . A -1
H21A H 0.744172 0.516434 0.578924 0.208 Uiso 1 1 calc GR . . A -1
H21B H 0.750827 0.475009 0.527393 0.208 Uiso 1 1 calc GR . . A -1
H21C H 0.727657 0.417302 0.568363 0.208 Uiso 1 1 calc GR . . A -1
C22 C 0.6107(3) 0.4252(3) 0.48961(16) 0.237(6) Uani 1 1 d G . . A -1
H22A H 0.635437 0.371002 0.500678 0.355 Uiso 1 1 calc GR . . A -1
H22B H 0.618261 0.441185 0.457076 0.355 Uiso 1 1 calc GR . . A -1
H22C H 0.557875 0.419160 0.486202 0.355 Uiso 1 1 calc GR . . A -1
C23 C 0.47021(17) 0.72991(16) 0.60635(9) 0.0352(6) Uani 1 1 d . . . . .
C24 C 0.39939(17) 0.73323(17) 0.61161(10) 0.0415(7) Uani 1 1 d . . . . .
H24 H 0.388917 0.709003 0.640431 0.050 Uiso 1 1 calc R . . . .
C25 C 0.3432(2) 0.7721(2) 0.57471(12) 0.0604(10) Uani 1 1 d . . . . .
H25 H 0.294718 0.774131 0.578463 0.073 Uiso 1 1 calc R . . . .
C26 C 0.3581(3) 0.8072(3) 0.53305(12) 0.0716(12) Uani 1 1 d . . . . .
H26 H 0.319882 0.833969 0.508173 0.086 Uiso 1 1 calc R . . . .
C27 C 0.4282(3) 0.8040(3) 0.52708(11) 0.0709(12) Uani 1 1 d . . . . .
H27 H 0.437838 0.828157 0.497978 0.085 Uiso 1 1 calc R . . . .
C28 C 0.4852(2) 0.7654(2) 0.56356(10) 0.0532(8) Uani 1 1 d . . . . .
H28 H 0.533553 0.763192 0.559402 0.064 Uiso 1 1 calc R . . . .
C29 C 0.62427(16) 0.73401(17) 0.65938(9) 0.0349(6) Uani 1 1 d . . . . .
C30 C 0.6225(2) 0.82296(19) 0.65548(11) 0.0485(8) Uani 1 1 d . . . . .
H30 H 0.576721 0.852014 0.646866 0.058 Uiso 1 1 calc R . . . .
C31 C 0.6875(2) 0.8685(2) 0.66418(15) 0.0669(11) Uani 1 1 d . . . . .
H31 H 0.686280 0.928808 0.661741 0.080 Uiso 1 1 calc R . . . .
C32 C 0.7535(2) 0.8268(3) 0.67624(14) 0.0711(13) Uani 1 1 d . . . . .
H32 H 0.797632 0.858820 0.681808 0.085 Uiso 1 1 calc R . . . .
C33 C 0.7575(2) 0.7379(3) 0.68062(12) 0.0588(10) Uani 1 1 d . . . . .
H33 H 0.803658 0.709619 0.689221 0.071 Uiso 1 1 calc R . . . .
C34 C 0.69205(16) 0.6923(2) 0.67202(9) 0.0412(7) Uani 1 1 d . . . . .
H34 H 0.693557 0.632079 0.674794 0.049 Uiso 1 1 calc R . . . .
N N 0.51914(11) 0.67270(11) 0.70677(6) 0.0224(4) Uani 1 1 d . . . . .
O O 0.49593(8) 0.49877(9) 0.68381(5) 0.0186(3) Uani 1 1 d . . . . .
P P 0.54054(3) 0.67487(4) 0.65380(2) 0.02398(14) Uani 1 1 d . . . . .
Zr Zr 0.500000 0.56130(2) 0.750000 0.01528(9) Uani 1 2 d S T P . .


_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
C1 C1 1.504(5) 2_656 ?
C1 N 1.482(3) . ?
C2 C3 1.470(3) . ?
C2 Zr 2.350(2) . ?
C3 C4 1.387(4) . ?
C3 C8 1.403(3) . ?
C4 C5 1.384(4) . ?
C5 C6 1.386(5) . ?
C6 C7 1.371(4) . ?
C7 C8 1.380(4) . ?
C9 C10 1.398(3) . ?
C9 C14 1.429(3) . ?
C9 O 1.321(2) . ?
C10 C11 1.412(3) . ?
C10 P 1.790(2) . ?
C11 C12 1.370(4) . ?
C12 C13 1.389(4) . ?
C12 C19 1.533(3) . ?
C13 C14 1.392(3) . ?
C14 C15 1.543(3) . ?
C15 C16 1.532(3) . ?
C15 C17 1.532(4) . ?
C15 C18 1.533(3) . ?
C19 C20 1.5298 . ?
C19 C21 1.5306 . ?
C19 C22 1.5302 . ?
C23 C24 1.384(4) . ?
C23 C28 1.403(4) . ?
C23 P 1.814(3) . ?
C24 C25 1.397(4) . ?
C25 C26 1.372(5) . ?
C26 C27 1.377(6) . ?
C27 C28 1.399(5) . ?
C29 C30 1.402(4) . ?
C29 C34 1.395(4) . ?
C29 P 1.804(3) . ?
C30 C31 1.385(5) . ?
C31 C32 1.366(6) . ?
C32 C33 1.403(6) . ?
C33 C34 1.392(4) . ?
N P 1.6194(18) . ?
N Zr 2.2033(17) . ?
O Zr 2.0582(14) . ?

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
N C1 C1 108.77(16) . 2_656 ?
C3 C2 Zr 117.48(16) . . ?
C4 C3 C2 121.2(2) . . ?
C4 C3 C8 115.8(2) . . ?
C8 C3 C2 123.0(2) . . ?
C5 C4 C3 122.1(3) . . ?
C4 C5 C6 120.4(3) . . ?
C7 C6 C5 118.8(3) . . ?
C6 C7 C8 120.3(3) . . ?
C7 C8 C3 122.3(2) . . ?
C10 C9 C14 118.23(19) . . ?
O C9 C10 120.61(19) . . ?
O C9 C14 121.16(19) . . ?
C9 C10 C11 121.0(2) . . ?
C9 C10 P 123.16(16) . . ?
C11 C10 P 115.77(17) . . ?
C12 C11 C10 121.3(2) . . ?
C11 C12 C13 117.2(2) . . ?
C11 C12 C19 120.9(2) . . ?
C13 C12 C19 121.9(2) . . ?
C12 C13 C14 124.5(2) . . ?
C9 C14 C15 121.41(19) . . ?
C13 C14 C9 117.8(2) . . ?
C13 C14 C15 120.8(2) . . ?
C16 C15 C14 110.62(19) . . ?
C16 C15 C17 109.6(2) . . ?
C16 C15 C18 107.0(2) . . ?
C17 C15 C14 109.6(2) . . ?
C17 C15 C18 107.8(2) . . ?
C18 C15 C14 112.1(2) . . ?
C20 C19 C12 112.1(2) . . ?
C20 C19 C21 108.7 . . ?
C20 C19 C22 108.7 . . ?
C21 C19 C12 108.26(18) . . ?
C22 C19 C12 110.34(18) . . ?
C22 C19 C21 108.6 . . ?
C24 C23 C28 119.6(3) . . ?
C24 C23 P 118.80(19) . . ?
C28 C23 P 121.5(3) . . ?
C23 C24 C25 120.3(3) . . ?
C26 C25 C24 120.1(4) . . ?
C25 C26 C27 120.4(3) . . ?
C26 C27 C28 120.5(3) . . ?
C27 C28 C23 119.2(4) . . ?
C30 C29 P 120.4(2) . . ?
C34 C29 C30 119.2(3) . . ?
C34 C29 P 120.2(2) . . ?
C31 C30 C29 120.1(4) . . ?
C32 C31 C30 120.1(3) . . ?
C31 C32 C33 121.6(3) . . ?
C34 C33 C32 118.2(4) . . ?
C33 C34 C29 120.8(3) . . ?
C1 N P 114.94(14) . . ?
C1 N Zr 115.61(13) . . ?
P N Zr 128.57(10) . . ?
C9 O Zr 140.58(13) . . ?
C10 P C23 108.66(11) . . ?
C10 P C29 106.78(12) . . ?
C29 P C23 105.64(13) . . ?
N P C10 113.76(10) . . ?
N P C23 110.50(12) . . ?
N P C29 111.11(10) . . ?
C2 Zr C2 143.92(12) 2_656 . ?
N Zr C2 114.44(8) . . ?
N Zr C2 94.50(8) . 2_656 ?
N Zr C2 94.50(8) 2_656 . ?
N Zr C2 114.44(8) 2_656 2_656 ?
N Zr N 74.74(9) 2_656 . ?
O Zr C2 81.96(7) . 2_656 ?
O Zr C2 81.04(7) . . ?
O Zr C2 81.95(7) 2_656 . ?
O Zr C2 81.04(7) 2_656 2_656 ?
O Zr N 82.57(6) 2_656 2_656 ?
O Zr N 152.66(6) . 2_656 ?
O Zr N 152.66(6) 2_656 . ?
O Zr N 82.57(6) . . ?
O Zr O 122.96(8) . 2_656 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.030 -0.379 -0.553 2895.4 1218.6 ?


_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT213_2a                  
;
PROBLEM: Atom C20       has ADP max/min Ratio .....   6.1 prolat
RESPONSE: The position of this tert-butyl group fluctuates around 
an average position of a few degrees and since this disorder seems 
rather continuous than discrete we simply let the anisotropic 
displacement parameters taking account for that.
;
_vrf_PLAT222_2a                  
;
PROBLEM: Non-Solv.  Resd 1  H   Uiso(max)/Uiso(min) Range       10.0 Ratio 
RESPONSE: The position of this tert-butyl group fluctuates around 
an average position of a few degrees and since this disorder seems 
rather continuous than discrete we simply let the anisotropic 
displacement parameters taking account for that.
;
_vrf_PLAT241_2a                  
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         C5 Check 
RESPONSE: The position of this tert-butyl group fluctuates around 
an average position of a few degrees and since this disorder seems 
rather continuous than discrete we simply let the anisotropic 
displacement parameters taking account for that.
;
_vrf_PLAT250_2a                  
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.5 Note  
RESPONSE: The position of this tert-butyl group fluctuates around 
an average position of a few degrees and since this disorder seems 
rather continuous than discrete we simply let the anisotropic 
displacement parameters taking account for that.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_2Cpp
_database_code_depnum_ccdc_archive 'CCDC 1978294'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne
France
;
_audit_update_record             
;
2020-01-16 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_audit_creation_date             2019-11-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C62 H72 N2 O2 P2 Zr, 3[C6H14]'
_chemical_formula_sum            'C80 H114 N2 O2 P2 Zr'
_chemical_formula_weight         1288.89
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.2872(7)
_cell_length_b                   16.4819(10)
_cell_length_c                   16.7752(9)
_cell_angle_alpha                69.077(2)
_cell_angle_beta                 75.579(3)
_cell_angle_gamma                80.202(3)
_cell_volume                     3310.0(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    115
_cell_measurement_theta_max      23.66
_cell_measurement_theta_min      2.17
_shelx_estimated_absorpt_T_max   0.969
_shelx_estimated_absorpt_T_min   0.937
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.8029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0619 before and 0.0552 after correction. The Ratio of minimum to maximum transmission is 0.9313. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_unetI/netI     0.0781
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            86942
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.615
_diffrn_reflns_theta_min         2.270
_diffrn_ambient_temperature      115.0
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10238
_reflns_number_total             15215
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL n/a (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         1.402
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         15215
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0531
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0840P)²+1.1464P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1546
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained planarity
 C5, C4, C9, C8, C7, C6, C14A
 with sigma of 0.02
3. Others
 Sof(C14A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C16A)=Sof(H16A)=
 Sof(H16B)=Sof(H16C)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=1-FVAR(1)
 Sof(C14)=Sof(C15)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=Sof(C17)=Sof(H17D)=Sof(H17E)=Sof(H17F)=FVAR(1)
4.a Free rotating group:
 C14A(C17A,C16A,C15A), C14(C15,C16,C17)
4.b Ternary CH refined with riding coordinates:
 C1(H1)
4.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C56(H56A,H56B)
4.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
 C26(H26), C27(H27), C28(H28), C29(H29), C33(H33), C35(H35), C45(H45), C46(H46),
  C47(H47), C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54),
 C55(H55), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62)
4.e Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C43(H43A,H43B,H43C), C17A(H17A,H17B,H17C), C16A(H16A,H16B,H16C),
 C15A(H15A,H15B,H15C), C15(H15D,H15E,H15F), C16(H16D,H16E,H16F), C17(H17D,H17E,
 H17F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr Zr 0.58981(2) 0.81509(2) 0.32677(2) 0.01814(9) Uani 1 1 d . . . . .
P1 P 0.79017(6) 0.67221(5) 0.40278(5) 0.01595(16) Uani 1 1 d . . . . .
P2 P 0.50559(6) 0.77850(5) 0.17128(5) 0.01643(16) Uani 1 1 d . . . . .
O1 O 0.58291(16) 0.75815(13) 0.45966(12) 0.0203(4) Uani 1 1 d . . . . .
O2 O 0.43119(16) 0.83033(13) 0.33153(13) 0.0219(5) Uani 1 1 d . . . . .
N1 N 0.7496(2) 0.74293(17) 0.32113(16) 0.0239(6) Uani 1 1 d . . . . .
N2 N 0.60228(19) 0.78462(16) 0.20747(16) 0.0224(6) Uani 1 1 d . . . . .
C57 C 0.6985(2) 0.9857(2) 0.3041(2) 0.0250(7) Uani 1 1 d . . . . .
C1 C 0.6655(3) 0.8551(2) 0.1873(2) 0.0338(8) Uani 1 1 d . . . . .
H1 H 0.640718 0.913692 0.149592 0.041 Uiso 1 1 calc R U . . .
C2 C 0.7825(2) 0.8267(2) 0.16611(19) 0.0264(7) Uani 1 1 d . . . . .
H2A H 0.801526 0.819307 0.108029 0.032 Uiso 1 1 calc R U . . .
H2B H 0.824046 0.871615 0.165331 0.032 Uiso 1 1 calc R U . . .
C3 C 0.8046(3) 0.7424(2) 0.2347(2) 0.0359(8) Uani 1 1 d . . . . .
H3A H 0.782959 0.694192 0.222385 0.043 Uiso 1 1 calc R U . . .
H3B H 0.880561 0.731731 0.233079 0.043 Uiso 1 1 calc R U . . .
C4 C 0.7452(2) 0.69973(15) 0.50055(17) 0.0195(6) Uani 1 1 d . . . . .
C5 C 0.6432(2) 0.73815(17) 0.51842(18) 0.0200(6) Uani 1 1 d . . . . .
C6 C 0.6069(2) 0.75530(18) 0.59864(18) 0.0213(6) Uani 1 1 d . . . . .
C7 C 0.6780(3) 0.7358(2) 0.6529(2) 0.0275(7) Uani 1 1 d . . . . .
H7 H 0.655024 0.748288 0.705963 0.033 Uiso 1 1 calc R U . . .
C8 C 0.7805(3) 0.6993(2) 0.6351(2) 0.0312(8) Uani 1 1 d . . . . .
C9 C 0.8129(2) 0.68132(17) 0.55798(19) 0.0254(7) Uani 1 1 d . . . . .
H9 H 0.881904 0.656181 0.543629 0.030 Uiso 1 1 calc R U . . .
C10 C 0.4949(3) 0.7921(2) 0.62539(19) 0.0247(7) Uani 1 1 d . . . . .
C11 C 0.4756(3) 0.8830(2) 0.5595(2) 0.0322(8) Uani 1 1 d . . . . .
H11A H 0.405433 0.908499 0.578464 0.048 Uiso 1 1 calc R U . . .
H11B H 0.481494 0.878018 0.501995 0.048 Uiso 1 1 calc R U . . .
H11C H 0.527426 0.920563 0.556030 0.048 Uiso 1 1 calc R U . . .
C12 C 0.4184(3) 0.7315(2) 0.6278(2) 0.0351(8) Uani 1 1 d . . . . .
H12A H 0.425286 0.676023 0.674932 0.053 Uiso 1 1 calc R U . . .
H12B H 0.433757 0.720683 0.571970 0.053 Uiso 1 1 calc R U . . .
H12C H 0.346985 0.758743 0.637923 0.053 Uiso 1 1 calc R U . . .
C13 C 0.4719(3) 0.8017(2) 0.7151(2) 0.0357(8) Uani 1 1 d . . . . .
H13A H 0.486467 0.745085 0.758450 0.054 Uiso 1 1 calc R U . . .
H13B H 0.398369 0.822498 0.729991 0.054 Uiso 1 1 calc R U . . .
H13C H 0.516128 0.843777 0.714862 0.054 Uiso 1 1 calc R U . . .
C18 C 0.9305(2) 0.66305(19) 0.38529(18) 0.0212(6) Uani 1 1 d . . . . .
C19 C 0.9765(3) 0.7414(2) 0.3577(2) 0.0310(8) Uani 1 1 d . . . . .
H19 H 0.934720 0.795469 0.344878 0.037 Uiso 1 1 calc R U . . .
C20 C 1.0825(3) 0.7401(3) 0.3491(2) 0.0428(10) Uani 1 1 d . . . . .
H20 H 1.113852 0.793327 0.330037 0.051 Uiso 1 1 calc R U . . .
C21 C 1.1437(3) 0.6613(3) 0.3682(2) 0.0507(12) Uani 1 1 d . . . . .
H21 H 1.216697 0.660656 0.362823 0.061 Uiso 1 1 calc R U . . .
C22 C 1.0994(3) 0.5849(3) 0.3946(2) 0.0448(10) Uani 1 1 d . . . . .
H22 H 1.141852 0.531206 0.407261 0.054 Uiso 1 1 calc R U . . .
C23 C 0.9932(3) 0.5847(2) 0.4033(2) 0.0305(8) Uani 1 1 d . . . . .
H23 H 0.963066 0.531088 0.421532 0.037 Uiso 1 1 calc R U . . .
C24 C 0.7506(3) 0.56493(19) 0.4270(2) 0.0250(7) Uani 1 1 d . . . . .
C25 C 0.6733(3) 0.5315(2) 0.4992(3) 0.0382(9) Uani 1 1 d . . . . .
H25 H 0.642904 0.564256 0.537103 0.046 Uiso 1 1 calc R U . . .
C26 C 0.6400(4) 0.4505(3) 0.5162(4) 0.0653(15) Uani 1 1 d . . . . .
H26 H 0.586641 0.427891 0.565474 0.078 Uiso 1 1 calc R U . . .
C27 C 0.6847(5) 0.4030(3) 0.4615(5) 0.080(2) Uani 1 1 d . . . . .
H27 H 0.662621 0.347202 0.473695 0.096 Uiso 1 1 calc R U . . .
C28 C 0.7605(5) 0.4353(3) 0.3899(4) 0.0689(16) Uani 1 1 d . . . . .
H28 H 0.790412 0.401943 0.352481 0.083 Uiso 1 1 calc R U . . .
C29 C 0.7944(3) 0.5170(2) 0.3711(3) 0.0422(10) Uani 1 1 d . . . . .
H29 H 0.846679 0.539681 0.320951 0.051 Uiso 1 1 calc R U . . .
C30 C 0.3889(2) 0.84422(18) 0.19736(18) 0.0191(6) Uani 1 1 d . . . . .
C31 C 0.3640(2) 0.86022(18) 0.27734(18) 0.0182(6) Uani 1 1 d . . . . .
C32 C 0.2674(2) 0.90745(18) 0.29910(18) 0.0189(6) Uani 1 1 d . . . . .
C33 C 0.2041(2) 0.93814(19) 0.23817(19) 0.0208(6) Uani 1 1 d . . . . .
H33 H 0.140443 0.971389 0.251729 0.025 Uiso 1 1 calc R U . . .
C34 C 0.2275(2) 0.92344(18) 0.15786(18) 0.0192(6) Uani 1 1 d . . . . .
C35 C 0.3198(2) 0.87592(18) 0.13914(18) 0.0179(6) Uani 1 1 d . . . . .
H35 H 0.337761 0.864017 0.085690 0.021 Uiso 1 1 calc R U . . .
C36 C 0.2342(2) 0.9259(2) 0.38623(19) 0.0240(7) Uani 1 1 d . . . . .
C37 C 0.1226(3) 0.9686(3) 0.3992(2) 0.0354(8) Uani 1 1 d . . . . .
H37A H 0.117248 1.024183 0.351978 0.053 Uiso 1 1 calc R U . . .
H37B H 0.104547 0.979001 0.455272 0.053 Uiso 1 1 calc R U . . .
H37C H 0.074499 0.929891 0.398733 0.053 Uiso 1 1 calc R U . . .
C38 C 0.3063(3) 0.9891(2) 0.3869(2) 0.0293(7) Uani 1 1 d . . . . .
H38A H 0.378859 0.963843 0.378093 0.044 Uiso 1 1 calc R U . . .
H38B H 0.287387 0.999232 0.443149 0.044 Uiso 1 1 calc R U . . .
H38C H 0.298814 1.044612 0.339978 0.044 Uiso 1 1 calc R U . . .
C39 C 0.2386(3) 0.8411(2) 0.4638(2) 0.0333(8) Uani 1 1 d . . . . .
H39A H 0.193141 0.800901 0.462258 0.050 Uiso 1 1 calc R U . . .
H39B H 0.215115 0.854219 0.518427 0.050 Uiso 1 1 calc R U . . .
H39C H 0.310500 0.813943 0.460203 0.050 Uiso 1 1 calc R U . . .
C40 C 0.1501(2) 0.9593(2) 0.09611(19) 0.0240(7) Uani 1 1 d . . . . .
C41 C 0.1254(3) 1.0579(2) 0.0782(2) 0.0300(8) Uani 1 1 d . . . . .
H41A H 0.094763 1.068976 0.133310 0.045 Uiso 1 1 calc R U . . .
H41B H 0.075804 1.080663 0.039128 0.045 Uiso 1 1 calc R U . . .
H41C H 0.189806 1.087029 0.050836 0.045 Uiso 1 1 calc R U . . .
C42 C 0.0493(3) 0.9134(2) 0.1391(2) 0.0304(8) Uani 1 1 d . . . . .
H42A H 0.064938 0.850708 0.149102 0.046 Uiso 1 1 calc R U . . .
H42B H -0.001062 0.937162 0.100741 0.046 Uiso 1 1 calc R U . . .
H42C H 0.019596 0.923153 0.194967 0.046 Uiso 1 1 calc R U . . .
C43 C 0.1956(3) 0.9438(2) 0.0085(2) 0.0341(8) Uani 1 1 d . . . . .
H43A H 0.261383 0.970965 -0.018312 0.051 Uiso 1 1 calc R U . . .
H43B H 0.145964 0.969611 -0.030288 0.051 Uiso 1 1 calc R U . . .
H43C H 0.208406 0.880992 0.018350 0.051 Uiso 1 1 calc R U . . .
C44 C 0.4739(2) 0.66690(19) 0.21647(19) 0.0225(6) Uani 1 1 d . . . . .
C45 C 0.3790(3) 0.6445(2) 0.2134(2) 0.0348(8) Uani 1 1 d . . . . .
H45 H 0.327956 0.688969 0.190676 0.042 Uiso 1 1 calc R U . . .
C46 C 0.3585(3) 0.5580(2) 0.2433(3) 0.0405(9) Uani 1 1 d . . . . .
H46 H 0.293767 0.543137 0.240386 0.049 Uiso 1 1 calc R U . . .
C47 C 0.4314(3) 0.4938(2) 0.2770(3) 0.0494(11) Uani 1 1 d . . . . .
H47 H 0.417602 0.434335 0.297025 0.059 Uiso 1 1 calc R U . . .
C48 C 0.5250(4) 0.5156(2) 0.2820(3) 0.0627(14) Uani 1 1 d . . . . .
H48 H 0.575121 0.470997 0.306107 0.075 Uiso 1 1 calc R U . . .
C49 C 0.5463(3) 0.6019(2) 0.2520(2) 0.0392(9) Uani 1 1 d . . . . .
H49 H 0.610727 0.616466 0.255800 0.047 Uiso 1 1 calc R U . . .
C50 C 0.5343(2) 0.80597(19) 0.05394(18) 0.0186(6) Uani 1 1 d . . . . .
C51 C 0.5594(3) 0.8887(2) 0.0026(2) 0.0290(8) Uani 1 1 d . . . . .
H51 H 0.558532 0.930832 0.029362 0.035 Uiso 1 1 calc R U . . .
C52 C 0.5859(3) 0.9121(2) -0.0877(2) 0.0292(7) Uani 1 1 d . . . . .
H52 H 0.604569 0.969250 -0.122142 0.035 Uiso 1 1 calc R U . . .
C53 C 0.5849(3) 0.8525(3) -0.1263(2) 0.0442(10) Uani 1 1 d . . . . .
H53 H 0.600760 0.868742 -0.188069 0.053 Uiso 1 1 calc R U . . .
C54 C 0.5609(5) 0.7682(3) -0.0760(3) 0.0689(16) Uani 1 1 d . . . . .
H54 H 0.561589 0.726473 -0.103249 0.083 Uiso 1 1 calc R U . . .
C55 C 0.5360(4) 0.7451(2) 0.0140(2) 0.0454(10) Uani 1 1 d . . . . .
H55 H 0.520042 0.687276 0.048566 0.054 Uiso 1 1 calc R U . . .
C56 C 0.5945(3) 0.95646(19) 0.3159(2) 0.0265(7) Uani 1 1 d . . . . .
H56A H 0.562755 0.994599 0.266197 0.032 Uiso 1 1 calc R U . . .
H56B H 0.549912 0.965761 0.369345 0.032 Uiso 1 1 calc R U . . .
C58 C 0.7495(3) 1.0403(2) 0.2243(2) 0.0314(8) Uani 1 1 d . . . . .
H58 H 0.718115 1.057428 0.175016 0.038 Uiso 1 1 calc R U . . .
C59 C 0.8434(3) 1.0699(3) 0.2154(3) 0.0437(9) Uani 1 1 d . . . . .
H59 H 0.875872 1.107352 0.160456 0.052 Uiso 1 1 calc R U . . .
C60 C 0.8913(3) 1.0452(3) 0.2865(3) 0.0476(10) Uani 1 1 d . . . . .
H60 H 0.955890 1.066276 0.280805 0.057 Uiso 1 1 calc R U . . .
C61 C 0.8438(3) 0.9897(3) 0.3652(2) 0.0405(9) Uani 1 1 d . . . . .
H61 H 0.876745 0.971472 0.413692 0.049 Uiso 1 1 calc R U . . .
C62 C 0.7493(3) 0.9604(2) 0.3744(2) 0.0292(7) Uani 1 1 d . . . . .
H62 H 0.717742 0.922399 0.429345 0.035 Uiso 1 1 calc R U . . .
C14A C 0.8627(8) 0.6873(6) 0.6916(7) 0.033(6) Uiso 0.261(6) 1 d G . P A 2
C17A C 0.9035(13) 0.5904(6) 0.7227(10) 0.062(6) Uiso 0.261(6) 1 d G . P A 2
H17A H 0.923992 0.569027 0.672865 0.094 Uiso 0.261(6) 1 calc R U P A 2
H17B H 0.848383 0.556719 0.766203 0.094 Uiso 0.261(6) 1 calc R U P A 2
H17C H 0.964024 0.583792 0.748666 0.094 Uiso 0.261(6) 1 calc R U P A 2
C16A C 0.8143(13) 0.7170(10) 0.7712(9) 0.080(7) Uiso 0.261(6) 1 d G . P A 2
H16A H 0.864363 0.701943 0.809493 0.119 Uiso 0.261(6) 1 calc R U P A 2
H16B H 0.750802 0.687729 0.803153 0.119 Uiso 0.261(6) 1 calc R U P A 2
H16C H 0.796814 0.780290 0.751566 0.119 Uiso 0.261(6) 1 calc R U P A 2
C15A C 0.9538(11) 0.7420(8) 0.6348(8) 0.054(5) Uiso 0.261(6) 1 d G . P A 2
H15A H 0.927219 0.803372 0.612405 0.081 Uiso 0.261(6) 1 calc R U P A 2
H15B H 0.987007 0.721044 0.585779 0.081 Uiso 0.261(6) 1 calc R U P A 2
H15C H 1.005014 0.736592 0.669891 0.081 Uiso 0.261(6) 1 calc R U P A 2
C14 C 0.8510(3) 0.6799(2) 0.7021(2) 0.047(3) Uani 0.739(6) 1 d G . P A 1
C15 C 0.9573(4) 0.6352(4) 0.6709(3) 0.080(3) Uani 0.739(6) 1 d G . P A 1
H15D H 0.990288 0.672712 0.613441 0.120 Uiso 0.739(6) 1 calc R U P A 1
H15E H 0.947276 0.579280 0.667029 0.120 Uiso 0.739(6) 1 calc R U P A 1
H15F H 1.002222 0.625062 0.712521 0.120 Uiso 0.739(6) 1 calc R U P A 1
C16 C 0.7991(4) 0.6209(3) 0.7922(3) 0.062(2) Uani 0.739(6) 1 d G . P A 1
H16D H 0.847278 0.605036 0.832162 0.094 Uiso 0.739(6) 1 calc R U P A 1
H16E H 0.781566 0.567865 0.786842 0.094 Uiso 0.739(6) 1 calc R U P A 1
H16F H 0.735249 0.652078 0.814998 0.094 Uiso 0.739(6) 1 calc R U P A 1
C17 C 0.8668(4) 0.7675(2) 0.7084(4) 0.062(2) Uani 0.739(6) 1 d G . P A 1
H17D H 0.800314 0.792609 0.734963 0.093 Uiso 0.739(6) 1 calc R U P A 1
H17E H 0.891816 0.807653 0.649916 0.093 Uiso 0.739(6) 1 calc R U P A 1
H17F H 0.918252 0.758089 0.744471 0.093 Uiso 0.739(6) 1 calc R U P A 1


_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
Zr O1 2.0717(19) . ?
Zr O2 2.064(2) . ?
Zr N1 2.248(3) . ?
Zr N2 2.193(2) . ?
Zr C1 2.207(4) . ?
Zr C56 2.282(3) . ?
P1 N1 1.593(2) . ?
P1 C4 1.790(3) . ?
P1 C18 1.803(3) . ?
P1 C24 1.807(3) . ?
P2 N2 1.583(2) . ?
P2 C30 1.789(3) . ?
P2 C44 1.801(3) . ?
P2 C50 1.809(3) . ?
O1 C5 1.339(3) . ?
O2 C31 1.342(3) . ?
N1 C3 1.455(4) . ?
N2 C1 1.442(4) . ?
C57 C56 1.484(4) . ?
C57 C58 1.398(5) . ?
C57 C62 1.404(4) . ?
C1 H1 1.0000 . ?
C1 C2 1.536(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.493(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.403(4) . ?
C4 C9 1.400(4) . ?
C5 C6 1.423(4) . ?
C6 C7 1.392(4) . ?
C6 C10 1.529(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.398(5) . ?
C8 C9 1.379(4) . ?
C8 C14A 1.562(10) . ?
C8 C14 1.550(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.537(4) . ?
C10 C12 1.527(5) . ?
C10 C13 1.520(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C18 C19 1.399(4) . ?
C18 C23 1.390(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.377(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.387(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.361(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.382(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.385(5) . ?
C24 C29 1.393(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.388(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.374(8) . ?
C27 H27 0.9500 . ?
C27 C28 1.366(8) . ?
C28 H28 0.9500 . ?
C28 C29 1.396(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.408(4) . ?
C30 C35 1.410(4) . ?
C31 C32 1.419(4) . ?
C32 C33 1.387(4) . ?
C32 C36 1.541(4) . ?
C33 H33 0.9500 . ?
C33 C34 1.403(4) . ?
C34 C35 1.368(4) . ?
C34 C40 1.538(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.527(4) . ?
C36 C38 1.536(4) . ?
C36 C39 1.537(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.536(4) . ?
C40 C42 1.537(4) . ?
C40 C43 1.537(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.390(4) . ?
C44 C49 1.381(4) . ?
C45 H45 0.9500 . ?
C45 C46 1.383(5) . ?
C46 H46 0.9500 . ?
C46 C47 1.370(5) . ?
C47 H47 0.9500 . ?
C47 C48 1.382(5) . ?
C48 H48 0.9500 . ?
C48 C49 1.382(5) . ?
C49 H49 0.9500 . ?
C50 C51 1.373(4) . ?
C50 C55 1.385(4) . ?
C51 H51 0.9500 . ?
C51 C52 1.389(4) . ?
C52 H52 0.9500 . ?
C52 C53 1.358(5) . ?
C53 H53 0.9500 . ?
C53 C54 1.387(5) . ?
C54 H54 0.9500 . ?
C54 C55 1.386(5) . ?
C55 H55 0.9500 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C58 H58 0.9500 . ?
C58 C59 1.371(5) . ?
C59 H59 0.9500 . ?
C59 C60 1.392(5) . ?
C60 H60 0.9500 . ?
C60 C61 1.377(6) . ?
C61 H61 0.9500 . ?
C61 C62 1.375(5) . ?
C62 H62 0.9500 . ?
C14A C17A 1.5382 . ?
C14A C16A 1.5387 . ?
C14A C15A 1.5391 . ?
C17A H17A 0.9800 . ?
C17A H17B 0.9800 . ?
C17A H17C 0.9800 . ?
C16A H16A 0.9800 . ?
C16A H16B 0.9800 . ?
C16A H16C 0.9800 . ?
C15A H15A 0.9800 . ?
C15A H15B 0.9800 . ?
C15A H15C 0.9800 . ?
C14 C15 1.5381 . ?
C14 C16 1.5384 . ?
C14 C17 1.5383 . ?
C15 H15D 0.9800 . ?
C15 H15E 0.9800 . ?
C15 H15F 0.9800 . ?
C16 H16D 0.9800 . ?
C16 H16E 0.9800 . ?
C16 H16F 0.9800 . ?
C17 H17D 0.9800 . ?
C17 H17E 0.9800 . ?
C17 H17F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zr N1 81.90(8) . . ?
O1 Zr N2 142.72(9) . . ?
O1 Zr C1 155.98(11) . . ?
O1 Zr C56 98.38(10) . . ?
O2 Zr O1 97.13(8) . . ?
O2 Zr N1 155.26(9) . . ?
O2 Zr N2 84.78(8) . . ?
O2 Zr C1 106.28(10) . . ?
O2 Zr C56 93.01(10) . . ?
N1 Zr C56 111.63(11) . . ?
N2 Zr N1 81.50(9) . . ?
N2 Zr C1 38.27(11) . . ?
N2 Zr C56 118.75(11) . . ?
C1 Zr N1 74.60(11) . . ?
C1 Zr C56 85.90(12) . . ?
N1 P1 C4 112.93(13) . . ?
N1 P1 C18 111.24(13) . . ?
N1 P1 C24 112.84(14) . . ?
C4 P1 C18 105.01(14) . . ?
C4 P1 C24 106.65(13) . . ?
C18 P1 C24 107.70(14) . . ?
N2 P2 C30 116.24(13) . . ?
N2 P2 C44 107.72(14) . . ?
N2 P2 C50 112.56(14) . . ?
C30 P2 C44 106.84(14) . . ?
C30 P2 C50 106.15(13) . . ?
C44 P2 C50 106.84(14) . . ?
C5 O1 Zr 140.47(19) . . ?
C31 O2 Zr 139.62(18) . . ?
P1 N1 Zr 124.73(14) . . ?
C3 N1 Zr 114.98(19) . . ?
C3 N1 P1 117.6(2) . . ?
P2 N2 Zr 124.29(15) . . ?
C1 N2 Zr 71.40(17) . . ?
C1 N2 P2 131.7(2) . . ?
C58 C57 C56 122.5(3) . . ?
C58 C57 C62 116.9(3) . . ?
C62 C57 C56 120.5(3) . . ?
Zr C1 H1 116.7 . . ?
N2 C1 Zr 70.33(17) . . ?
N2 C1 H1 116.7 . . ?
N2 C1 C2 111.9(3) . . ?
C2 C1 Zr 116.1(2) . . ?
C2 C1 H1 116.7 . . ?
C1 C2 H2A 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
C3 C2 C1 108.0(3) . . ?
C3 C2 H2A 110.1 . . ?
C3 C2 H2B 110.1 . . ?
N1 C3 C2 111.5(3) . . ?
N1 C3 H3A 109.3 . . ?
N1 C3 H3B 109.3 . . ?
C2 C3 H3A 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C5 C4 P1 119.6(2) . . ?
C9 C4 P1 118.8(2) . . ?
C9 C4 C5 121.6(3) . . ?
O1 C5 C4 119.4(3) . . ?
O1 C5 C6 121.8(3) . . ?
C4 C5 C6 118.8(2) . . ?
C5 C6 C10 122.0(2) . . ?
C7 C6 C5 116.9(3) . . ?
C7 C6 C10 121.1(3) . . ?
C6 C7 H7 117.5 . . ?
C6 C7 C8 124.9(3) . . ?
C8 C7 H7 117.5 . . ?
C7 C8 C14A 124.2(5) . . ?
C7 C8 C14 119.5(3) . . ?
C9 C8 C7 117.0(3) . . ?
C9 C8 C14A 118.5(5) . . ?
C9 C8 C14 123.4(3) . . ?
C4 C9 H9 119.6 . . ?
C8 C9 C4 120.7(3) . . ?
C8 C9 H9 119.6 . . ?
C6 C10 C11 109.1(3) . . ?
C12 C10 C6 109.9(3) . . ?
C12 C10 C11 110.0(3) . . ?
C13 C10 C6 113.1(2) . . ?
C13 C10 C11 107.5(3) . . ?
C13 C10 C12 107.1(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C18 P1 116.0(2) . . ?
C23 C18 P1 124.7(2) . . ?
C23 C18 C19 119.1(3) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 C18 119.9(3) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 119.9 . . ?
C19 C20 C21 120.2(3) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 H21 119.9 . . ?
C22 C21 C20 120.1(3) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 119.7 . . ?
C21 C22 C23 120.6(4) . . ?
C23 C22 H22 119.7 . . ?
C18 C23 H23 120.0 . . ?
C22 C23 C18 120.0(3) . . ?
C22 C23 H23 120.0 . . ?
C25 C24 P1 120.2(3) . . ?
C25 C24 C29 119.7(3) . . ?
C29 C24 P1 120.1(3) . . ?
C24 C25 H25 119.8 . . ?
C24 C25 C26 120.3(4) . . ?
C26 C25 H25 119.8 . . ?
C25 C26 H26 120.2 . . ?
C27 C26 C25 119.7(5) . . ?
C27 C26 H26 120.2 . . ?
C26 C27 H27 119.7 . . ?
C28 C27 C26 120.7(4) . . ?
C28 C27 H27 119.7 . . ?
C27 C28 H28 119.7 . . ?
C27 C28 C29 120.5(5) . . ?
C29 C28 H28 119.7 . . ?
C24 C29 C28 119.1(4) . . ?
C24 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
C31 C30 P2 120.0(2) . . ?
C31 C30 C35 120.5(3) . . ?
C35 C30 P2 119.3(2) . . ?
O2 C31 C30 119.7(3) . . ?
O2 C31 C32 121.4(2) . . ?
C30 C31 C32 118.9(2) . . ?
C31 C32 C36 121.8(2) . . ?
C33 C32 C31 117.5(3) . . ?
C33 C32 C36 120.7(3) . . ?
C32 C33 H33 117.8 . . ?
C32 C33 C34 124.5(3) . . ?
C34 C33 H33 117.8 . . ?
C33 C34 C40 119.9(3) . . ?
C35 C34 C33 117.0(3) . . ?
C35 C34 C40 123.1(3) . . ?
C30 C35 H35 119.2 . . ?
C34 C35 C30 121.5(3) . . ?
C34 C35 H35 119.2 . . ?
C37 C36 C32 112.1(2) . . ?
C37 C36 C38 107.4(3) . . ?
C37 C36 C39 107.0(3) . . ?
C38 C36 C32 109.1(2) . . ?
C38 C36 C39 110.2(3) . . ?
C39 C36 C32 111.0(3) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C40 C34 109.5(2) . . ?
C41 C40 C42 109.6(3) . . ?
C41 C40 C43 108.3(3) . . ?
C42 C40 C34 109.1(2) . . ?
C43 C40 C34 111.3(3) . . ?
C43 C40 C42 108.9(3) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 C44 P2 121.1(2) . . ?
C49 C44 P2 119.7(2) . . ?
C49 C44 C45 119.2(3) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 C44 120.4(3) . . ?
C46 C45 H45 119.8 . . ?
C45 C46 H46 120.0 . . ?
C47 C46 C45 120.0(3) . . ?
C47 C46 H46 120.0 . . ?
C46 C47 H47 120.0 . . ?
C46 C47 C48 119.9(3) . . ?
C48 C47 H47 120.0 . . ?
C47 C48 H48 119.8 . . ?
C47 C48 C49 120.4(4) . . ?
C49 C48 H48 119.8 . . ?
C44 C49 C48 120.0(3) . . ?
C44 C49 H49 120.0 . . ?
C48 C49 H49 120.0 . . ?
C51 C50 P2 119.2(2) . . ?
C51 C50 C55 118.7(3) . . ?
C55 C50 P2 122.1(2) . . ?
C50 C51 H51 119.3 . . ?
C50 C51 C52 121.4(3) . . ?
C52 C51 H51 119.3 . . ?
C51 C52 H52 120.3 . . ?
C53 C52 C51 119.4(3) . . ?
C53 C52 H52 120.3 . . ?
C52 C53 H53 119.8 . . ?
C52 C53 C54 120.4(3) . . ?
C54 C53 H53 119.8 . . ?
C53 C54 H54 120.1 . . ?
C55 C54 C53 119.8(4) . . ?
C55 C54 H54 120.1 . . ?
C50 C55 C54 120.3(3) . . ?
C50 C55 H55 119.9 . . ?
C54 C55 H55 119.9 . . ?
Zr C56 H56A 108.0 . . ?
Zr C56 H56B 108.0 . . ?
C57 C56 Zr 117.0(2) . . ?
C57 C56 H56A 108.0 . . ?
C57 C56 H56B 108.0 . . ?
H56A C56 H56B 107.3 . . ?
C57 C58 H58 119.1 . . ?
C59 C58 C57 121.8(3) . . ?
C59 C58 H58 119.1 . . ?
C58 C59 H59 119.9 . . ?
C58 C59 C60 120.2(4) . . ?
C60 C59 H59 119.9 . . ?
C59 C60 H60 120.5 . . ?
C61 C60 C59 119.0(4) . . ?
C61 C60 H60 120.5 . . ?
C60 C61 H61 119.6 . . ?
C62 C61 C60 120.8(3) . . ?
C62 C61 H61 119.6 . . ?
C57 C62 H62 119.4 . . ?
C61 C62 C57 121.2(3) . . ?
C61 C62 H62 119.4 . . ?
C17A C14A C8 108.9(8) . . ?
C17A C14A C16A 109.5 . . ?
C17A C14A C15A 109.5 . . ?
C16A C14A C8 111.0(9) . . ?
C16A C14A C15A 109.5 . . ?
C15A C14A C8 108.6(8) . . ?
C14A C17A H17A 109.5 . . ?
C14A C17A H17B 109.5 . . ?
C14A C17A H17C 109.5 . . ?
H17A C17A H17B 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
C14A C16A H16A 109.5 . . ?
C14A C16A H16B 109.5 . . ?
C14A C16A H16C 109.5 . . ?
H16A C16A H16B 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C14A C15A H15A 109.5 . . ?
C14A C15A H15B 109.5 . . ?
C14A C15A H15C 109.5 . . ?
H15A C15A H15B 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
C15 C14 C8 110.0(3) . . ?
C15 C14 C16 109.5 . . ?
C15 C14 C17 109.5 . . ?
C16 C14 C8 110.7(3) . . ?
C17 C14 C8 107.7(3) . . ?
C17 C14 C16 109.5 . . ?
C14 C15 H15D 109.5 . . ?
C14 C15 H15E 109.5 . . ?
C14 C15 H15F 109.5 . . ?
H15D C15 H15E 109.5 . . ?
H15D C15 H15F 109.5 . . ?
H15E C15 H15F 109.5 . . ?
C14 C16 H16D 109.5 . . ?
C14 C16 H16E 109.5 . . ?
C14 C16 H16F 109.5 . . ?
H16D C16 H16E 109.5 . . ?
H16D C16 H16F 109.5 . . ?
H16E C16 H16F 109.5 . . ?
C14 C17 H17D 109.5 . . ?
C14 C17 H17E 109.5 . . ?
C14 C17 H17F 109.5 . . ?
H17D C17 H17E 109.5 . . ?
H17D C17 H17F 109.5 . . ?
H17E C17 H17F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr O1 C5 C4 -44.5(4) . . . . ?
Zr O1 C5 C6 135.1(3) . . . . ?
Zr O2 C31 C30 38.8(4) . . . . ?
Zr O2 C31 C32 -141.6(2) . . . . ?
Zr N1 C3 C2 36.2(3) . . . . ?
Zr N2 C1 C2 111.1(2) . . . . ?
Zr C1 C2 C3 30.7(3) . . . . ?
P1 N1 C3 C2 -161.5(2) . . . . ?
P1 C4 C5 O1 -3.7(3) . . . . ?
P1 C4 C5 C6 176.7(2) . . . . ?
P1 C4 C9 C8 -178.2(2) . . . . ?
P1 C18 C19 C20 175.1(3) . . . . ?
P1 C18 C23 C22 -174.3(3) . . . . ?
P1 C24 C25 C26 177.7(3) . . . . ?
P1 C24 C29 C28 -178.2(3) . . . . ?
P2 N2 C1 Zr 119.8(3) . . . . ?
P2 N2 C1 C2 -129.1(3) . . . . ?
P2 C30 C31 O2 4.0(4) . . . . ?
P2 C30 C31 C32 -175.7(2) . . . . ?
P2 C30 C35 C34 177.3(2) . . . . ?
P2 C44 C45 C46 175.8(3) . . . . ?
P2 C44 C49 C48 -176.1(3) . . . . ?
P2 C50 C51 C52 177.5(3) . . . . ?
P2 C50 C55 C54 -178.4(4) . . . . ?
O1 C5 C6 C7 -176.9(3) . . . . ?
O1 C5 C6 C10 4.1(4) . . . . ?
O2 C31 C32 C33 178.1(3) . . . . ?
O2 C31 C32 C36 -0.7(4) . . . . ?
N1 P1 C4 C5 38.6(2) . . . . ?
N1 P1 C4 C9 -142.08(17) . . . . ?
N1 P1 C18 C19 50.2(3) . . . . ?
N1 P1 C18 C23 -134.7(3) . . . . ?
N1 P1 C24 C25 -106.8(3) . . . . ?
N1 P1 C24 C29 70.4(3) . . . . ?
N2 P2 C30 C31 -33.3(3) . . . . ?
N2 P2 C30 C35 149.9(2) . . . . ?
N2 P2 C44 C45 164.9(3) . . . . ?
N2 P2 C44 C49 -17.4(3) . . . . ?
N2 P2 C50 C51 -63.1(3) . . . . ?
N2 P2 C50 C55 114.2(3) . . . . ?
N2 C1 C2 C3 -47.4(4) . . . . ?
C57 C58 C59 C60 0.5(6) . . . . ?
C1 C2 C3 N1 -42.2(4) . . . . ?
C4 P1 N1 Zr -37.9(2) . . . . ?
C4 P1 N1 C3 161.7(2) . . . . ?
C4 P1 C18 C19 -72.3(2) . . . . ?
C4 P1 C18 C23 102.8(3) . . . . ?
C4 P1 C24 C25 17.8(3) . . . . ?
C4 P1 C24 C29 -165.0(3) . . . . ?
C4 C5 C6 C7 2.7(4) . . . . ?
C4 C5 C6 C10 -176.4(2) . . . . ?
C5 C4 C9 C8 1.1(3) . . . . ?
C5 C6 C7 C8 -1.4(5) . . . . ?
C5 C6 C10 C11 -62.8(4) . . . . ?
C5 C6 C10 C12 57.9(4) . . . . ?
C5 C6 C10 C13 177.6(3) . . . . ?
C6 C7 C8 C9 -0.1(5) . . . . ?
C6 C7 C8 C14A 173.0(5) . . . . ?
C6 C7 C8 C14 -179.3(3) . . . . ?
C7 C6 C10 C11 118.2(3) . . . . ?
C7 C6 C10 C12 -121.1(3) . . . . ?
C7 C6 C10 C13 -1.4(4) . . . . ?
C7 C8 C9 C4 0.3(4) . . . . ?
C7 C8 C14A C17A 123.2(6) . . . . ?
C7 C8 C14A C16A 2.7(7) . . . . ?
C7 C8 C14A C15A -117.7(6) . . . . ?
C7 C8 C14 C15 176.7(3) . . . . ?
C7 C8 C14 C16 55.5(4) . . . . ?
C7 C8 C14 C17 -64.1(4) . . . . ?
C9 C4 C5 O1 177.0(2) . . . . ?
C9 C4 C5 C6 -2.6(3) . . . . ?
C9 C8 C14A C17A -63.8(7) . . . . ?
C9 C8 C14A C16A 175.6(6) . . . . ?
C9 C8 C14A C15A 55.3(7) . . . . ?
C9 C8 C14 C15 -2.4(4) . . . . ?
C9 C8 C14 C16 -123.6(3) . . . . ?
C9 C8 C14 C17 116.8(3) . . . . ?
C10 C6 C7 C8 177.6(3) . . . . ?
C18 P1 N1 Zr -155.70(16) . . . . ?
C18 P1 N1 C3 43.9(3) . . . . ?
C18 P1 C4 C5 159.99(18) . . . . ?
C18 P1 C4 C9 -20.70(19) . . . . ?
C18 P1 C24 C25 130.1(3) . . . . ?
C18 P1 C24 C29 -52.7(3) . . . . ?
C18 C19 C20 C21 -0.4(5) . . . . ?
C19 C18 C23 C22 0.6(5) . . . . ?
C19 C20 C21 C22 0.7(6) . . . . ?
C20 C21 C22 C23 -0.4(6) . . . . ?
C21 C22 C23 C18 -0.3(6) . . . . ?
C23 C18 C19 C20 -0.3(5) . . . . ?
C24 P1 N1 Zr 83.1(2) . . . . ?
C24 P1 N1 C3 -77.2(3) . . . . ?
C24 P1 C4 C5 -85.9(2) . . . . ?
C24 P1 C4 C9 93.42(18) . . . . ?
C24 P1 C18 C19 174.3(2) . . . . ?
C24 P1 C18 C23 -10.6(3) . . . . ?
C24 C25 C26 C27 0.5(6) . . . . ?
C25 C24 C29 C28 -1.0(5) . . . . ?
C25 C26 C27 C28 -0.9(7) . . . . ?
C26 C27 C28 C29 0.3(7) . . . . ?
C27 C28 C29 C24 0.6(6) . . . . ?
C29 C24 C25 C26 0.5(5) . . . . ?
C30 P2 N2 Zr 28.6(2) . . . . ?
C30 P2 N2 C1 -66.6(3) . . . . ?
C30 P2 C44 C45 39.4(3) . . . . ?
C30 P2 C44 C49 -143.0(3) . . . . ?
C30 P2 C50 C51 65.1(3) . . . . ?
C30 P2 C50 C55 -117.6(3) . . . . ?
C30 C31 C32 C33 -2.3(4) . . . . ?
C30 C31 C32 C36 178.9(3) . . . . ?
C31 C30 C35 C34 0.5(4) . . . . ?
C31 C32 C33 C34 2.0(4) . . . . ?
C31 C32 C36 C37 -173.6(3) . . . . ?
C31 C32 C36 C38 67.6(3) . . . . ?
C31 C32 C36 C39 -54.0(4) . . . . ?
C32 C33 C34 C35 -0.4(4) . . . . ?
C32 C33 C34 C40 178.8(3) . . . . ?
C33 C32 C36 C37 7.6(4) . . . . ?
C33 C32 C36 C38 -111.3(3) . . . . ?
C33 C32 C36 C39 127.2(3) . . . . ?
C33 C34 C35 C30 -0.9(4) . . . . ?
C33 C34 C40 C41 54.6(4) . . . . ?
C33 C34 C40 C42 -65.4(4) . . . . ?
C33 C34 C40 C43 174.4(3) . . . . ?
C35 C30 C31 O2 -179.3(3) . . . . ?
C35 C30 C31 C32 1.1(4) . . . . ?
C35 C34 C40 C41 -126.2(3) . . . . ?
C35 C34 C40 C42 113.8(3) . . . . ?
C35 C34 C40 C43 -6.4(4) . . . . ?
C36 C32 C33 C34 -179.1(3) . . . . ?
C40 C34 C35 C30 179.9(3) . . . . ?
C44 P2 N2 Zr -91.17(18) . . . . ?
C44 P2 N2 C1 173.7(3) . . . . ?
C44 P2 C30 C31 87.0(2) . . . . ?
C44 P2 C30 C35 -89.8(2) . . . . ?
C44 P2 C50 C51 178.8(3) . . . . ?
C44 P2 C50 C55 -3.9(3) . . . . ?
C44 C45 C46 C47 0.7(6) . . . . ?
C45 C44 C49 C48 1.6(6) . . . . ?
C45 C46 C47 C48 0.6(7) . . . . ?
C46 C47 C48 C49 -0.8(8) . . . . ?
C47 C48 C49 C44 -0.3(7) . . . . ?
C49 C44 C45 C46 -1.8(5) . . . . ?
C50 P2 N2 Zr 151.32(15) . . . . ?
C50 P2 N2 C1 56.1(3) . . . . ?
C50 P2 C30 C31 -159.3(2) . . . . ?
C50 P2 C30 C35 23.9(3) . . . . ?
C50 P2 C44 C45 -73.9(3) . . . . ?
C50 P2 C44 C49 103.7(3) . . . . ?
C50 C51 C52 C53 1.4(5) . . . . ?
C51 C50 C55 C54 -1.1(6) . . . . ?
C51 C52 C53 C54 -2.1(6) . . . . ?
C52 C53 C54 C55 1.2(8) . . . . ?
C53 C54 C55 C50 0.4(8) . . . . ?
C55 C50 C51 C52 0.1(5) . . . . ?
C56 C57 C58 C59 177.1(3) . . . . ?
C56 C57 C62 C61 -177.5(3) . . . . ?
C58 C57 C56 Zr 106.0(3) . . . . ?
C58 C57 C62 C61 1.3(5) . . . . ?
C58 C59 C60 C61 1.0(6) . . . . ?
C59 C60 C61 C62 -1.4(6) . . . . ?
C60 C61 C62 C57 0.3(6) . . . . ?
C62 C57 C56 Zr -75.3(3) . . . . ?
C62 C57 C58 C59 -1.7(5) . . . . ?
C14A C8 C9 C4 -173.2(4) . . . . ?
C14 C8 C9 C4 179.5(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.299 0.500 0.000 808.6 295.4 '6 C6H14'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.031 0.500 0.000 807 142 ' '
2 0.042 0.179 0.500 7 0 ' '
3 0.958 0.821 0.500 7 0 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT213_2Cpp                
;
PROBLEM: Atom C17 has ADP max/min Ratio ..... 5.4 prolat
RESPONSE: C14, C15, C16 and C17 belong to a disordered tert-butyl group.
The model was improved by including a minor tert-butyl group 
as an isotropic rigid group with an occupation factor of 0.26. 
The major component was anisotropically refined. 
It is not uncommon to observed, in such a case, elongated ADP ellipsoids.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_1cH2
_database_code_depnum_ccdc_archive 'CCDC 1978291'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne
France
;
_audit_update_record             
;
2020-01-16 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_audit_creation_date             2019-11-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C55 H68 N2 O2 P2'
_chemical_formula_sum            'C55 H68 N2 O2 P2'
_chemical_formula_weight         851.05
_chemical_absolute_configuration ?
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'

_cell_length_a                   9.7379(4)
_cell_length_b                   18.0542(8)
_cell_length_c                   28.0036(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4923.3(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6024
_cell_measurement_temperature    115
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      2.38
_shelx_estimated_absorpt_T_max   0.990
_shelx_estimated_absorpt_T_min   0.966
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.8947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0524 before and 0.0462 after correction. The Ratio of minimum to maximum transmission is 0.9219. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            22819
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.567
_diffrn_reflns_theta_min         2.214
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       "φ and ω scans'"
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.766
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.945
_reflns_number_gt                9638
_reflns_number_total             11079
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 
;
 Flack x determined using 3746 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         11079
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0395
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0377P)²+0.2203P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0851
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H3BC)=Sof(H3BD)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H1BC)=Sof(H1BD)=1-FVAR(1)
 Sof(H3AA)=Sof(H3AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H1AA)=Sof(H1AB)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C3(H3AA,H3AB), C3(H3BC,H3BD), C2(H2A,H2B), C2B(H2BA,H2BB), C1(H1AA,H1AB),
 C1(H1BC,H1BD)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
 C26(H26), C27(H27), C28(H28), C29(H29), C33(H33), C35(H35), C45(H45), C46(H46),
  C47(H47), C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C3 C 0.5055(3) 0.57922(14) 0.50572(10) 0.0214(6) Uani 1 1 d . . . . .
H3AA H 0.445600 0.584705 0.534073 0.026 Uiso 0.745(6) 1 calc R . P A 1
H3AB H 0.446845 0.584508 0.477048 0.026 Uiso 0.745(6) 1 calc R . P A 1
H3BC H 0.527919 0.603796 0.536349 0.026 Uiso 0.255(6) 1 calc R . P A 2
H3BD H 0.404264 0.575335 0.503585 0.026 Uiso 0.255(6) 1 calc R . P A 2
C2 C 0.6107(4) 0.64210(18) 0.50591(12) 0.0210(10) Uani 0.745(6) 1 d . . P A 1
H2A H 0.560334 0.689561 0.508618 0.025 Uiso 0.745(6) 1 calc R . P A 1
H2B H 0.668033 0.636969 0.534911 0.025 Uiso 0.745(6) 1 calc R . P A 1
C2B C 0.5551(11) 0.6256(6) 0.4663(4) 0.022(3) Uiso 0.255(6) 1 d . . P A 2
H2BA H 0.501267 0.672144 0.467003 0.027 Uiso 0.255(6) 1 calc R . P A 2
H2BB H 0.531300 0.599940 0.436213 0.027 Uiso 0.255(6) 1 calc R . P A 2
C1 C 0.7051(3) 0.64701(14) 0.46320(10) 0.0217(6) Uani 1 1 d . . . . .
H1AA H 0.648711 0.649279 0.433826 0.026 Uiso 0.745(6) 1 calc R . P A 1
H1AB H 0.758325 0.693629 0.465256 0.026 Uiso 0.745(6) 1 calc R . P A 1
H1BC H 0.717684 0.679697 0.435151 0.026 Uiso 0.255(6) 1 calc R . P A 2
H1BD H 0.729277 0.676059 0.491980 0.026 Uiso 0.255(6) 1 calc R . P A 2
C4 C 0.7221(2) 0.55274(13) 0.36400(8) 0.0130(5) Uani 1 1 d . . . . .
C5 C 0.6159(2) 0.50019(13) 0.37326(8) 0.0126(5) Uani 1 1 d . . . . .
C6 C 0.5146(2) 0.49067(13) 0.33594(8) 0.0139(5) Uani 1 1 d . . . . .
C7 C 0.5221(2) 0.53564(14) 0.29649(8) 0.0151(5) Uani 1 1 d . . . . .
H7 H 0.454057 0.529300 0.272529 0.018 Uiso 1 1 calc R . . . .
C8 C 0.6233(2) 0.59077(13) 0.28866(8) 0.0144(5) Uani 1 1 d . . . . .
C9 C 0.7236(2) 0.59800(14) 0.32295(9) 0.0145(5) Uani 1 1 d . . . . .
H9 H 0.794359 0.633691 0.318945 0.017 Uiso 1 1 calc R . . . .
C10 C 0.4024(3) 0.43211(14) 0.34243(9) 0.0201(6) Uani 1 1 d . . . . .
C11 C 0.3153(3) 0.45101(18) 0.38625(10) 0.0302(7) Uani 1 1 d . . . . .
H11A H 0.372819 0.449409 0.414939 0.045 Uiso 1 1 calc GR . . . .
H11B H 0.240569 0.414938 0.389308 0.045 Uiso 1 1 calc GR . . . .
H11C H 0.276552 0.500794 0.382571 0.045 Uiso 1 1 calc GR . . . .
C12 C 0.4695(3) 0.35531(15) 0.34855(10) 0.0301(7) Uani 1 1 d . . . . .
H12A H 0.397764 0.317784 0.352742 0.045 Uiso 1 1 calc GR . . . .
H12B H 0.529320 0.355780 0.376679 0.045 Uiso 1 1 calc GR . . . .
H12C H 0.523920 0.343566 0.320108 0.045 Uiso 1 1 calc GR . . . .
C13 C 0.3063(3) 0.42742(16) 0.29889(11) 0.0313(7) Uani 1 1 d . . . . .
H13A H 0.261528 0.475430 0.293957 0.047 Uiso 1 1 calc GR . . . .
H13B H 0.236342 0.389387 0.304535 0.047 Uiso 1 1 calc GR . . . .
H13C H 0.359797 0.414451 0.270451 0.047 Uiso 1 1 calc GR . . . .
C14 C 0.6162(3) 0.63870(14) 0.24348(8) 0.0179(5) Uani 1 1 d . . . . .
C15 C 0.6114(3) 0.58923(16) 0.19887(9) 0.0300(7) Uani 1 1 d . . . . .
H15A H 0.604231 0.620310 0.170288 0.045 Uiso 1 1 calc GR . . . .
H15B H 0.531439 0.556373 0.200717 0.045 Uiso 1 1 calc GR . . . .
H15C H 0.695361 0.559440 0.197149 0.045 Uiso 1 1 calc GR . . . .
C16 C 0.4850(3) 0.68594(15) 0.24440(9) 0.0226(6) Uani 1 1 d . . . . .
H16A H 0.486079 0.718111 0.272586 0.034 Uiso 1 1 calc GR . . . .
H16B H 0.404489 0.653415 0.245732 0.034 Uiso 1 1 calc GR . . . .
H16C H 0.480652 0.716405 0.215480 0.034 Uiso 1 1 calc GR . . . .
C17 C 0.7389(3) 0.69087(18) 0.23935(11) 0.0348(8) Uani 1 1 d . . . . .
H17A H 0.740878 0.724113 0.267012 0.052 Uiso 1 1 calc GR . . . .
H17B H 0.730781 0.720172 0.210029 0.052 Uiso 1 1 calc GR . . . .
H17C H 0.823915 0.661847 0.238367 0.052 Uiso 1 1 calc GR . . . .
C18 C 0.9935(2) 0.60806(13) 0.38617(9) 0.0146(5) Uani 1 1 d . . . . .
C19 C 1.0547(3) 0.59249(15) 0.34213(10) 0.0214(6) Uani 1 1 d . . . . .
H19 H 1.017264 0.554974 0.322219 0.026 Uiso 1 1 calc R . . . .
C20 C 1.1693(3) 0.63142(15) 0.32743(11) 0.0277(7) Uani 1 1 d . . . . .
H20 H 1.210399 0.620470 0.297486 0.033 Uiso 1 1 calc R . . . .
C21 C 1.2243(3) 0.68610(17) 0.35602(11) 0.0333(7) Uani 1 1 d . . . . .
H21 H 1.303091 0.712716 0.345720 0.040 Uiso 1 1 calc R . . . .
C22 C 1.1654(3) 0.70210(18) 0.39936(12) 0.0409(8) Uani 1 1 d . . . . .
H22 H 1.203601 0.739772 0.418966 0.049 Uiso 1 1 calc R . . . .
C23 C 1.0494(3) 0.66323(16) 0.41475(10) 0.0290(7) Uani 1 1 d . . . . .
H23 H 1.008928 0.674521 0.444742 0.035 Uiso 1 1 calc R . . . .
C24 C 0.9226(2) 0.46167(13) 0.41621(8) 0.0134(5) Uani 1 1 d . . . . .
C25 C 0.9070(2) 0.40939(14) 0.38019(9) 0.0166(5) Uani 1 1 d . . . . .
H25 H 0.854640 0.421257 0.352600 0.020 Uiso 1 1 calc R . . . .
C26 C 0.9670(3) 0.34017(14) 0.38416(9) 0.0198(6) Uani 1 1 d . . . . .
H26 H 0.956095 0.304777 0.359349 0.024 Uiso 1 1 calc R . . . .
C27 C 1.0431(3) 0.32263(14) 0.42443(9) 0.0186(5) Uani 1 1 d . . . . .
H27 H 1.084141 0.275107 0.427344 0.022 Uiso 1 1 calc R . . . .
C28 C 1.0592(2) 0.37457(14) 0.46043(9) 0.0181(5) Uani 1 1 d . . . . .
H28 H 1.111392 0.362367 0.487985 0.022 Uiso 1 1 calc R . . . .
C29 C 1.0000(2) 0.44408(14) 0.45666(8) 0.0156(5) Uani 1 1 d . . . . .
H29 H 1.011971 0.479519 0.481391 0.019 Uiso 1 1 calc R . . . .
C30 C 0.6919(2) 0.52092(13) 0.59732(8) 0.0143(5) Uani 1 1 d . . . . .
C31 C 0.8256(2) 0.54780(13) 0.58507(8) 0.0138(5) Uani 1 1 d . . . . .
C32 C 0.8893(2) 0.59776(13) 0.61859(8) 0.0136(5) Uani 1 1 d . . . . .
C33 C 0.8172(3) 0.61671(13) 0.65949(8) 0.0157(5) Uani 1 1 d . . . . .
H33 H 0.860840 0.648951 0.681593 0.019 Uiso 1 1 calc R . . . .
C34 C 0.6843(2) 0.59171(14) 0.67066(8) 0.0150(5) Uani 1 1 d . . . . .
C35 C 0.6230(2) 0.54389(13) 0.63860(8) 0.0147(5) Uani 1 1 d . . . . .
H35 H 0.532728 0.526330 0.644653 0.018 Uiso 1 1 calc R . . . .
C36 C 1.0326(2) 0.62902(15) 0.60770(9) 0.0183(5) Uani 1 1 d . . . . .
C37 C 1.1355(3) 0.56553(15) 0.60258(11) 0.0283(7) Uani 1 1 d . . . . .
H37A H 1.106473 0.532757 0.576570 0.042 Uiso 1 1 calc GR . . . .
H37B H 1.139332 0.537401 0.632484 0.042 Uiso 1 1 calc GR . . . .
H37C H 1.226581 0.585732 0.595411 0.042 Uiso 1 1 calc GR . . . .
C38 C 1.0273(3) 0.67327(16) 0.56086(10) 0.0280(6) Uani 1 1 d . . . . .
H38A H 0.992739 0.641455 0.535174 0.042 Uiso 1 1 calc GR . . . .
H38B H 1.119737 0.690659 0.552759 0.042 Uiso 1 1 calc GR . . . .
H38C H 0.966035 0.715903 0.564769 0.042 Uiso 1 1 calc GR . . . .
C39 C 1.0856(3) 0.68130(16) 0.64675(10) 0.0255(6) Uani 1 1 d . . . . .
H39A H 1.179084 0.697292 0.638866 0.038 Uiso 1 1 calc GR . . . .
H39B H 1.086213 0.655326 0.677478 0.038 Uiso 1 1 calc GR . . . .
H39C H 1.025451 0.724690 0.648850 0.038 Uiso 1 1 calc GR . . . .
C40 C 0.6064(3) 0.61549(14) 0.71600(9) 0.0187(5) Uani 1 1 d . . . . .
C41 C 0.5649(3) 0.54662(15) 0.74484(9) 0.0249(6) Uani 1 1 d . . . . .
H41A H 0.508096 0.561641 0.772061 0.037 Uiso 1 1 calc GR . . . .
H41B H 0.647570 0.521475 0.756475 0.037 Uiso 1 1 calc GR . . . .
H41C H 0.512533 0.512827 0.724385 0.037 Uiso 1 1 calc GR . . . .
C42 C 0.4754(3) 0.65830(16) 0.70174(11) 0.0309(7) Uani 1 1 d . . . . .
H42A H 0.500851 0.702466 0.683427 0.046 Uiso 1 1 calc GR . . . .
H42B H 0.425528 0.673189 0.730581 0.046 Uiso 1 1 calc GR . . . .
H42C H 0.416586 0.626391 0.682147 0.046 Uiso 1 1 calc GR . . . .
C43 C 0.6932(3) 0.66500(17) 0.74856(10) 0.0303(7) Uani 1 1 d . . . . .
H43A H 0.776078 0.638219 0.758362 0.045 Uiso 1 1 calc GR . . . .
H43B H 0.639679 0.678435 0.776906 0.045 Uiso 1 1 calc GR . . . .
H43C H 0.719377 0.710019 0.731265 0.045 Uiso 1 1 calc GR . . . .
C44 C 0.4673(2) 0.42049(13) 0.58393(9) 0.0160(5) Uani 1 1 d . . . . .
C45 C 0.3377(3) 0.42253(14) 0.56312(9) 0.0188(5) Uani 1 1 d . . . . .
H45 H 0.324475 0.446625 0.533317 0.023 Uiso 1 1 calc R . . . .
C46 C 0.2272(3) 0.38892(15) 0.58634(10) 0.0254(6) Uani 1 1 d . . . . .
H46 H 0.138324 0.390385 0.572358 0.031 Uiso 1 1 calc R . . . .
C47 C 0.2464(3) 0.35365(15) 0.62944(11) 0.0289(7) Uani 1 1 d . . . . .
H47 H 0.170604 0.330965 0.645017 0.035 Uiso 1 1 calc R . . . .
C48 C 0.3750(3) 0.35100(14) 0.65021(10) 0.0262(6) Uani 1 1 d . . . . .
H48 H 0.387587 0.326600 0.679949 0.031 Uiso 1 1 calc R . . . .
C49 C 0.4856(3) 0.38407(15) 0.62750(9) 0.0215(6) Uani 1 1 d . . . . .
H49 H 0.574170 0.381979 0.641624 0.026 Uiso 1 1 calc R . . . .
C50 C 0.7154(2) 0.38418(13) 0.53639(8) 0.0133(5) Uani 1 1 d . . . . .
C51 C 0.6852(2) 0.34621(13) 0.49428(9) 0.0149(5) Uani 1 1 d . . . . .
H51 H 0.619133 0.365424 0.472624 0.018 Uiso 1 1 calc R . . . .
C52 C 0.7521(3) 0.28040(14) 0.48422(10) 0.0197(6) Uani 1 1 d . . . . .
H52 H 0.732493 0.254607 0.455455 0.024 Uiso 1 1 calc R . . . .
C53 C 0.8476(3) 0.25206(14) 0.51598(10) 0.0211(6) Uani 1 1 d . . . . .
H53 H 0.891283 0.206141 0.509334 0.025 Uiso 1 1 calc R . . . .
C54 C 0.8799(3) 0.29026(14) 0.55736(9) 0.0213(6) Uani 1 1 d . . . . .
H54 H 0.946710 0.271074 0.578747 0.026 Uiso 1 1 calc R . . . .
C55 C 0.8145(3) 0.35643(14) 0.56749(9) 0.0192(6) Uani 1 1 d . . . . .
H55 H 0.837142 0.382995 0.595692 0.023 Uiso 1 1 calc R . . . .
N1 N 0.8010(2) 0.58492(12) 0.45918(7) 0.0157(4) Uani 1 1 d . . . . .
H1 H 0.821(3) 0.5641(14) 0.4853(10) 0.019 Uiso 1 1 d R . . . .
N2 N 0.5641(2) 0.50444(12) 0.50599(8) 0.0158(5) Uani 1 1 d . . . . .
H2 H 0.592(3) 0.4903(15) 0.4806(10) 0.019 Uiso 1 1 d R . . . .
O1 O 0.61550(16) 0.46350(9) 0.41268(6) 0.0163(4) Uani 1 1 d . . . . .
O2 O 0.88077(17) 0.52704(9) 0.54535(5) 0.0167(4) Uani 1 1 d . . . . .
P1 P 0.85135(6) 0.55296(3) 0.40788(2) 0.01233(13) Uani 1 1 d . . . . .
P2 P 0.61396(6) 0.46263(3) 0.55428(2) 0.01327(13) 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
C3 C2 1.529(4) . ?
C3 C2B 1.467(11) . ?
C3 N2 1.466(3) . ?
C2 C1 1.512(4) . ?
C2B C1 1.514(10) . ?
C1 N1 1.463(3) . ?
C4 C5 1.427(3) . ?
C4 C9 1.410(3) . ?
C4 P1 1.759(2) . ?
C5 C6 1.448(3) . ?
C5 O1 1.287(3) . ?
C6 C7 1.373(3) . ?
C6 C10 1.531(3) . ?
C7 C8 1.418(3) . ?
C8 C9 1.376(3) . ?
C8 C14 1.534(3) . ?
C10 C11 1.531(4) . ?
C10 C12 1.542(4) . ?
C10 C13 1.540(4) . ?
C14 C15 1.537(4) . ?
C14 C16 1.537(4) . ?
C14 C17 1.526(4) . ?
C18 C19 1.398(4) . ?
C18 C23 1.389(4) . ?
C18 P1 1.810(2) . ?
C19 C20 1.382(4) . ?
C20 C21 1.379(4) . ?
C21 C22 1.373(4) . ?
C22 C23 1.398(4) . ?
C24 C25 1.390(3) . ?
C24 C29 1.397(3) . ?
C24 P1 1.803(2) . ?
C25 C26 1.384(3) . ?
C26 C27 1.386(3) . ?
C27 C28 1.386(4) . ?
C28 C29 1.385(3) . ?
C30 C31 1.431(3) . ?
C30 C35 1.399(3) . ?
C30 P2 1.771(2) . ?
C31 C32 1.442(3) . ?
C31 O2 1.291(3) . ?
C32 C33 1.386(3) . ?
C32 C36 1.536(3) . ?
C33 C34 1.406(3) . ?
C34 C35 1.381(3) . ?
C34 C40 1.540(3) . ?
C36 C37 1.529(3) . ?
C36 C38 1.537(4) . ?
C36 C39 1.534(4) . ?
C40 C41 1.537(3) . ?
C40 C42 1.544(4) . ?
C40 C43 1.531(4) . ?
C44 C45 1.391(3) . ?
C44 C49 1.397(4) . ?
C44 P2 1.819(2) . ?
C45 C46 1.396(4) . ?
C46 C47 1.377(4) . ?
C47 C48 1.382(4) . ?
C48 C49 1.386(4) . ?
C50 C51 1.395(3) . ?
C50 C55 1.393(3) . ?
C50 P2 1.798(2) . ?
C51 C52 1.384(3) . ?
C52 C53 1.385(4) . ?
C53 C54 1.385(4) . ?
C54 C55 1.383(3) . ?
N1 P1 1.624(2) . ?
N2 P2 1.623(2) . ?

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 C3 C2 115.0(2) . . ?
N2 C3 C2B 113.7(5) . . ?
C1 C2 C3 116.6(3) . . ?
C3 C2B C1 120.5(7) . . ?
N1 C1 C2 113.8(2) . . ?
N1 C1 C2B 115.2(5) . . ?
C5 C4 P1 113.14(17) . . ?
C9 C4 C5 122.7(2) . . ?
C9 C4 P1 124.09(18) . . ?
C4 C5 C6 116.2(2) . . ?
O1 C5 C4 120.0(2) . . ?
O1 C5 C6 123.8(2) . . ?
C5 C6 C10 118.9(2) . . ?
C7 C6 C5 118.3(2) . . ?
C7 C6 C10 122.8(2) . . ?
C6 C7 C8 125.2(2) . . ?
C7 C8 C14 119.5(2) . . ?
C9 C8 C7 116.9(2) . . ?
C9 C8 C14 123.6(2) . . ?
C8 C9 C4 120.4(2) . . ?
C6 C10 C12 109.4(2) . . ?
C6 C10 C13 112.2(2) . . ?
C11 C10 C6 109.7(2) . . ?
C11 C10 C12 110.3(2) . . ?
C11 C10 C13 108.1(2) . . ?
C13 C10 C12 107.2(2) . . ?
C8 C14 C15 110.1(2) . . ?
C8 C14 C16 109.7(2) . . ?
C15 C14 C16 108.1(2) . . ?
C17 C14 C8 112.1(2) . . ?
C17 C14 C15 108.7(2) . . ?
C17 C14 C16 108.1(2) . . ?
C19 C18 P1 120.8(2) . . ?
C23 C18 C19 119.0(2) . . ?
C23 C18 P1 120.0(2) . . ?
C20 C19 C18 120.3(3) . . ?
C21 C20 C19 120.3(3) . . ?
C22 C21 C20 120.1(3) . . ?
C21 C22 C23 120.3(3) . . ?
C18 C23 C22 120.0(3) . . ?
C25 C24 C29 119.5(2) . . ?
C25 C24 P1 119.00(18) . . ?
C29 C24 P1 121.34(18) . . ?
C26 C25 C24 120.6(2) . . ?
C25 C26 C27 119.8(2) . . ?
C28 C27 C26 119.8(2) . . ?
C29 C28 C27 120.7(2) . . ?
C28 C29 C24 119.5(2) . . ?
C31 C30 P2 115.36(17) . . ?
C35 C30 C31 122.3(2) . . ?
C35 C30 P2 122.19(18) . . ?
C30 C31 C32 116.6(2) . . ?
O2 C31 C30 119.1(2) . . ?
O2 C31 C32 124.3(2) . . ?
C31 C32 C36 119.4(2) . . ?
C33 C32 C31 118.3(2) . . ?
C33 C32 C36 122.2(2) . . ?
C32 C33 C34 124.8(2) . . ?
C33 C34 C40 123.2(2) . . ?
C35 C34 C33 117.0(2) . . ?
C35 C34 C40 119.8(2) . . ?
C34 C35 C30 121.0(2) . . ?
C32 C36 C38 109.3(2) . . ?
C37 C36 C32 109.8(2) . . ?
C37 C36 C38 109.4(2) . . ?
C37 C36 C39 107.9(2) . . ?
C39 C36 C32 113.0(2) . . ?
C39 C36 C38 107.4(2) . . ?
C34 C40 C42 109.5(2) . . ?
C41 C40 C34 109.7(2) . . ?
C41 C40 C42 108.9(2) . . ?
C43 C40 C34 112.5(2) . . ?
C43 C40 C41 107.7(2) . . ?
C43 C40 C42 108.5(2) . . ?
C45 C44 C49 119.6(2) . . ?
C45 C44 P2 120.68(19) . . ?
C49 C44 P2 119.72(19) . . ?
C44 C45 C46 119.5(2) . . ?
C47 C46 C45 120.3(3) . . ?
C46 C47 C48 120.5(3) . . ?
C47 C48 C49 119.7(3) . . ?
C48 C49 C44 120.3(3) . . ?
C51 C50 P2 120.47(18) . . ?
C55 C50 C51 119.8(2) . . ?
C55 C50 P2 119.31(19) . . ?
C52 C51 C50 119.7(2) . . ?
C51 C52 C53 120.2(2) . . ?
C54 C53 C52 120.4(2) . . ?
C55 C54 C53 119.8(2) . . ?
C54 C55 C50 120.1(2) . . ?
C1 N1 P1 122.20(17) . . ?
C3 N2 P2 123.30(17) . . ?
C4 P1 C18 108.29(11) . . ?
C4 P1 C24 111.32(11) . . ?
C24 P1 C18 104.58(11) . . ?
N1 P1 C4 113.75(11) . . ?
N1 P1 C18 109.44(12) . . ?
N1 P1 C24 109.06(11) . . ?
C30 P2 C44 105.93(11) . . ?
C30 P2 C50 114.98(11) . . ?
C50 P2 C44 103.24(11) . . ?
N2 P2 C30 114.77(11) . . ?
N2 P2 C44 109.87(12) . . ?
N2 P2 C50 107.37(11) . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1aH2
_database_code_depnum_ccdc_archive 'CCDC 1978293'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne
France
;
_audit_update_record             
;
2020-01-16 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_audit_creation_date             2019-11-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H66 N2 O2 P2, 0.1(C H2 Cl2)'
_chemical_formula_sum            'C54.10 H66.20 Cl0.20 N2 O2 P2'
_chemical_formula_weight         845.52
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   16.866(18)
_cell_length_b                   13.874(14)
_cell_length_c                   20.49(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.56(3)
_cell_angle_gamma                90
_cell_volume                     4790(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5065
_cell_measurement_temperature    110
_cell_measurement_theta_max      26.096
_cell_measurement_theta_min      2.72
_shelx_estimated_absorpt_T_max   0.986
_shelx_estimated_absorpt_T_min   0.986
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.7785
_exptl_absorpt_correction_T_min  0.7092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0819 before and 0.0672 after correction. The Ratio of minimum to maximum transmission is 0.9110. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1817
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1124
_diffrn_reflns_av_unetI/netI     0.0795
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28200
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.990
_diffrn_ambient_temperature      110
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       "φ and ω scans'"
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2606
_reflns_number_total             4189
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4189
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0484
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0502P)²+2.1582P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1176
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(Cl1) = Uiso(Cl2)
3. Rigid body (RIGU) restrains
 Cl2, C28, Cl1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Cl1(0.05) C28(0.05) H28A(0.05) H28B(0.05) Cl2(0.05)
5.a Riding coordinates:
 N(H)
5.b Free rotating group:
 Cl1(C28,Cl2)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C28(H28A,H28B)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23),
 C24(H24), C25(H25), C26(H26), C27(H27)
5.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.52515(14) 0.96267(17) 0.71967(12) 0.0196(6) Uani 1 1 d . . . . .
H1A H 0.490205 0.976069 0.680614 0.023 Uiso 1 1 calc R . . . .
H1B H 0.564613 1.015377 0.723825 0.023 Uiso 1 1 calc R . . . .
C2 C 0.46405(14) 0.72154(18) 0.64258(12) 0.0176(6) Uani 1 1 d . . . . .
C3 C 0.39047(14) 0.77277(18) 0.64236(12) 0.0174(6) Uani 1 1 d . . . . .
C4 C 0.31865(14) 0.71778(18) 0.62940(12) 0.0187(6) Uani 1 1 d . . . . .
C5 C 0.32660(14) 0.61984(18) 0.61658(12) 0.0202(6) Uani 1 1 d . . . . .
H5 H 0.279350 0.584012 0.607691 0.024 Uiso 1 1 calc R . . . .
C6 C 0.39929(15) 0.56949(17) 0.61575(13) 0.0206(6) Uani 1 1 d . . . . .
C7 C 0.46733(14) 0.62203(18) 0.62873(12) 0.0199(6) Uani 1 1 d . . . . .
H7 H 0.517418 0.590766 0.628359 0.024 Uiso 1 1 calc R . . . .
C8 C 0.40020(15) 0.45969(18) 0.60160(13) 0.0253(7) Uani 1 1 d . . . . .
C9 C 0.48413(17) 0.4201(2) 0.59998(18) 0.0422(8) Uani 1 1 d . . . . .
H9A H 0.513174 0.454574 0.566828 0.063 Uiso 1 1 calc GR . . . .
H9B H 0.482061 0.351278 0.589201 0.063 Uiso 1 1 calc GR . . . .
H9C H 0.511250 0.428827 0.642870 0.063 Uiso 1 1 calc GR . . . .
C10 C 0.35817(19) 0.4378(2) 0.53545(15) 0.0416(8) Uani 1 1 d . . . . .
H10A H 0.303149 0.460491 0.535667 0.062 Uiso 1 1 calc GR . . . .
H10B H 0.358747 0.368182 0.527571 0.062 Uiso 1 1 calc GR . . . .
H10C H 0.385731 0.470875 0.500773 0.062 Uiso 1 1 calc GR . . . .
C11 C 0.3567(2) 0.4064(2) 0.65480(17) 0.0464(9) Uani 1 1 d . . . . .
H11A H 0.383594 0.418579 0.697389 0.070 Uiso 1 1 calc GR . . . .
H11B H 0.356810 0.337087 0.645710 0.070 Uiso 1 1 calc GR . . . .
H11C H 0.301817 0.429536 0.655358 0.070 Uiso 1 1 calc GR . . . .
C12 C 0.23782(14) 0.76910(18) 0.63117(13) 0.0228(6) Uani 1 1 d . . . . .
C13 C 0.16811(15) 0.6992(2) 0.61804(17) 0.0397(8) Uani 1 1 d . . . . .
H13A H 0.171020 0.672079 0.574044 0.059 Uiso 1 1 calc GR . . . .
H13B H 0.117882 0.733921 0.621455 0.059 Uiso 1 1 calc GR . . . .
H13C H 0.171030 0.646945 0.650268 0.059 Uiso 1 1 calc GR . . . .
C14 C 0.22716(16) 0.81405(19) 0.69881(13) 0.0259(6) Uani 1 1 d . . . . .
H14A H 0.227830 0.763075 0.731931 0.039 Uiso 1 1 calc GR . . . .
H14B H 0.176333 0.848282 0.698767 0.039 Uiso 1 1 calc GR . . . .
H14C H 0.270525 0.859448 0.708827 0.039 Uiso 1 1 calc GR . . . .
C15 C 0.23225(16) 0.8480(2) 0.57853(13) 0.0307(7) Uani 1 1 d . . . . .
H15A H 0.276787 0.892824 0.585093 0.046 Uiso 1 1 calc GR . . . .
H15B H 0.182147 0.883091 0.581694 0.046 Uiso 1 1 calc GR . . . .
H15C H 0.234258 0.818349 0.535220 0.046 Uiso 1 1 calc GR . . . .
C16 C 0.55892(14) 0.86073(17) 0.57526(12) 0.0173(6) Uani 1 1 d . . . . .
C17 C 0.51826(15) 0.83046(18) 0.51803(12) 0.0210(6) Uani 1 1 d . . . . .
H17 H 0.482244 0.777907 0.519168 0.025 Uiso 1 1 calc R . . . .
C18 C 0.53057(15) 0.87732(19) 0.45939(13) 0.0248(6) Uani 1 1 d . . . . .
H18 H 0.502894 0.856675 0.420474 0.030 Uiso 1 1 calc R . . . .
C19 C 0.58295(15) 0.95390(19) 0.45746(13) 0.0226(6) Uani 1 1 d . . . . .
H19 H 0.590749 0.986149 0.417355 0.027 Uiso 1 1 calc R . . . .
C20 C 0.62386(15) 0.98345(18) 0.51376(13) 0.0220(6) Uani 1 1 d . . . . .
H20 H 0.660100 1.035729 0.512185 0.026 Uiso 1 1 calc R . . . .
C21 C 0.61241(15) 0.93730(17) 0.57260(13) 0.0211(6) Uani 1 1 d . . . . .
H21 H 0.640969 0.957786 0.611140 0.025 Uiso 1 1 calc R . . . .
C22 C 0.63393(14) 0.71356(17) 0.65700(12) 0.0175(6) Uani 1 1 d . . . . .
C23 C 0.64016(15) 0.64670(18) 0.70792(13) 0.0234(6) Uani 1 1 d . . . . .
H23 H 0.600543 0.644389 0.739414 0.028 Uiso 1 1 calc R . . . .
C24 C 0.70424(16) 0.58340(19) 0.71268(13) 0.0251(7) Uani 1 1 d . . . . .
H24 H 0.708502 0.538650 0.747750 0.030 Uiso 1 1 calc R . . . .
C25 C 0.76146(16) 0.5853(2) 0.66680(14) 0.0286(7) Uani 1 1 d . . . . .
H25 H 0.804239 0.540769 0.669554 0.034 Uiso 1 1 calc R . . . .
C26 C 0.75664(16) 0.6519(2) 0.61691(14) 0.0315(7) Uani 1 1 d . . . . .
H26 H 0.796948 0.654268 0.586016 0.038 Uiso 1 1 calc R . . . .
C27 C 0.69305(15) 0.71586(19) 0.61148(13) 0.0254(6) Uani 1 1 d . . . . .
H27 H 0.689892 0.761160 0.576703 0.030 Uiso 1 1 calc R . . . .
N N 0.56703(11) 0.87124(14) 0.70986(10) 0.0187(5) Uani 1 1 d . . . . .
H H 0.597730 0.854555 0.749275 0.022 Uiso 1 1 d R . . . .
O O 0.39167(9) 0.86447(12) 0.65464(8) 0.0225(4) Uani 1 1 d . . . . .
P P 0.55036(4) 0.79461(5) 0.65003(3) 0.01778(18) Uani 1 1 d . . . . .
Cl1 Cl 0.4264(10) 0.1844(14) 0.7077(9) 0.024(2) Uiso 0.05 1 d . U P A -1
C28 C 0.505(2) 0.2538(15) 0.743(2) 0.014(10) Uiso 0.05 1 d G U P A -1
H28A H 0.482493 0.312549 0.762157 0.017 Uiso 0.05 1 calc R . P A -1
H28B H 0.539704 0.274292 0.707601 0.017 Uiso 0.05 1 calc R . P A -1
Cl2 Cl 0.5615(10) 0.1910(14) 0.8029(9) 0.024(2) Uiso 0.05 1 d G U P A -1


_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
C1 C1 1.536(5) 2_656 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 N 1.470(3) . ?
C2 C3 1.430(3) . ?
C2 C7 1.411(4) . ?
C2 P 1.775(3) . ?
C3 C4 1.446(3) . ?
C3 O 1.297(3) . ?
C4 C5 1.392(4) . ?
C4 C12 1.540(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.412(4) . ?
C6 C7 1.375(4) . ?
C6 C8 1.551(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.520(4) . ?
C8 C10 1.532(4) . ?
C8 C11 1.531(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.539(4) . ?
C12 C14 1.538(4) . ?
C12 C15 1.537(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.397(4) . ?
C16 C21 1.396(3) . ?
C16 P 1.797(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.390(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.384(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.380(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.386(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.397(4) . ?
C22 C27 1.396(4) . ?
C22 P 1.804(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.393(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.377(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.378(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.392(4) . ?
C27 H27 0.9500 . ?
N H 0.9679 . ?
N P 1.637(2) . ?
Cl1 C28 1.7590 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 Cl2 1.7613 . ?

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
C1 C1 H1A 108.9 2_656 . ?
C1 C1 H1B 108.9 2_656 . ?
H1A C1 H1B 107.7 . . ?
N C1 C1 113.38(15) . 2_656 ?
N C1 H1A 108.9 . . ?
N C1 H1B 108.9 . . ?
C3 C2 P 115.1(2) . . ?
C7 C2 C3 121.8(2) . . ?
C7 C2 P 122.47(19) . . ?
C2 C3 C4 117.3(2) . . ?
O C3 C2 118.7(2) . . ?
O C3 C4 124.0(2) . . ?
C3 C4 C12 119.1(2) . . ?
C5 C4 C3 117.6(2) . . ?
C5 C4 C12 123.3(2) . . ?
C4 C5 H5 117.4 . . ?
C4 C5 C6 125.2(2) . . ?
C6 C5 H5 117.4 . . ?
C5 C6 C8 120.3(2) . . ?
C7 C6 C5 116.9(2) . . ?
C7 C6 C8 122.8(2) . . ?
C2 C7 H7 119.4 . . ?
C6 C7 C2 121.2(2) . . ?
C6 C7 H7 119.4 . . ?
C9 C8 C6 112.1(2) . . ?
C9 C8 C10 107.7(2) . . ?
C9 C8 C11 108.5(3) . . ?
C10 C8 C6 110.6(2) . . ?
C11 C8 C6 109.4(2) . . ?
C11 C8 C10 108.5(2) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C4 112.0(2) . . ?
C14 C12 C4 110.4(2) . . ?
C14 C12 C13 107.1(2) . . ?
C15 C12 C4 109.8(2) . . ?
C15 C12 C13 107.7(2) . . ?
C15 C12 C14 109.7(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 P 120.5(2) . . ?
C21 C16 C17 119.3(2) . . ?
C21 C16 P 119.89(19) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 119.9(2) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 119.9 . . ?
C19 C18 C17 120.3(2) . . ?
C19 C18 H18 119.9 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 120.0(2) . . ?
C20 C19 H19 120.0 . . ?
C19 C20 H20 119.8 . . ?
C19 C20 C21 120.4(2) . . ?
C21 C20 H20 119.8 . . ?
C16 C21 H21 120.0 . . ?
C20 C21 C16 120.0(2) . . ?
C20 C21 H21 120.0 . . ?
C23 C22 P 120.37(19) . . ?
C27 C22 C23 118.8(2) . . ?
C27 C22 P 120.8(2) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 C22 120.2(2) . . ?
C24 C23 H23 119.9 . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.3(3) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 120.0(3) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 119.8 . . ?
C25 C26 C27 120.4(3) . . ?
C27 C26 H26 119.8 . . ?
C22 C27 H27 119.9 . . ?
C26 C27 C22 120.2(3) . . ?
C26 C27 H27 119.9 . . ?
C1 N H 109.5 . . ?
C1 N P 126.52(17) . . ?
P N H 122.5 . . ?
C2 P C16 108.37(12) . . ?
C2 P C22 106.60(14) . . ?
C16 P C22 107.06(12) . . ?
N P C2 123.23(12) . . ?
N P C16 106.81(14) . . ?
N P C22 103.77(12) . . ?
Cl1 C28 H28A 109.0 . . ?
Cl1 C28 H28B 109.0 . . ?
Cl1 C28 Cl2 112.9 . . ?
H28A C28 H28B 107.8 . . ?
Cl2 C28 H28A 109.0 . . ?
Cl2 C28 H28B 109.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C1 N P 112.9(3) 2_656 . . . ?
C1 N P C2 -71.0(2) . . . . ?
C1 N P C16 55.2(2) . . . . ?
C1 N P C22 168.17(19) . . . . ?
C2 C3 C4 C5 -1.5(3) . . . . ?
C2 C3 C4 C12 177.8(2) . . . . ?
C3 C2 C7 C6 -1.4(4) . . . . ?
C3 C2 P C16 -70.5(2) . . . . ?
C3 C2 P C22 174.61(18) . . . . ?
C3 C2 P N 55.1(2) . . . . ?
C3 C4 C5 C6 0.6(4) . . . . ?
C3 C4 C12 C13 -178.5(2) . . . . ?
C3 C4 C12 C14 -59.3(3) . . . . ?
C3 C4 C12 C15 61.9(3) . . . . ?
C4 C5 C6 C7 0.0(4) . . . . ?
C4 C5 C6 C8 179.2(2) . . . . ?
C5 C4 C12 C13 0.7(4) . . . . ?
C5 C4 C12 C14 119.9(3) . . . . ?
C5 C4 C12 C15 -118.9(3) . . . . ?
C5 C6 C7 C2 0.4(4) . . . . ?
C5 C6 C8 C9 177.5(3) . . . . ?
C5 C6 C8 C10 57.3(3) . . . . ?
C5 C6 C8 C11 -62.1(3) . . . . ?
C7 C2 C3 C4 2.0(4) . . . . ?
C7 C2 C3 O -179.1(2) . . . . ?
C7 C2 P C16 101.0(2) . . . . ?
C7 C2 P C22 -13.9(2) . . . . ?
C7 C2 P N -133.4(2) . . . . ?
C7 C6 C8 C9 -3.4(4) . . . . ?
C7 C6 C8 C10 -123.5(3) . . . . ?
C7 C6 C8 C11 117.1(3) . . . . ?
C8 C6 C7 C2 -178.8(2) . . . . ?
C12 C4 C5 C6 -178.7(2) . . . . ?
C16 C17 C18 C19 0.0(4) . . . . ?
C17 C16 C21 C20 1.0(4) . . . . ?
C17 C16 P C2 -18.9(2) . . . . ?
C17 C16 P C22 95.8(2) . . . . ?
C17 C16 P N -153.6(2) . . . . ?
C17 C18 C19 C20 0.7(4) . . . . ?
C18 C19 C20 C21 -0.5(4) . . . . ?
C19 C20 C21 C16 -0.3(4) . . . . ?
C21 C16 C17 C18 -0.8(4) . . . . ?
C21 C16 P C2 167.40(19) . . . . ?
C21 C16 P C22 -78.0(2) . . . . ?
C21 C16 P N 32.7(2) . . . . ?
C22 C23 C24 C25 -0.8(4) . . . . ?
C23 C22 C27 C26 0.4(4) . . . . ?
C23 C22 P C2 -59.0(2) . . . . ?
C23 C22 P C16 -174.83(19) . . . . ?
C23 C22 P N 72.4(2) . . . . ?
C23 C24 C25 C26 1.8(4) . . . . ?
C24 C25 C26 C27 -1.7(4) . . . . ?
C25 C26 C27 C22 0.6(4) . . . . ?
C27 C22 C23 C24 -0.3(4) . . . . ?
C27 C22 P C2 120.4(2) . . . . ?
C27 C22 P C16 4.6(2) . . . . ?
C27 C22 P N -108.1(2) . . . . ?
O C3 C4 C5 179.6(2) . . . . ?
O C3 C4 C12 -1.1(4) . . . . ?
P C2 C3 C4 173.54(18) . . . . ?
P C2 C3 O -7.5(3) . . . . ?
P C2 C7 C6 -172.4(2) . . . . ?
P C16 C17 C18 -174.57(19) . . . . ?
P C16 C21 C20 174.78(19) . . . . ?
P C22 C23 C24 179.18(19) . . . . ?
P C22 C27 C26 -179.1(2) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6c
_database_code_depnum_ccdc_archive 'CCDC 1978295'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne
France
;
_audit_update_record             
;
2020-01-16 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_audit_creation_date             2020-01-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C59 H78 N4 O2 P2 Ti'
_chemical_formula_sum            'C59 H78 N4 O2 P2 Ti'
_chemical_formula_weight         985.09
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   13.449(3)
_cell_length_b                   27.820(7)
_cell_length_c                   14.860(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.910(4)
_cell_angle_gamma                90
_cell_volume                     5507(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7564
_cell_measurement_temperature    115
_cell_measurement_theta_max      23.85
_cell_measurement_theta_min      2.20
_shelx_estimated_absorpt_T_max   0.975
_shelx_estimated_absorpt_T_min   0.950
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0680 before and 0.0607 after correction. The Ratio of minimum to maximum transmission is 0.8954. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2112
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of benzene and pentane  by slow evaporation'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            67556
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.657
_diffrn_reflns_theta_min         2.596
_diffrn_ambient_temperature      115.0
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8710
_reflns_number_total             12796
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         12796
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0560
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0342P)²+4.7140P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1182
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C41B)=Sof(H41d)=Sof(H41e)=Sof(H41f)=Sof(C42B)=Sof(H42d)=Sof(H42e)=
 Sof(H42f)=Sof(C43B)=Sof(H43d)=Sof(H43e)=Sof(H43f)=1-FVAR(1)
 Sof(C41)=Sof(H41a)=Sof(H41b)=Sof(H41c)=Sof(C42)=Sof(H42a)=Sof(H42b)=Sof(H42c)=
 Sof(C43)=Sof(H43a)=Sof(H43b)=Sof(H43c)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
 C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C34(H34), C45(H45), C46(H46),
  C47(H47), C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
4.c Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C15(H15a,H15b,
 H15c), C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C37(H37a,H37b,H37c), C38(H38a,
 H38b,H38c), C39(H39a,H39b,H39c), C41(H41a,H41b,H41c), C41B(H41d,H41e,H41f),
 C42(H42a,H42b,H42c), C42B(H42d,H42e,H42f), C43(H43a,H43b,H43c), C43B(H43d,H43e,
 H43f), C56(H56a,H56b,H56c), C57(H57a,H57b,H57c), C58(H58a,H58b,H58c), C59(H59a,
 H59b,H59c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti Ti 0.47200(3) 0.70590(2) 0.50745(3) 0.01150(10) Uani 1 1 d . . . . .
C1 C 0.29363(18) 0.71517(8) 0.34521(16) 0.0164(5) Uani 1 1 d . . . . .
H1A H 0.282190 0.745594 0.376781 0.020 Uiso 1 1 calc R . . . .
H1B H 0.227439 0.703074 0.316825 0.020 Uiso 1 1 calc R . . . .
N1 N 0.33807(15) 0.67994(7) 0.41275(13) 0.0144(4) Uani 1 1 d . . . . .
O1 O 0.42114(12) 0.66219(6) 0.59218(10) 0.0155(4) Uani 1 1 d . . . . .
P1 P 0.29982(5) 0.62605(2) 0.41657(4) 0.01402(13) Uani 1 1 d . . . . .
C2 C 0.35808(19) 0.72567(9) 0.27043(15) 0.0187(5) Uani 1 1 d . . . . .
H2A H 0.342967 0.701434 0.221681 0.022 Uiso 1 1 calc R . . . .
H2B H 0.339295 0.757574 0.243873 0.022 Uiso 1 1 calc R . . . .
N2 N 0.49882(14) 0.74756(7) 0.39328(12) 0.0129(4) Uani 1 1 d . . . . .
O2 O 0.37616(12) 0.75945(5) 0.52953(10) 0.0140(3) Uani 1 1 d . . . . .
P2 P 0.50954(4) 0.80481(2) 0.40450(4) 0.01245(13) Uani 1 1 d . . . . .
C3 C 0.47030(18) 0.72521(9) 0.30297(15) 0.0160(5) Uani 1 1 d . . . . .
H3A H 0.494092 0.691501 0.305486 0.019 Uiso 1 1 calc R . . . .
H3B H 0.505049 0.742411 0.257989 0.019 Uiso 1 1 calc R . . . .
N3 N 0.56881(15) 0.73675(7) 0.59937(13) 0.0185(5) Uani 1 1 d . . . . .
C4 C 0.36153(17) 0.62572(8) 0.60397(16) 0.0144(5) Uani 1 1 d . . . . .
N4 N 0.56783(15) 0.65748(7) 0.47288(13) 0.0166(4) Uani 1 1 d . . . . .
C5 C 0.36216(18) 0.60559(9) 0.69269(16) 0.0155(5) Uani 1 1 d . . . . .
C6 C 0.30153(19) 0.56592(9) 0.70066(17) 0.0205(6) Uani 1 1 d . . . . .
H6 H 0.301276 0.552628 0.759509 0.025 Uiso 1 1 calc R . . . .
C7 C 0.2405(2) 0.54403(9) 0.62782(18) 0.0228(6) Uani 1 1 d . . . . .
C8 C 0.23980(19) 0.56455(9) 0.54348(17) 0.0203(6) Uani 1 1 d . . . . .
H8 H 0.198311 0.551112 0.492807 0.024 Uiso 1 1 calc R . . . .
C9 C 0.29889(18) 0.60483(8) 0.53055(16) 0.0155(5) Uani 1 1 d . . . . .
C10 C 0.43048(19) 0.62678(9) 0.77492(16) 0.0194(5) Uani 1 1 d . . . . .
C11 C 0.54164(19) 0.62246(10) 0.76165(18) 0.0247(6) Uani 1 1 d . . . . .
H11A H 0.558418 0.588559 0.753977 0.037 Uiso 1 1 calc GR . . . .
H11B H 0.583950 0.635510 0.815016 0.037 Uiso 1 1 calc GR . . . .
H11C H 0.553317 0.640554 0.707498 0.037 Uiso 1 1 calc GR . . . .
C12 C 0.4058(2) 0.68005(9) 0.78663(17) 0.0228(6) Uani 1 1 d . . . . .
H12A H 0.415089 0.697671 0.731309 0.034 Uiso 1 1 calc GR . . . .
H12B H 0.450468 0.693311 0.838306 0.034 Uiso 1 1 calc GR . . . .
H12C H 0.335892 0.683197 0.797756 0.034 Uiso 1 1 calc GR . . . .
C13 C 0.4165(2) 0.60064(10) 0.86356(17) 0.0264(6) Uani 1 1 d . . . . .
H13A H 0.346002 0.602729 0.873300 0.040 Uiso 1 1 calc GR . . . .
H13B H 0.459001 0.615750 0.914640 0.040 Uiso 1 1 calc GR . . . .
H13C H 0.435508 0.566808 0.859186 0.040 Uiso 1 1 calc GR . . . .
C14 C 0.1779(2) 0.49934(11) 0.6444(2) 0.0337(7) Uani 1 1 d . . . . .
C15 C 0.0929(3) 0.51421(14) 0.6961(4) 0.0771(15) Uani 1 1 d . U . . .
H15A H 0.048573 0.536811 0.659270 0.116 Uiso 1 1 calc GR . . . .
H15B H 0.120740 0.529694 0.753317 0.116 Uiso 1 1 calc GR . . . .
H15C H 0.054448 0.485714 0.709185 0.116 Uiso 1 1 calc GR . . . .
C16 C 0.2430(2) 0.46195(11) 0.6987(2) 0.0439(8) Uani 1 1 d . U . . .
H16A H 0.267023 0.474686 0.759300 0.066 Uiso 1 1 calc GR . . . .
H16B H 0.300608 0.454250 0.667424 0.066 Uiso 1 1 calc GR . . . .
H16C H 0.203549 0.432776 0.704447 0.066 Uiso 1 1 calc GR . . . .
C17 C 0.1342(4) 0.47518(17) 0.5553(3) 0.103(2) Uani 1 1 d . U . . .
H17A H 0.098933 0.445717 0.568502 0.155 Uiso 1 1 calc GR . . . .
H17B H 0.188590 0.467183 0.520308 0.155 Uiso 1 1 calc GR . . . .
H17C H 0.086966 0.497149 0.519985 0.155 Uiso 1 1 calc GR . . . .
C18 C 0.17271(18) 0.61961(9) 0.35822(16) 0.0166(5) Uani 1 1 d . . . . .
C19 C 0.0969(2) 0.64715(9) 0.38776(18) 0.0240(6) Uani 1 1 d . . . . .
H19 H 0.111001 0.665716 0.441646 0.029 Uiso 1 1 calc R . . . .
C20 C 0.0009(2) 0.64776(10) 0.3394(2) 0.0294(7) Uani 1 1 d . . . . .
H20 H -0.050282 0.666562 0.360174 0.035 Uiso 1 1 calc R . . . .
C21 C -0.0198(2) 0.62078(10) 0.26049(19) 0.0296(7) Uani 1 1 d . . . . .
H21 H -0.084866 0.621831 0.226248 0.036 Uiso 1 1 calc R . . . .
C22 C 0.0536(2) 0.59256(10) 0.23184(18) 0.0292(7) Uani 1 1 d . . . . .
H22 H 0.038560 0.573541 0.178611 0.035 Uiso 1 1 calc R . . . .
C23 C 0.1499(2) 0.59164(9) 0.28032(17) 0.0233(6) Uani 1 1 d . . . . .
H23 H 0.200095 0.571905 0.260234 0.028 Uiso 1 1 calc R . . . .
C24 C 0.37311(18) 0.58223(9) 0.36274(16) 0.0174(5) Uani 1 1 d . . . . .
C25 C 0.3975(2) 0.53672(9) 0.39807(19) 0.0290(7) Uani 1 1 d . . . . .
H25 H 0.375225 0.527114 0.453322 0.035 Uiso 1 1 calc R . . . .
C26 C 0.4540(2) 0.50526(10) 0.3532(2) 0.0363(7) Uani 1 1 d . . . . .
H26 H 0.470754 0.474438 0.378374 0.044 Uiso 1 1 calc R . . . .
C27 C 0.4858(2) 0.51839(10) 0.2727(2) 0.0307(7) Uani 1 1 d . . . . .
H27 H 0.523759 0.496565 0.241935 0.037 Uiso 1 1 calc R . . . .
C28 C 0.4625(2) 0.56345(10) 0.23667(19) 0.0273(6) Uani 1 1 d . . . . .
H28 H 0.484376 0.572609 0.181032 0.033 Uiso 1 1 calc R . . . .
C29 C 0.40714(19) 0.59528(9) 0.28161(17) 0.0213(6) Uani 1 1 d . . . . .
H29 H 0.392212 0.626354 0.256875 0.026 Uiso 1 1 calc R . . . .
C30 C 0.35454(17) 0.80466(8) 0.51018(15) 0.0132(5) Uani 1 1 d . . . . .
C31 C 0.26966(18) 0.82749(9) 0.54131(16) 0.0162(5) Uani 1 1 d . . . . .
C32 C 0.25436(19) 0.87622(9) 0.52376(17) 0.0198(5) Uani 1 1 d . . . . .
H32 H 0.199236 0.891228 0.546163 0.024 Uiso 1 1 calc R . . . .
C33 C 0.31456(19) 0.90474(9) 0.47534(17) 0.0187(5) Uani 1 1 d . . . . .
C34 C 0.39306(18) 0.88200(8) 0.44242(16) 0.0164(5) Uani 1 1 d . . . . .
H34 H 0.434795 0.899988 0.408206 0.020 Uiso 1 1 calc R . . . .
C35 C 0.41316(17) 0.83277(8) 0.45812(16) 0.0144(5) Uani 1 1 d . . . . .
C36 C 0.19680(19) 0.79879(9) 0.59151(17) 0.0208(5) Uani 1 1 d . . . . .
C37 C 0.1542(2) 0.75604(11) 0.5327(2) 0.0324(7) Uani 1 1 d . . . . .
H37A H 0.121396 0.767883 0.473895 0.049 Uiso 1 1 calc GR . . . .
H37B H 0.105141 0.738813 0.563650 0.049 Uiso 1 1 calc GR . . . .
H37C H 0.208954 0.734213 0.523064 0.049 Uiso 1 1 calc GR . . . .
C38 C 0.2507(2) 0.78026(10) 0.68302(18) 0.0277(6) Uani 1 1 d . . . . .
H38A H 0.306688 0.759437 0.672295 0.042 Uiso 1 1 calc GR . . . .
H38B H 0.203366 0.761969 0.714173 0.042 Uiso 1 1 calc GR . . . .
H38C H 0.276487 0.807593 0.720849 0.042 Uiso 1 1 calc GR . . . .
C39 C 0.1071(2) 0.82939(11) 0.6114(2) 0.0349(7) Uani 1 1 d . . . . .
H39A H 0.131160 0.855717 0.652590 0.052 Uiso 1 1 calc GR . . . .
H39B H 0.060402 0.809274 0.639951 0.052 Uiso 1 1 calc GR . . . .
H39C H 0.072586 0.842687 0.554490 0.052 Uiso 1 1 calc GR . . . .
C40 C 0.2949(2) 0.95876(9) 0.46064(19) 0.0238(6) Uani 1 1 d . . . . .
C41 C 0.1864(11) 0.9706(5) 0.4399(12) 0.056(4) Uani 0.471(16) 1 d . . P A 1
H41A H 0.152149 0.961428 0.491374 0.084 Uiso 0.471(16) 1 calc GR . P A 1
H41B H 0.156997 0.953023 0.385531 0.084 Uiso 0.471(16) 1 calc GR . P A 1
H41C H 0.178512 1.005251 0.429020 0.084 Uiso 0.471(16) 1 calc GR . P A 1
C41B C 0.1899(9) 0.9731(4) 0.4844(8) 0.036(2) Uani 0.529(16) 1 d . . P A 2
H41D H 0.187628 0.967394 0.549103 0.054 Uiso 0.529(16) 1 calc GR . P A 2
H41E H 0.138172 0.953797 0.448159 0.054 Uiso 0.529(16) 1 calc GR . P A 2
H41F H 0.177814 1.007273 0.470768 0.054 Uiso 0.529(16) 1 calc GR . P A 2
C42 C 0.3379(11) 0.9857(3) 0.5517(6) 0.043(3) Uani 0.471(16) 1 d . . P A 1
H42A H 0.410069 0.979418 0.565846 0.064 Uiso 0.471(16) 1 calc GR . P A 1
H42B H 0.303637 0.973960 0.601490 0.064 Uiso 0.471(16) 1 calc GR . P A 1
H42C H 0.326583 1.020332 0.544031 0.064 Uiso 0.471(16) 1 calc GR . P A 1
C42B C 0.3752(7) 0.9863(3) 0.5135(11) 0.057(4) Uani 0.529(16) 1 d . . P A 2
H42D H 0.361317 1.020730 0.505495 0.086 Uiso 0.529(16) 1 calc GR . P A 2
H42E H 0.439328 0.978699 0.492495 0.086 Uiso 0.529(16) 1 calc GR . P A 2
H42F H 0.378701 0.977931 0.577907 0.086 Uiso 0.529(16) 1 calc GR . P A 2
C43 C 0.3509(12) 0.9805(3) 0.3865(7) 0.048(3) Uani 0.471(16) 1 d . . P A 1
H43A H 0.333019 1.014511 0.378127 0.072 Uiso 0.471(16) 1 calc GR . P A 1
H43B H 0.331914 0.963227 0.329217 0.072 Uiso 0.471(16) 1 calc GR . P A 1
H43C H 0.423508 0.977592 0.404914 0.072 Uiso 0.471(16) 1 calc GR . P A 1
C43B C 0.2882(11) 0.9690(3) 0.3559(7) 0.050(3) Uani 0.529(16) 1 d . . P A 2
H43D H 0.271865 1.002969 0.344036 0.075 Uiso 0.529(16) 1 calc GR . P A 2
H43E H 0.235801 0.948843 0.322668 0.075 Uiso 0.529(16) 1 calc GR . P A 2
H43F H 0.352904 0.961666 0.335641 0.075 Uiso 0.529(16) 1 calc GR . P A 2
C44 C 0.63089(18) 0.82132(8) 0.46650(15) 0.0147(5) Uani 1 1 d . . . . .
C45 C 0.71474(18) 0.79325(9) 0.45863(16) 0.0196(5) Uani 1 1 d . . . . .
H45 H 0.707736 0.764615 0.423481 0.023 Uiso 1 1 calc R . . . .
C46 C 0.80850(19) 0.80678(10) 0.50175(17) 0.0231(6) Uani 1 1 d . . . . .
H46 H 0.865375 0.787305 0.496252 0.028 Uiso 1 1 calc R . . . .
C47 C 0.81968(19) 0.84835(10) 0.55259(17) 0.0221(6) Uani 1 1 d . . . . .
H47 H 0.884123 0.857632 0.581772 0.027 Uiso 1 1 calc R . . . .
C48 C 0.7368(2) 0.87644(10) 0.56091(18) 0.0253(6) Uani 1 1 d . . . . .
H48 H 0.744458 0.905205 0.595622 0.030 Uiso 1 1 calc R . . . .
C49 C 0.6427(2) 0.86292(9) 0.51897(17) 0.0222(6) Uani 1 1 d . . . . .
H49 H 0.585908 0.882129 0.526001 0.027 Uiso 1 1 calc R . . . .
C50 C 0.50467(18) 0.83331(8) 0.29387(16) 0.0144(5) Uani 1 1 d . . . . .
C51 C 0.59202(19) 0.83768(9) 0.25353(16) 0.0190(5) Uani 1 1 d . . . . .
H51 H 0.655011 0.829554 0.287204 0.023 Uiso 1 1 calc R . . . .
C52 C 0.5877(2) 0.85375(10) 0.16479(17) 0.0244(6) Uani 1 1 d . . . . .
H52 H 0.647544 0.856354 0.137767 0.029 Uiso 1 1 calc R . . . .
C53 C 0.4966(2) 0.86596(10) 0.11567(18) 0.0272(6) Uani 1 1 d . . . . .
H53 H 0.493689 0.876926 0.054818 0.033 Uiso 1 1 calc R . . . .
C54 C 0.4089(2) 0.86225(9) 0.15513(17) 0.0241(6) Uani 1 1 d . . . . .
H54 H 0.346320 0.870927 0.121382 0.029 Uiso 1 1 calc R . . . .
C55 C 0.41284(19) 0.84595(9) 0.24339(17) 0.0192(5) Uani 1 1 d . . . . .
H55 H 0.352737 0.843310 0.269961 0.023 Uiso 1 1 calc R . . . .
C56 C 0.5511(2) 0.77407(10) 0.66427(17) 0.0268(6) Uani 1 1 d . . . . .
H56A H 0.482268 0.786122 0.649770 0.040 Uiso 1 1 calc GR . . . .
H56B H 0.598515 0.800530 0.660837 0.040 Uiso 1 1 calc GR . . . .
H56C H 0.560551 0.760628 0.725818 0.040 Uiso 1 1 calc GR . . . .
C57 C 0.6709(2) 0.71943(11) 0.62455(19) 0.0305(7) Uani 1 1 d . . . . .
H57A H 0.678829 0.707268 0.687018 0.046 Uiso 1 1 calc GR . . . .
H57B H 0.718247 0.745859 0.620306 0.046 Uiso 1 1 calc GR . . . .
H57C H 0.684506 0.693507 0.583285 0.046 Uiso 1 1 calc GR . . . .
C58 C 0.6455(2) 0.66280(10) 0.41425(18) 0.0250(6) Uani 1 1 d . . . . .
H58A H 0.639950 0.694616 0.385680 0.037 Uiso 1 1 calc GR . . . .
H58B H 0.636968 0.637938 0.367098 0.037 Uiso 1 1 calc GR . . . .
H58C H 0.711685 0.659434 0.450513 0.037 Uiso 1 1 calc GR . . . .
C59 C 0.5825(2) 0.61008(9) 0.51502(19) 0.0257(6) Uani 1 1 d . . . . .
H59A H 0.646959 0.609379 0.554880 0.039 Uiso 1 1 calc GR . . . .
H59B H 0.582507 0.585570 0.467652 0.039 Uiso 1 1 calc GR . . . .
H59C H 0.528045 0.603514 0.550789 0.039 Uiso 1 1 calc GR . . . .


_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
Ti N1 2.247(2) . ?
Ti O1 1.9414(17) . ?
Ti N2 2.126(2) . ?
Ti O2 2.0260(16) . ?
Ti N3 1.951(2) . ?
Ti N4 1.980(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 N1 1.470(3) . ?
C1 C2 1.529(3) . ?
N1 P1 1.589(2) . ?
O1 C4 1.320(3) . ?
P1 C9 1.795(2) . ?
P1 C18 1.816(2) . ?
P1 C24 1.820(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.520(3) . ?
N2 P2 1.606(2) . ?
N2 C3 1.481(3) . ?
O2 C30 1.314(3) . ?
P2 C35 1.790(2) . ?
P2 C44 1.819(2) . ?
P2 C50 1.818(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N3 C56 1.459(3) . ?
N3 C57 1.455(3) . ?
C4 C5 1.431(3) . ?
C4 C9 1.409(3) . ?
N4 C58 1.456(3) . ?
N4 C59 1.461(3) . ?
C5 C6 1.387(3) . ?
C5 C10 1.541(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.404(4) . ?
C7 C8 1.376(3) . ?
C7 C14 1.540(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.402(3) . ?
C10 C11 1.539(4) . ?
C10 C12 1.534(3) . ?
C10 C13 1.539(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.520(5) . ?
C14 C16 1.519(4) . ?
C14 C17 1.528(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.394(4) . ?
C18 C23 1.394(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.388(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.387(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.374(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.393(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.393(3) . ?
C24 C29 1.395(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.388(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.375(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.382(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.386(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.437(3) . ?
C30 C35 1.414(3) . ?
C31 C32 1.391(3) . ?
C31 C36 1.535(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.401(3) . ?
C33 C34 1.377(3) . ?
C33 C40 1.536(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.409(3) . ?
C36 C37 1.539(4) . ?
C36 C38 1.539(3) . ?
C36 C39 1.538(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.487(15) . ?
C40 C41B 1.554(12) . ?
C40 C42 1.584(9) . ?
C40 C42B 1.461(9) . ?
C40 C43 1.542(9) . ?
C40 C43B 1.573(9) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C41B H41D 0.9800 . ?
C41B H41E 0.9800 . ?
C41B H41F 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C42B H42D 0.9800 . ?
C42B H42E 0.9800 . ?
C42B H42F 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C43B H43D 0.9800 . ?
C43B H43E 0.9800 . ?
C43B H43F 0.9800 . ?
C44 C45 1.390(3) . ?
C44 C49 1.392(3) . ?
C45 H45 0.9500 . ?
C45 C46 1.386(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.378(4) . ?
C47 H47 0.9500 . ?
C47 C48 1.380(4) . ?
C48 H48 0.9500 . ?
C48 C49 1.383(4) . ?
C49 H49 0.9500 . ?
C50 C51 1.396(3) . ?
C50 C55 1.399(3) . ?
C51 H51 0.9500 . ?
C51 C52 1.386(3) . ?
C52 H52 0.9500 . ?
C52 C53 1.380(4) . ?
C53 H53 0.9500 . ?
C53 C54 1.391(4) . ?
C54 H54 0.9500 . ?
C54 C55 1.382(3) . ?
C55 H55 0.9500 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti N1 83.19(7) . . ?
O1 Ti N2 166.56(7) . . ?
O1 Ti O2 93.83(7) . . ?
O1 Ti N3 94.71(8) . . ?
O1 Ti N4 92.42(8) . . ?
N2 Ti N1 83.38(7) . . ?
O2 Ti N1 82.23(7) . . ?
O2 Ti N2 84.83(7) . . ?
N3 Ti N1 168.48(8) . . ?
N3 Ti N2 98.55(8) . . ?
N3 Ti O2 86.63(8) . . ?
N3 Ti N4 94.91(9) . . ?
N4 Ti N1 96.50(8) . . ?
N4 Ti N2 88.62(8) . . ?
N4 Ti O2 173.43(8) . . ?
H1A C1 H1B 107.7 . . ?
N1 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
N1 C1 C2 113.9(2) . . ?
C2 C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
C1 N1 Ti 115.41(14) . . ?
C1 N1 P1 123.40(16) . . ?
P1 N1 Ti 121.10(10) . . ?
C4 O1 Ti 147.39(15) . . ?
N1 P1 C9 112.85(11) . . ?
N1 P1 C18 111.35(11) . . ?
N1 P1 C24 114.75(11) . . ?
C9 P1 C18 106.84(11) . . ?
C9 P1 C24 105.60(11) . . ?
C18 P1 C24 104.79(11) . . ?
C1 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C3 C2 C1 113.87(19) . . ?
C3 C2 H2A 108.8 . . ?
C3 C2 H2B 108.8 . . ?
P2 N2 Ti 118.72(10) . . ?
C3 N2 Ti 116.29(14) . . ?
C3 N2 P2 121.26(16) . . ?
C30 O2 Ti 142.66(15) . . ?
N2 P2 C35 114.65(11) . . ?
N2 P2 C44 111.37(11) . . ?
N2 P2 C50 110.30(10) . . ?
C35 P2 C44 108.60(11) . . ?
C35 P2 C50 105.95(11) . . ?
C50 P2 C44 105.43(11) . . ?
C2 C3 H3A 108.8 . . ?
C2 C3 H3B 108.8 . . ?
N2 C3 C2 114.00(19) . . ?
N2 C3 H3A 108.8 . . ?
N2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.6 . . ?
C56 N3 Ti 128.45(17) . . ?
C57 N3 Ti 123.33(17) . . ?
C57 N3 C56 107.5(2) . . ?
O1 C4 C5 119.8(2) . . ?
O1 C4 C9 121.6(2) . . ?
C9 C4 C5 118.6(2) . . ?
C58 N4 Ti 129.17(16) . . ?
C58 N4 C59 106.4(2) . . ?
C59 N4 Ti 123.86(16) . . ?
C4 C5 C10 120.5(2) . . ?
C6 C5 C4 117.4(2) . . ?
C6 C5 C10 122.0(2) . . ?
C5 C6 H6 117.7 . . ?
C5 C6 C7 124.6(2) . . ?
C7 C6 H6 117.7 . . ?
C6 C7 C14 120.1(2) . . ?
C8 C7 C6 116.9(2) . . ?
C8 C7 C14 123.0(2) . . ?
C7 C8 H8 119.2 . . ?
C7 C8 C9 121.6(2) . . ?
C9 C8 H8 119.2 . . ?
C4 C9 P1 120.92(18) . . ?
C8 C9 P1 118.01(18) . . ?
C8 C9 C4 120.9(2) . . ?
C11 C10 C5 110.6(2) . . ?
C12 C10 C5 110.2(2) . . ?
C12 C10 C11 108.6(2) . . ?
C12 C10 C13 107.8(2) . . ?
C13 C10 C5 111.6(2) . . ?
C13 C10 C11 108.0(2) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C7 109.1(3) . . ?
C15 C14 C17 109.4(4) . . ?
C16 C14 C7 110.5(2) . . ?
C16 C14 C15 109.7(3) . . ?
C16 C14 C17 106.5(3) . . ?
C17 C14 C7 111.7(2) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 P1 118.49(19) . . ?
C23 C18 P1 122.5(2) . . ?
C23 C18 C19 118.8(2) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 C18 120.8(3) . . ?
C20 C19 H19 119.6 . . ?
C19 C20 H20 120.1 . . ?
C21 C20 C19 119.7(3) . . ?
C21 C20 H20 120.1 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.1(3) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 119.8 . . ?
C21 C22 C23 120.4(3) . . ?
C23 C22 H22 119.8 . . ?
C18 C23 H23 119.9 . . ?
C22 C23 C18 120.2(3) . . ?
C22 C23 H23 119.9 . . ?
C25 C24 P1 123.8(2) . . ?
C25 C24 C29 118.3(2) . . ?
C29 C24 P1 117.86(18) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 C24 120.6(3) . . ?
C26 C25 H25 119.7 . . ?
C25 C26 H26 119.8 . . ?
C27 C26 C25 120.5(3) . . ?
C27 C26 H26 119.8 . . ?
C26 C27 H27 120.1 . . ?
C26 C27 C28 119.8(3) . . ?
C28 C27 H27 120.1 . . ?
C27 C28 H28 120.0 . . ?
C27 C28 C29 120.1(3) . . ?
C29 C28 H28 120.0 . . ?
C24 C29 H29 119.6 . . ?
C28 C29 C24 120.8(2) . . ?
C28 C29 H29 119.6 . . ?
O2 C30 C31 120.9(2) . . ?
O2 C30 C35 121.7(2) . . ?
C35 C30 C31 117.3(2) . . ?
C30 C31 C36 121.0(2) . . ?
C32 C31 C30 118.3(2) . . ?
C32 C31 C36 120.7(2) . . ?
C31 C32 H32 117.7 . . ?
C31 C32 C33 124.6(2) . . ?
C33 C32 H32 117.7 . . ?
C32 C33 C40 121.8(2) . . ?
C34 C33 C32 116.6(2) . . ?
C34 C33 C40 121.6(2) . . ?
C33 C34 H34 119.1 . . ?
C33 C34 C35 121.8(2) . . ?
C35 C34 H34 119.1 . . ?
C30 C35 P2 119.71(17) . . ?
C34 C35 P2 118.87(18) . . ?
C34 C35 C30 121.3(2) . . ?
C31 C36 C37 109.8(2) . . ?
C31 C36 C38 110.4(2) . . ?
C31 C36 C39 112.1(2) . . ?
C37 C36 C38 109.7(2) . . ?
C39 C36 C37 107.2(2) . . ?
C39 C36 C38 107.6(2) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C33 C40 C41B 111.3(5) . . ?
C33 C40 C42 107.8(4) . . ?
C33 C40 C43 113.2(4) . . ?
C33 C40 C43B 107.7(3) . . ?
C41 C40 C33 113.0(6) . . ?
C41 C40 C42 107.7(7) . . ?
C41 C40 C43 109.1(6) . . ?
C41B C40 C43B 104.3(5) . . ?
C42B C40 C33 109.7(4) . . ?
C42B C40 C41B 111.7(6) . . ?
C42B C40 C43B 112.0(6) . . ?
C43 C40 C42 105.6(5) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C41B H41D 109.5 . . ?
C40 C41B H41E 109.5 . . ?
C40 C41B H41F 109.5 . . ?
H41D C41B H41E 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C42B H42D 109.5 . . ?
C40 C42B H42E 109.5 . . ?
C40 C42B H42F 109.5 . . ?
H42D C42B H42E 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C40 C43B H43D 109.5 . . ?
C40 C43B H43E 109.5 . . ?
C40 C43B H43F 109.5 . . ?
H43D C43B H43E 109.5 . . ?
H43D C43B H43F 109.5 . . ?
H43E C43B H43F 109.5 . . ?
C45 C44 P2 119.82(18) . . ?
C45 C44 C49 118.9(2) . . ?
C49 C44 P2 121.26(19) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 C44 120.4(2) . . ?
C46 C45 H45 119.8 . . ?
C45 C46 H46 119.8 . . ?
C47 C46 C45 120.3(2) . . ?
C47 C46 H46 119.8 . . ?
C46 C47 H47 120.1 . . ?
C46 C47 C48 119.7(2) . . ?
C48 C47 H47 120.1 . . ?
C47 C48 H48 119.8 . . ?
C47 C48 C49 120.4(2) . . ?
C49 C48 H48 119.8 . . ?
C44 C49 H49 119.8 . . ?
C48 C49 C44 120.4(2) . . ?
C48 C49 H49 119.8 . . ?
C51 C50 P2 119.91(18) . . ?
C51 C50 C55 118.8(2) . . ?
C55 C50 P2 120.91(18) . . ?
C50 C51 H51 119.7 . . ?
C52 C51 C50 120.6(2) . . ?
C52 C51 H51 119.7 . . ?
C51 C52 H52 120.0 . . ?
C53 C52 C51 120.0(2) . . ?
C53 C52 H52 120.0 . . ?
C52 C53 H53 120.0 . . ?
C52 C53 C54 120.1(2) . . ?
C54 C53 H53 120.0 . . ?
C53 C54 H54 120.0 . . ?
C55 C54 C53 120.1(2) . . ?
C55 C54 H54 120.0 . . ?
C50 C55 H55 119.8 . . ?
C54 C55 C50 120.5(2) . . ?
C54 C55 H55 119.8 . . ?
N3 C56 H56A 109.5 . . ?
N3 C56 H56B 109.5 . . ?
N3 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N3 C57 H57A 109.5 . . ?
N3 C57 H57B 109.5 . . ?
N3 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
N4 C58 H58A 109.5 . . ?
N4 C58 H58B 109.5 . . ?
N4 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
N4 C59 H59A 109.5 . . ?
N4 C59 H59B 109.5 . . ?
N4 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT213_6c                  
;
PROBLEM: Atom C17 has ADP max/min Ratio ..... 4.4 prolat
RESPONSE: 
C17 belongs to a tert-Bu group whose position seems to fluctuate 
slightly around an average position. 
We let the ADP ellipsoids taking account for that. 
;
####################################################################### 
# 
# 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_1bH2
_database_code_depnum_ccdc_archive 'CCDC 1978292'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne
France
;
_audit_update_record             
;
2020-01-16 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_audit_creation_date             2019-11-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C58 H65.96 Br0.04 N2 O2 P2, 0.96(C5 H12)'
_chemical_formula_sum            'C62.79 H77.45 Br0.04 N2 O2 P2'
_chemical_formula_weight         957.33
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.628
_cell_length_b                   15.392
_cell_length_c                   19.387
_cell_angle_alpha                73.03
_cell_angle_beta                 82.93
_cell_angle_gamma                88.87
_cell_volume                     2726.5
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.69
_cell_measurement_theta_min      2.41
_shelx_estimated_absorpt_T_max   0.947
_shelx_estimated_absorpt_T_min   0.688
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0873 before and 0.0563 after correction. The Ratio of minimum to maximum transmission is 0.8661. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1031
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25461
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        66.781
_diffrn_reflns_theta_max         66.781
_diffrn_reflns_theta_min         2.401
_diffrn_ambient_temperature      100
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Cu'
_diffrn_measurement_method       "φ and ω scans'"
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'QUAZAR MX multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'high brilliance microfocus sealed tube, Cu'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7729
_reflns_number_total             9579
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.970
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         9579
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0553
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0635P)²+3.6206P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1467
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C63-C62
 1.471 with sigma of 0.02
 C60-C59
 1.471 with sigma of 0.02
 C62-C61
 1.457 with sigma of 0.02
 C61-C60
 1.457 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C59, C60, C61, C62, C63
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{C63, C62, C61, C60, C59} sigma for 1-2: 0.02, 1-3: 0.04
as
{C59, C60, C61, C62, C63}
5. Others
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=1-FVAR(1)
 Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19B)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=FVAR(1)
 Sof(Br)=1-FVAR(2)
 Sof(H5)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C60)=Sof(H60A)=Sof(H60B)=
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(C63)=Sof(H63A)=
 Sof(H63B)=Sof(H63C)=FVAR(2)
 Sof(C44B)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C45B)=Sof(H45D)=Sof(H45E)=
 Sof(H45F)=Sof(C46B)=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(3)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C12(H12), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
  C36(H36), C38(H38), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
 C54(H54), C55(H55), C56(H56), C57(H57), C58(H58)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C18B(H18D,H18E,H18F), C19(H19A,H19B,H19C), C19B(H19D,H19E,H19F),
 C20(H20A,H20B,H20C), C20B(H20D,H20E,H20F), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C44B(H44D,H44E,H44F),
 C45(H45A,H45B,H45C), C45B(H45D,H45E,H45F), C46(H46A,H46B,H46C), C46B(H46D,H46E,
 H46F), C59(H59A,H59B,H59C), C63(H63A,H63B,H63C)
6.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br 0.6391(8) 0.7502(6) 0.3668(4) 0.035(3) Uani 0.0424(15) 1 d . . P A 2
C1 C 0.6445(2) 0.77895(16) 0.57135(13) 0.0136(5) Uani 1 1 d . . . . .
C2 C 0.5419(2) 0.84528(16) 0.57520(12) 0.0133(5) Uani 1 1 d . . . . .
C3 C 0.4680(2) 0.88142(17) 0.51617(13) 0.0169(5) Uani 1 1 d . . . . .
H3 H 0.401747 0.927477 0.518132 0.020 Uiso 1 1 calc R . . . .
C4 C 0.4885(3) 0.85196(18) 0.45453(13) 0.0187(5) Uani 1 1 d . . . . .
H4 H 0.436066 0.877134 0.415127 0.022 Uiso 1 1 calc R . . . .
C5 C 0.5863(3) 0.78533(17) 0.45097(13) 0.0177(5) Uani 1 1 d . . . . .
H5 H 0.600076 0.763880 0.409428 0.021 Uiso 0.9576(15) 1 calc R . P A 1
C6 C 0.6639(2) 0.75023(17) 0.50854(13) 0.0164(5) Uani 1 1 d . . . . .
H6 H 0.731988 0.705610 0.505241 0.020 Uiso 1 1 calc R . . . .
C7 C 0.7904(2) 0.62339(17) 0.75287(13) 0.0159(5) Uani 1 1 d . . . . .
C8 C 0.7738(2) 0.69051(17) 0.78958(13) 0.0166(5) Uani 1 1 d . . . . .
C9 C 0.7632(3) 0.66398(18) 0.86632(14) 0.0193(5) Uani 1 1 d . . . . .
C10 C 0.7728(3) 0.57184(19) 0.90193(14) 0.0206(6) Uani 1 1 d . . . . .
H10 H 0.767070 0.553733 0.953442 0.025 Uiso 1 1 calc R . . . .
C11 C 0.7902(3) 0.50443(18) 0.86699(14) 0.0198(5) Uani 1 1 d . . . . .
C12 C 0.7972(2) 0.53185(18) 0.79167(14) 0.0176(5) Uani 1 1 d . . . . .
H12 H 0.806833 0.487472 0.766189 0.021 Uiso 1 1 calc R . . . .
C13 C 0.7415(3) 0.7344(2) 0.90897(14) 0.0257(6) Uani 1 1 d . . . . .
C14 C 0.6060(3) 0.7867(2) 0.89241(16) 0.0345(7) Uani 1 1 d . . . . .
H14A H 0.590966 0.829320 0.921477 0.052 Uiso 1 1 calc GR . . . .
H14B H 0.526720 0.743726 0.904529 0.052 Uiso 1 1 calc GR . . . .
H14C H 0.613876 0.820436 0.840657 0.052 Uiso 1 1 calc GR . . . .
C15 C 0.7275(4) 0.6893(2) 0.99173(15) 0.0356(7) Uani 1 1 d . . . . .
H15A H 0.812041 0.654888 1.004477 0.053 Uiso 1 1 calc GR . . . .
H15B H 0.645860 0.648083 1.006490 0.053 Uiso 1 1 calc GR . . . .
H15C H 0.715661 0.736237 1.016843 0.053 Uiso 1 1 calc GR . . . .
C16 C 0.8675(3) 0.8000(2) 0.88932(16) 0.0296(6) Uani 1 1 d . . . . .
H16A H 0.877046 0.832062 0.837207 0.044 Uiso 1 1 calc GR . . . .
H16B H 0.952577 0.765837 0.901183 0.044 Uiso 1 1 calc GR . . . .
H16C H 0.853346 0.844222 0.917010 0.044 Uiso 1 1 calc GR . . . .
C17 C 0.7995(3) 0.4044(2) 0.91024(16) 0.0302(7) Uani 1 1 d . . . . .
C18 C 0.9291(6) 0.4008(4) 0.9564(3) 0.0299(14) Uani 0.544(6) 1 d . . P B 1
H18A H 0.936439 0.339195 0.988858 0.045 Uiso 0.544(6) 1 calc GR . P B 1
H18B H 0.913722 0.443635 0.985236 0.045 Uiso 0.544(6) 1 calc GR . P B 1
H18C H 1.015992 0.417387 0.923080 0.045 Uiso 0.544(6) 1 calc GR . P B 1
C18B C 0.7970(11) 0.3813(5) 0.9882(4) 0.051(3) Uani 0.456(6) 1 d . . P B 2
H18D H 0.797889 0.315075 1.008675 0.076 Uiso 0.456(6) 1 calc GR . P B 2
H18E H 0.711881 0.404993 1.009089 0.076 Uiso 0.456(6) 1 calc GR . P B 2
H18F H 0.879359 0.408078 0.999790 0.076 Uiso 0.456(6) 1 calc GR . P B 2
C19 C 0.6695(7) 0.3791(4) 0.9671(3) 0.0385(16) Uani 0.544(6) 1 d . . P B 1
H19A H 0.585812 0.381943 0.942431 0.058 Uiso 0.544(6) 1 calc GR . P B 1
H19B H 0.660881 0.421760 0.996212 0.058 Uiso 0.544(6) 1 calc GR . P B 1
H19C H 0.678814 0.317280 0.998900 0.058 Uiso 0.544(6) 1 calc GR . P B 1
C19B C 0.6634(8) 0.3516(5) 0.8940(4) 0.041(2) Uani 0.456(6) 1 d . . P B 2
H19D H 0.667063 0.360839 0.841649 0.061 Uiso 0.456(6) 1 calc GR . P B 2
H19E H 0.576326 0.376367 0.911844 0.061 Uiso 0.456(6) 1 calc GR . P B 2
H19F H 0.666710 0.286462 0.919111 0.061 Uiso 0.456(6) 1 calc GR . P B 2
C20 C 0.8247(8) 0.3445(4) 0.8660(3) 0.0349(16) Uani 0.544(6) 1 d . . P B 1
H20A H 0.910302 0.363966 0.832168 0.052 Uiso 0.544(6) 1 calc GR . P B 1
H20B H 0.745406 0.346085 0.838423 0.052 Uiso 0.544(6) 1 calc GR . P B 1
H20C H 0.835605 0.282507 0.896973 0.052 Uiso 0.544(6) 1 calc GR . P B 1
C20B C 0.9259(9) 0.3566(5) 0.8767(4) 0.040(2) Uani 0.456(6) 1 d . . P B 2
H20D H 0.918876 0.365502 0.825098 0.060 Uiso 0.456(6) 1 calc GR . P B 2
H20E H 0.922917 0.291462 0.902385 0.060 Uiso 0.456(6) 1 calc GR . P B 2
H20F H 1.014363 0.383185 0.881802 0.060 Uiso 0.456(6) 1 calc GR . P B 2
C21 C 0.7381(3) 0.56087(16) 0.62894(13) 0.0156(5) Uani 1 1 d . . . . .
C22 C 0.8244(3) 0.5089(2) 0.59438(16) 0.0264(6) Uani 1 1 d . . . . .
H22 H 0.922950 0.518533 0.587473 0.032 Uiso 1 1 calc R . . . .
C23 C 0.7669(3) 0.4429(2) 0.56985(19) 0.0355(7) Uani 1 1 d . . . . .
H23 H 0.826240 0.407030 0.546685 0.043 Uiso 1 1 calc R . . . .
C24 C 0.6239(3) 0.4295(2) 0.57909(17) 0.0295(7) Uani 1 1 d . . . . .
H24 H 0.584851 0.384764 0.561836 0.035 Uiso 1 1 calc R . . . .
C25 C 0.5372(3) 0.4809(2) 0.61338(16) 0.0289(6) Uani 1 1 d . . . . .
H25 H 0.438666 0.471468 0.619751 0.035 Uiso 1 1 calc R . . . .
C26 C 0.5942(3) 0.54606(19) 0.63845(15) 0.0235(6) Uani 1 1 d . . . . .
H26 H 0.534385 0.580968 0.662361 0.028 Uiso 1 1 calc R . . . .
C27 C 0.9884(2) 0.66265(16) 0.62245(13) 0.0140(5) Uani 1 1 d . . . . .
C28 C 1.0338(3) 0.71935(17) 0.55244(13) 0.0171(5) Uani 1 1 d . . . . .
H28 H 0.967724 0.752611 0.522774 0.020 Uiso 1 1 calc R . . . .
C29 C 1.1754(3) 0.72666(18) 0.52671(14) 0.0197(5) Uani 1 1 d . . . . .
H29 H 1.206300 0.764699 0.479253 0.024 Uiso 1 1 calc R . . . .
C30 C 1.2721(3) 0.67846(18) 0.57020(14) 0.0192(5) Uani 1 1 d . . . . .
H30 H 1.369093 0.683936 0.552709 0.023 Uiso 1 1 calc R . . . .
C31 C 1.2268(3) 0.62239(18) 0.63915(14) 0.0201(5) Uani 1 1 d . . . . .
H31 H 1.293148 0.589202 0.668666 0.024 Uiso 1 1 calc R . . . .
C32 C 1.0856(3) 0.61427(17) 0.66545(14) 0.0185(5) Uani 1 1 d . . . . .
H32 H 1.055472 0.575687 0.712802 0.022 Uiso 1 1 calc R . . . .
C33 C 0.4339(3) 0.94389(17) 0.74748(13) 0.0154(5) Uani 1 1 d . . . . .
C34 C 0.5616(3) 0.99334(17) 0.73341(13) 0.0161(5) Uani 1 1 d . . . . .
C35 C 0.5862(3) 1.04789(18) 0.77847(14) 0.0196(5) Uani 1 1 d . . . . .
C36 C 0.4857(3) 1.04675(18) 0.83672(14) 0.0201(5) Uani 1 1 d . . . . .
H36 H 0.503012 1.082603 0.867301 0.024 Uiso 1 1 calc R . . . .
C37 C 0.3607(3) 0.99603(18) 0.85310(14) 0.0184(5) Uani 1 1 d . . . . .
C38 C 0.3370(3) 0.94560(17) 0.80690(13) 0.0170(5) Uani 1 1 d . . . . .
H38 H 0.252424 0.911173 0.815925 0.020 Uiso 1 1 calc R . . . .
C39 C 0.7230(3) 1.10432(19) 0.76397(15) 0.0232(6) Uani 1 1 d . . . . .
C40 C 0.7409(3) 1.17001(19) 0.68595(15) 0.0278(6) Uani 1 1 d . . . . .
H40A H 0.824281 1.208531 0.679002 0.042 Uiso 1 1 calc GR . . . .
H40B H 0.658188 1.208221 0.678532 0.042 Uiso 1 1 calc GR . . . .
H40C H 0.751373 1.134912 0.650856 0.042 Uiso 1 1 calc GR . . . .
C41 C 0.8478(3) 1.0407(2) 0.77392(16) 0.0291(7) Uani 1 1 d . . . . .
H41A H 0.935043 1.076668 0.760998 0.044 Uiso 1 1 calc GR . . . .
H41B H 0.846698 1.001199 0.742420 0.044 Uiso 1 1 calc GR . . . .
H41C H 0.841688 1.003321 0.824730 0.044 Uiso 1 1 calc GR . . . .
C42 C 0.7245(4) 1.1618(2) 0.81607(18) 0.0393(8) Uani 1 1 d . . . . .
H42A H 0.717236 1.121914 0.866130 0.059 Uiso 1 1 calc GR . . . .
H42B H 0.645142 1.203033 0.810724 0.059 Uiso 1 1 calc GR . . . .
H42C H 0.812139 1.197220 0.804819 0.059 Uiso 1 1 calc GR . . . .
C43 C 0.2527(3) 0.99472(19) 0.91858(14) 0.0217(6) Uani 1 1 d . . . . .
C44 C 0.2969(4) 1.0539(3) 0.9635(2) 0.0332(10) Uani 0.835(5) 1 d . . P C 1
H44A H 0.385662 1.032332 0.981668 0.050 Uiso 0.835(5) 1 calc GR . P C 1
H44B H 0.224697 1.050361 1.004552 0.050 Uiso 0.835(5) 1 calc GR . P C 1
H44C H 0.308625 1.117108 0.932901 0.050 Uiso 0.835(5) 1 calc GR . P C 1
C44B C 0.173(2) 1.0938(14) 0.9010(11) 0.040(5) Uani 0.165(5) 1 d . . P C 2
H44D H 0.238456 1.141197 0.902375 0.061 Uiso 0.165(5) 1 calc GR . P C 2
H44E H 0.091919 1.090408 0.937485 0.061 Uiso 0.165(5) 1 calc GR . P C 2
H44F H 0.142347 1.108510 0.852622 0.061 Uiso 0.165(5) 1 calc GR . P C 2
C45 C 0.1141(3) 1.0260(3) 0.89197(19) 0.0298(9) Uani 0.835(5) 1 d . . P C 1
H45A H 0.124270 1.088449 0.859786 0.045 Uiso 0.835(5) 1 calc GR . P C 1
H45B H 0.043859 1.023929 0.933597 0.045 Uiso 0.835(5) 1 calc GR . P C 1
H45C H 0.084037 0.986071 0.865240 0.045 Uiso 0.835(5) 1 calc GR . P C 1
C45B C 0.1268(19) 0.9271(13) 0.9306(9) 0.030(5) Uani 0.165(5) 1 d . . P C 2
H45D H 0.077923 0.942800 0.887234 0.045 Uiso 0.165(5) 1 calc GR . P C 2
H45E H 0.061993 0.931029 0.972638 0.045 Uiso 0.165(5) 1 calc GR . P C 2
H45F H 0.161679 0.865026 0.939363 0.045 Uiso 0.165(5) 1 calc GR . P C 2
C46 C 0.2370(4) 0.8960(2) 0.96905(18) 0.0293(9) Uani 0.835(5) 1 d . . P C 1
H46A H 0.206328 0.856293 0.942245 0.044 Uiso 0.835(5) 1 calc GR . P C 1
H46B H 0.167435 0.893598 1.010983 0.044 Uiso 0.835(5) 1 calc GR . P C 1
H46C H 0.327294 0.875504 0.985869 0.044 Uiso 0.835(5) 1 calc GR . P C 1
C46B C 0.3169(19) 0.9795(16) 0.9870(10) 0.032(5) Uani 0.165(5) 1 d . . P C 2
H46D H 0.367358 0.922128 0.996791 0.048 Uiso 0.165(5) 1 calc GR . P C 2
H46E H 0.243325 0.976811 1.027288 0.048 Uiso 0.165(5) 1 calc GR . P C 2
H46F H 0.382330 1.029605 0.981894 0.048 Uiso 0.165(5) 1 calc GR . P C 2
C47 C 0.2306(2) 0.92933(17) 0.65346(13) 0.0156(5) Uani 1 1 d . . . . .
C48 C 0.2125(3) 1.02253(18) 0.64096(14) 0.0197(5) Uani 1 1 d . . . . .
H48 H 0.279069 1.057551 0.654251 0.024 Uiso 1 1 calc R . . . .
C49 C 0.0977(3) 1.06420(18) 0.60919(15) 0.0234(6) Uani 1 1 d . . . . .
H49 H 0.086729 1.127869 0.600114 0.028 Uiso 1 1 calc R . . . .
C50 C -0.0009(3) 1.01370(19) 0.59062(14) 0.0213(6) Uani 1 1 d . . . . .
H50 H -0.080040 1.042502 0.569507 0.026 Uiso 1 1 calc R . . . .
C51 C 0.0159(3) 0.92106(19) 0.60283(14) 0.0215(6) Uani 1 1 d . . . . .
H51 H -0.052040 0.886288 0.590286 0.026 Uiso 1 1 calc R . . . .
C52 C 0.1319(3) 0.87895(18) 0.63336(14) 0.0183(5) Uani 1 1 d . . . . .
H52 H 0.144146 0.815657 0.640617 0.022 Uiso 1 1 calc R . . . .
C53 C 0.3302(3) 0.76520(17) 0.74867(13) 0.0160(5) Uani 1 1 d . . . . .
C54 C 0.1946(3) 0.74302(18) 0.78462(14) 0.0189(5) Uani 1 1 d . . . . .
H54 H 0.124358 0.787912 0.778434 0.023 Uiso 1 1 calc R . . . .
C55 C 0.1627(3) 0.65555(19) 0.82928(15) 0.0234(6) Uani 1 1 d . . . . .
H55 H 0.070286 0.640513 0.853069 0.028 Uiso 1 1 calc R . . . .
C56 C 0.2655(3) 0.58994(19) 0.83929(15) 0.0251(6) Uani 1 1 d . . . . .
H56 H 0.243348 0.530202 0.870032 0.030 Uiso 1 1 calc R . . . .
C57 C 0.3999(3) 0.61153(19) 0.80456(15) 0.0237(6) Uani 1 1 d . . . . .
H57 H 0.470430 0.566867 0.811807 0.028 Uiso 1 1 calc R . . . .
C58 C 0.4317(3) 0.69896(18) 0.75887(14) 0.0193(5) Uani 1 1 d . . . . .
H58 H 0.523810 0.713322 0.734472 0.023 Uiso 1 1 calc R . . . .
N1 N 0.7206(2) 0.74614(14) 0.63074(11) 0.0156(4) Uani 1 1 d . . . . .
N2 N 0.5249(2) 0.87738(14) 0.63691(11) 0.0155(4) Uani 1 1 d . . . . .
O1 O 0.76777(19) 0.77940(12) 0.75327(9) 0.0197(4) Uani 1 1 d . . . . .
H1 H 0.752925 0.785079 0.710390 0.029 Uiso 1 1 calc GR . . . .
O2 O 0.65979(18) 0.99056(12) 0.67845(9) 0.0184(4) Uani 1 1 d . . . . .
H2 H 0.635319 0.952677 0.658461 0.028 Uiso 1 1 calc GR . . . .
P1 P 0.80326(6) 0.65486(4) 0.65503(3) 0.01297(15) Uani 1 1 d . . . . .
P2 P 0.38696(6) 0.87817(4) 0.69064(3) 0.01339(15) Uani 1 1 d . . . . .
C59 C 0.5828(7) 0.6486(4) 0.1870(3) 0.0945(18) Uani 0.9576(15) 1 d D U P A 1
H59A H 0.560225 0.707864 0.154856 0.142 Uiso 0.9576(15) 1 calc GR . P A 1
H59B H 0.506698 0.628379 0.226845 0.142 Uiso 0.9576(15) 1 calc GR . P A 1
H59C H 0.594333 0.604323 0.159326 0.142 Uiso 0.9576(15) 1 calc GR . P A 1
C60 C 0.7145(5) 0.6567(3) 0.2170(2) 0.0591(11) Uani 0.9576(15) 1 d D U P A 1
H60A H 0.791977 0.674820 0.176816 0.071 Uiso 0.9576(15) 1 calc R . P A 1
H60B H 0.736939 0.596826 0.249618 0.071 Uiso 0.9576(15) 1 calc R . P A 1
C61 C 0.7026(4) 0.7258(3) 0.2588(2) 0.0528(10) Uani 0.9576(15) 1 d D U P A 1
H61A H 0.624647 0.707938 0.298780 0.063 Uiso 0.9576(15) 1 calc R . P A 1
H61B H 0.681177 0.785769 0.226125 0.063 Uiso 0.9576(15) 1 calc R . P A 1
C62 C 0.8376(4) 0.7329(3) 0.2900(3) 0.0586(11) Uani 0.9576(15) 1 d D U P A 1
H62A H 0.914928 0.750426 0.249662 0.070 Uiso 0.9576(15) 1 calc R . P A 1
H62B H 0.828613 0.781910 0.313843 0.070 Uiso 0.9576(15) 1 calc R . P A 1
C63 C 0.8750(7) 0.6477(4) 0.3435(6) 0.164(5) Uani 0.9576(15) 1 d D U P A 1
H63A H 0.802957 0.632622 0.385729 0.246 Uiso 0.9576(15) 1 calc GR . P A 1
H63B H 0.965532 0.656071 0.359106 0.246 Uiso 0.9576(15) 1 calc GR . P A 1
H63C H 0.881043 0.598256 0.320965 0.246 Uiso 0.9576(15) 1 calc GR . P A 1


_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
Br C5 1.874(8) . ?
C1 C2 1.418(3) . ?
C1 C6 1.403(3) . ?
C1 N1 1.404(3) . ?
C2 C3 1.392(3) . ?
C2 N2 1.413(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.391(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.412(4) . ?
C7 C12 1.395(4) . ?
C7 P1 1.804(2) . ?
C8 C9 1.414(4) . ?
C8 O1 1.347(3) . ?
C9 C10 1.391(4) . ?
C9 C13 1.541(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.392(4) . ?
C11 C12 1.390(4) . ?
C11 C17 1.529(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.538(4) . ?
C13 C15 1.541(4) . ?
C13 C16 1.531(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.614(6) . ?
C17 C18B 1.446(8) . ?
C17 C19 1.537(7) . ?
C17 C19B 1.664(8) . ?
C17 C20 1.431(7) . ?
C17 C20B 1.580(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C18B H18D 0.9800 . ?
C18B H18E 0.9800 . ?
C18B H18F 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19B H19D 0.9800 . ?
C19B H19E 0.9800 . ?
C19B H19F 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C20B H20F 0.9800 . ?
C21 C22 1.389(4) . ?
C21 C26 1.389(4) . ?
C21 P1 1.812(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.391(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.378(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.382(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.384(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.404(3) . ?
C27 C32 1.389(4) . ?
C27 P1 1.810(2) . ?
C28 H28 0.9500 . ?
C28 C29 1.388(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.389(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.385(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.387(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.414(3) . ?
C33 C38 1.396(3) . ?
C33 P2 1.798(2) . ?
C34 C35 1.418(4) . ?
C34 O2 1.344(3) . ?
C35 C36 1.390(4) . ?
C35 C39 1.543(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.399(4) . ?
C37 C38 1.385(4) . ?
C37 C43 1.534(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.546(4) . ?
C39 C41 1.530(4) . ?
C39 C42 1.525(4) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.529(4) . ?
C43 C44B 1.66(2) . ?
C43 C45 1.510(4) . ?
C43 C45B 1.564(17) . ?
C43 C46 1.547(4) . ?
C43 C46B 1.486(19) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C44B H44D 0.9800 . ?
C44B H44E 0.9800 . ?
C44B H44F 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C45B H45D 0.9800 . ?
C45B H45E 0.9800 . ?
C45B H45F 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C46B H46D 0.9800 . ?
C46B H46E 0.9800 . ?
C46B H46F 0.9800 . ?
C47 C48 1.395(4) . ?
C47 C52 1.398(3) . ?
C47 P2 1.815(2) . ?
C48 H48 0.9500 . ?
C48 C49 1.386(4) . ?
C49 H49 0.9500 . ?
C49 C50 1.383(4) . ?
C50 H50 0.9500 . ?
C50 C51 1.385(4) . ?
C51 H51 0.9500 . ?
C51 C52 1.388(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.401(3) . ?
C53 C58 1.387(4) . ?
C53 P2 1.825(3) . ?
C54 H54 0.9500 . ?
C54 C55 1.388(4) . ?
C55 H55 0.9500 . ?
C55 C56 1.389(4) . ?
C56 H56 0.9500 . ?
C56 C57 1.382(4) . ?
C57 H57 0.9500 . ?
C57 C58 1.394(4) . ?
C58 H58 0.9500 . ?
N1 P1 1.579(2) . ?
N2 P2 1.586(2) . ?
O1 H1 0.8400 . ?
O2 H2 0.8400 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C59 C60 1.481(7) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C60 C61 1.508(5) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C62 1.519(5) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 C63 1.484(7) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?

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
C6 C1 C2 118.1(2) . . ?
C6 C1 N1 124.0(2) . . ?
N1 C1 C2 117.9(2) . . ?
C3 C2 C1 119.2(2) . . ?
C3 C2 N2 121.9(2) . . ?
N2 C2 C1 118.7(2) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.8(2) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.4(2) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 Br 123.3(3) . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.7(2) . . ?
C6 C5 Br 116.5(3) . . ?
C6 C5 H5 120.2 . . ?
C1 C6 H6 119.1 . . ?
C5 C6 C1 121.8(2) . . ?
C5 C6 H6 119.1 . . ?
C8 C7 P1 120.45(19) . . ?
C12 C7 C8 120.5(2) . . ?
C12 C7 P1 119.04(19) . . ?
C7 C8 C9 119.3(2) . . ?
O1 C8 C7 121.6(2) . . ?
O1 C8 C9 119.1(2) . . ?
C8 C9 C13 121.3(2) . . ?
C10 C9 C8 117.5(2) . . ?
C10 C9 C13 121.2(2) . . ?
C9 C10 H10 117.9 . . ?
C9 C10 C11 124.3(2) . . ?
C11 C10 H10 117.9 . . ?
C10 C11 C17 121.0(2) . . ?
C12 C11 C10 117.2(2) . . ?
C12 C11 C17 121.8(2) . . ?
C7 C12 H12 119.4 . . ?
C11 C12 C7 121.1(2) . . ?
C11 C12 H12 119.4 . . ?
C14 C13 C9 110.1(2) . . ?
C14 C13 C15 107.0(2) . . ?
C15 C13 C9 111.9(2) . . ?
C16 C13 C9 110.0(2) . . ?
C16 C13 C14 110.5(3) . . ?
C16 C13 C15 107.2(2) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C11 C17 C18 104.9(3) . . ?
C11 C17 C19 108.4(3) . . ?
C11 C17 C19B 106.3(3) . . ?
C11 C17 C20B 111.6(3) . . ?
C18B C17 C11 118.7(4) . . ?
C18B C17 C19B 107.2(5) . . ?
C18B C17 C20B 110.2(5) . . ?
C19 C17 C18 105.2(4) . . ?
C20 C17 C11 113.9(3) . . ?
C20 C17 C18 109.4(4) . . ?
C20 C17 C19 114.2(4) . . ?
C20B C17 C19B 101.2(5) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C18B H18D 109.5 . . ?
C17 C18B H18E 109.5 . . ?
C17 C18B H18F 109.5 . . ?
H18D C18B H18E 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C19B H19D 109.5 . . ?
C17 C19B H19E 109.5 . . ?
C17 C19B H19F 109.5 . . ?
H19D C19B H19E 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C20B H20D 109.5 . . ?
C17 C20B H20E 109.5 . . ?
C17 C20B H20F 109.5 . . ?
H20D C20B H20E 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
C22 C21 C26 119.2(2) . . ?
C22 C21 P1 122.73(19) . . ?
C26 C21 P1 117.9(2) . . ?
C21 C22 H22 119.9 . . ?
C21 C22 C23 120.1(3) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 H23 120.0 . . ?
C24 C23 C22 120.1(3) . . ?
C24 C23 H23 120.0 . . ?
C23 C24 H24 119.9 . . ?
C23 C24 C25 120.2(3) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 120.1 . . ?
C24 C25 C26 119.9(3) . . ?
C26 C25 H25 120.1 . . ?
C21 C26 H26 119.7 . . ?
C25 C26 C21 120.5(3) . . ?
C25 C26 H26 119.7 . . ?
C28 C27 P1 119.00(19) . . ?
C32 C27 C28 119.7(2) . . ?
C32 C27 P1 121.29(18) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 C27 119.8(2) . . ?
C29 C28 H28 120.1 . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C30 120.1(2) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 120.1 . . ?
C31 C30 C29 119.9(2) . . ?
C31 C30 H30 120.1 . . ?
C30 C31 H31 119.7 . . ?
C30 C31 C32 120.6(2) . . ?
C32 C31 H31 119.7 . . ?
C27 C32 H32 120.1 . . ?
C31 C32 C27 119.9(2) . . ?
C31 C32 H32 120.1 . . ?
C34 C33 P2 122.66(19) . . ?
C38 C33 C34 120.3(2) . . ?
C38 C33 P2 117.08(19) . . ?
C33 C34 C35 118.8(2) . . ?
O2 C34 C33 122.0(2) . . ?
O2 C34 C35 119.2(2) . . ?
C34 C35 C39 120.4(2) . . ?
C36 C35 C34 118.1(2) . . ?
C36 C35 C39 121.5(2) . . ?
C35 C36 H36 118.0 . . ?
C35 C36 C37 124.0(2) . . ?
C37 C36 H36 118.0 . . ?
C36 C37 C43 122.9(2) . . ?
C38 C37 C36 116.8(2) . . ?
C38 C37 C43 120.3(2) . . ?
C33 C38 H38 119.0 . . ?
C37 C38 C33 121.9(2) . . ?
C37 C38 H38 119.0 . . ?
C35 C39 C40 110.6(2) . . ?
C41 C39 C35 109.6(2) . . ?
C41 C39 C40 109.4(2) . . ?
C42 C39 C35 111.8(2) . . ?
C42 C39 C40 107.3(2) . . ?
C42 C39 C41 108.0(2) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C37 C43 C44B 108.2(7) . . ?
C37 C43 C45B 114.4(6) . . ?
C37 C43 C46 108.2(2) . . ?
C44 C43 C37 112.9(2) . . ?
C44 C43 C46 107.3(3) . . ?
C45 C43 C37 109.0(2) . . ?
C45 C43 C44 109.8(3) . . ?
C45 C43 C46 109.5(3) . . ?
C45B C43 C44B 101.7(11) . . ?
C46B C43 C37 112.8(7) . . ?
C46B C43 C44B 108.9(12) . . ?
C46B C43 C45B 110.2(11) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C44B H44D 109.5 . . ?
C43 C44B H44E 109.5 . . ?
C43 C44B H44F 109.5 . . ?
H44D C44B H44E 109.5 . . ?
H44D C44B H44F 109.5 . . ?
H44E C44B H44F 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C45B H45D 109.5 . . ?
C43 C45B H45E 109.5 . . ?
C43 C45B H45F 109.5 . . ?
H45D C45B H45E 109.5 . . ?
H45D C45B H45F 109.5 . . ?
H45E C45B H45F 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C46B H46D 109.5 . . ?
C43 C46B H46E 109.5 . . ?
C43 C46B H46F 109.5 . . ?
H46D C46B H46E 109.5 . . ?
H46D C46B H46F 109.5 . . ?
H46E C46B H46F 109.5 . . ?
C48 C47 C52 119.1(2) . . ?
C48 C47 P2 118.91(19) . . ?
C52 C47 P2 121.9(2) . . ?
C47 C48 H48 119.9 . . ?
C49 C48 C47 120.2(2) . . ?
C49 C48 H48 119.9 . . ?
C48 C49 H49 119.8 . . ?
C50 C49 C48 120.4(3) . . ?
C50 C49 H49 119.8 . . ?
C49 C50 H50 120.0 . . ?
C49 C50 C51 119.9(2) . . ?
C51 C50 H50 120.0 . . ?
C50 C51 H51 119.9 . . ?
C50 C51 C52 120.1(2) . . ?
C52 C51 H51 119.9 . . ?
C47 C52 H52 119.9 . . ?
C51 C52 C47 120.3(2) . . ?
C51 C52 H52 119.9 . . ?
C54 C53 P2 124.4(2) . . ?
C58 C53 C54 119.1(2) . . ?
C58 C53 P2 116.42(19) . . ?
C53 C54 H54 119.9 . . ?
C55 C54 C53 120.1(2) . . ?
C55 C54 H54 119.9 . . ?
C54 C55 H55 119.9 . . ?
C54 C55 C56 120.2(2) . . ?
C56 C55 H55 119.9 . . ?
C55 C56 H56 120.0 . . ?
C57 C56 C55 120.0(3) . . ?
C57 C56 H56 120.0 . . ?
C56 C57 H57 120.1 . . ?
C56 C57 C58 119.9(3) . . ?
C58 C57 H57 120.1 . . ?
C53 C58 C57 120.7(2) . . ?
C53 C58 H58 119.7 . . ?
C57 C58 H58 119.7 . . ?
C1 N1 P1 129.86(18) . . ?
C2 N2 P2 128.48(17) . . ?
C8 O1 H1 109.5 . . ?
C34 O2 H2 109.5 . . ?
C7 P1 C21 108.54(11) . . ?
C7 P1 C27 106.23(11) . . ?
C27 P1 C21 104.80(11) . . ?
N1 P1 C7 106.42(11) . . ?
N1 P1 C21 115.07(11) . . ?
N1 P1 C27 115.33(11) . . ?
C33 P2 C47 106.09(12) . . ?
C33 P2 C53 108.31(11) . . ?
C47 P2 C53 104.88(11) . . ?
N2 P2 C33 104.69(11) . . ?
N2 P2 C47 119.07(11) . . ?
N2 P2 C53 113.25(12) . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C60 C59 H59A 109.5 . . ?
C60 C59 H59B 109.5 . . ?
C60 C59 H59C 109.5 . . ?
C59 C60 H60A 109.4 . . ?
C59 C60 H60B 109.4 . . ?
C59 C60 C61 111.3(4) . . ?
H60A C60 H60B 108.0 . . ?
C61 C60 H60A 109.4 . . ?
C61 C60 H60B 109.4 . . ?
C60 C61 H61A 109.4 . . ?
C60 C61 H61B 109.4 . . ?
C60 C61 C62 111.0(4) . . ?
H61A C61 H61B 108.0 . . ?
C62 C61 H61A 109.4 . . ?
C62 C61 H61B 109.4 . . ?
C61 C62 H62A 108.8 . . ?
C61 C62 H62B 108.8 . . ?
H62A C62 H62B 107.7 . . ?
C63 C62 C61 113.9(4) . . ?
C63 C62 H62A 108.8 . . ?
C63 C62 H62B 108.8 . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br C5 C6 C1 173.1(3) . . . . ?
C1 C2 C3 C4 2.3(4) . . . . ?
C1 C2 N2 P2 -124.5(2) . . . . ?
C1 N1 P1 C7 -148.1(2) . . . . ?
C1 N1 P1 C21 -27.9(3) . . . . ?
C1 N1 P1 C27 94.4(2) . . . . ?
C2 C1 C6 C5 0.3(3) . . . . ?
C2 C1 N1 P1 158.42(18) . . . . ?
C2 C3 C4 C5 -0.7(4) . . . . ?
C2 N2 P2 C33 -171.3(2) . . . . ?
C2 N2 P2 C47 -53.0(3) . . . . ?
C2 N2 P2 C53 71.0(2) . . . . ?
C3 C2 N2 P2 60.1(3) . . . . ?
C3 C4 C5 Br -172.3(3) . . . . ?
C3 C4 C5 C6 -1.1(4) . . . . ?
C4 C5 C6 C1 1.3(4) . . . . ?
C6 C1 C2 C3 -2.1(3) . . . . ?
C6 C1 C2 N2 -177.6(2) . . . . ?
C6 C1 N1 P1 -21.7(3) . . . . ?
C7 C8 C9 C10 1.3(3) . . . . ?
C7 C8 C9 C13 -178.6(2) . . . . ?
C8 C7 C12 C11 -1.0(4) . . . . ?
C8 C7 P1 C21 -152.09(19) . . . . ?
C8 C7 P1 C27 95.7(2) . . . . ?
C8 C7 P1 N1 -27.7(2) . . . . ?
C8 C9 C10 C11 -0.9(4) . . . . ?
C8 C9 C13 C14 58.9(3) . . . . ?
C8 C9 C13 C15 177.8(2) . . . . ?
C8 C9 C13 C16 -63.1(3) . . . . ?
C9 C10 C11 C12 -0.5(4) . . . . ?
C9 C10 C11 C17 -179.9(2) . . . . ?
C10 C9 C13 C14 -120.9(3) . . . . ?
C10 C9 C13 C15 -2.0(4) . . . . ?
C10 C9 C13 C16 117.0(3) . . . . ?
C10 C11 C12 C7 1.5(4) . . . . ?
C10 C11 C17 C18 -57.3(4) . . . . ?
C10 C11 C17 C18B -3.1(6) . . . . ?
C10 C11 C17 C19 54.7(4) . . . . ?
C10 C11 C17 C19B 117.7(4) . . . . ?
C10 C11 C17 C20 -176.9(4) . . . . ?
C10 C11 C17 C20B -132.8(4) . . . . ?
C12 C7 C8 C9 -0.4(4) . . . . ?
C12 C7 C8 O1 179.6(2) . . . . ?
C12 C7 P1 C21 28.0(2) . . . . ?
C12 C7 P1 C27 -84.2(2) . . . . ?
C12 C7 P1 N1 152.38(19) . . . . ?
C12 C11 C17 C18 123.4(3) . . . . ?
C12 C11 C17 C18B 177.6(5) . . . . ?
C12 C11 C17 C19 -124.6(4) . . . . ?
C12 C11 C17 C19B -61.6(4) . . . . ?
C12 C11 C17 C20 3.8(5) . . . . ?
C12 C11 C17 C20B 47.9(5) . . . . ?
C13 C9 C10 C11 179.0(2) . . . . ?
C17 C11 C12 C7 -179.2(2) . . . . ?
C21 C22 C23 C24 0.7(5) . . . . ?
C22 C21 C26 C25 -0.5(4) . . . . ?
C22 C21 P1 C7 -110.7(2) . . . . ?
C22 C21 P1 C27 2.5(3) . . . . ?
C22 C21 P1 N1 130.2(2) . . . . ?
C22 C23 C24 C25 -0.6(5) . . . . ?
C23 C24 C25 C26 0.1(5) . . . . ?
C24 C25 C26 C21 0.5(4) . . . . ?
C26 C21 C22 C23 -0.1(4) . . . . ?
C26 C21 P1 C7 75.1(2) . . . . ?
C26 C21 P1 C27 -171.7(2) . . . . ?
C26 C21 P1 N1 -44.0(2) . . . . ?
C27 C28 C29 C30 -0.4(4) . . . . ?
C28 C27 C32 C31 0.2(4) . . . . ?
C28 C27 P1 C7 -154.23(19) . . . . ?
C28 C27 P1 C21 91.0(2) . . . . ?
C28 C27 P1 N1 -36.6(2) . . . . ?
C28 C29 C30 C31 0.6(4) . . . . ?
C29 C30 C31 C32 -0.4(4) . . . . ?
C30 C31 C32 C27 0.0(4) . . . . ?
C32 C27 C28 C29 0.0(4) . . . . ?
C32 C27 P1 C7 25.3(2) . . . . ?
C32 C27 P1 C21 -89.5(2) . . . . ?
C32 C27 P1 N1 142.9(2) . . . . ?
C33 C34 C35 C36 3.0(4) . . . . ?
C33 C34 C35 C39 -178.8(2) . . . . ?
C34 C33 C38 C37 1.0(4) . . . . ?
C34 C33 P2 C47 -117.4(2) . . . . ?
C34 C33 P2 C53 130.4(2) . . . . ?
C34 C33 P2 N2 9.3(2) . . . . ?
C34 C35 C36 C37 -1.0(4) . . . . ?
C34 C35 C39 C40 57.4(3) . . . . ?
C34 C35 C39 C41 -63.3(3) . . . . ?
C34 C35 C39 C42 176.9(3) . . . . ?
C35 C36 C37 C38 -1.1(4) . . . . ?
C35 C36 C37 C43 178.9(2) . . . . ?
C36 C35 C39 C40 -124.5(3) . . . . ?
C36 C35 C39 C41 114.8(3) . . . . ?
C36 C35 C39 C42 -5.0(4) . . . . ?
C36 C37 C38 C33 1.1(4) . . . . ?
C36 C37 C43 C44 -0.2(4) . . . . ?
C36 C37 C43 C44B 72.5(9) . . . . ?
C36 C37 C43 C45 122.0(3) . . . . ?
C36 C37 C43 C45B -175.0(9) . . . . ?
C36 C37 C43 C46 -118.9(3) . . . . ?
C36 C37 C43 C46B -48.0(10) . . . . ?
C38 C33 C34 C35 -3.1(4) . . . . ?
C38 C33 C34 O2 177.3(2) . . . . ?
C38 C33 P2 C47 61.7(2) . . . . ?
C38 C33 P2 C53 -50.4(2) . . . . ?
C38 C33 P2 N2 -171.51(19) . . . . ?
C38 C37 C43 C44 179.7(3) . . . . ?
C38 C37 C43 C44B -107.5(9) . . . . ?
C38 C37 C43 C45 -58.0(3) . . . . ?
C38 C37 C43 C45B 5.0(9) . . . . ?
C38 C37 C43 C46 61.1(3) . . . . ?
C38 C37 C43 C46B 132.0(10) . . . . ?
C39 C35 C36 C37 -179.1(2) . . . . ?
C43 C37 C38 C33 -178.9(2) . . . . ?
C47 C48 C49 C50 1.0(4) . . . . ?
C48 C47 C52 C51 -1.4(4) . . . . ?
C48 C47 P2 C33 31.2(2) . . . . ?
C48 C47 P2 C53 145.7(2) . . . . ?
C48 C47 P2 N2 -86.3(2) . . . . ?
C48 C49 C50 C51 -0.9(4) . . . . ?
C49 C50 C51 C52 -0.3(4) . . . . ?
C50 C51 C52 C47 1.5(4) . . . . ?
C52 C47 C48 C49 0.2(4) . . . . ?
C52 C47 P2 C33 -152.4(2) . . . . ?
C52 C47 P2 C53 -37.8(2) . . . . ?
C52 C47 P2 N2 90.1(2) . . . . ?
C53 C54 C55 C56 0.8(4) . . . . ?
C54 C53 C58 C57 -0.4(4) . . . . ?
C54 C53 P2 C33 83.9(2) . . . . ?
C54 C53 P2 C47 -29.0(2) . . . . ?
C54 C53 P2 N2 -160.4(2) . . . . ?
C54 C55 C56 C57 -0.2(4) . . . . ?
C55 C56 C57 C58 -0.7(4) . . . . ?
C56 C57 C58 C53 1.0(4) . . . . ?
C58 C53 C54 C55 -0.5(4) . . . . ?
C58 C53 P2 C33 -93.8(2) . . . . ?
C58 C53 P2 C47 153.28(19) . . . . ?
C58 C53 P2 N2 21.9(2) . . . . ?
N1 C1 C2 C3 177.8(2) . . . . ?
N1 C1 C2 N2 2.3(3) . . . . ?
N1 C1 C6 C5 -179.6(2) . . . . ?
N2 C2 C3 C4 177.7(2) . . . . ?
O1 C8 C9 C10 -178.7(2) . . . . ?
O1 C8 C9 C13 1.5(4) . . . . ?
O2 C34 C35 C36 -177.4(2) . . . . ?
O2 C34 C35 C39 0.8(4) . . . . ?
P1 C7 C8 C9 179.67(18) . . . . ?
P1 C7 C8 O1 -0.3(3) . . . . ?
P1 C7 C12 C11 178.87(19) . . . . ?
P1 C21 C22 C23 -174.3(2) . . . . ?
P1 C21 C26 C25 174.0(2) . . . . ?
P1 C27 C28 C29 179.57(19) . . . . ?
P1 C27 C32 C31 -179.4(2) . . . . ?
P2 C33 C34 C35 176.09(19) . . . . ?
P2 C33 C34 O2 -3.5(3) . . . . ?
P2 C33 C38 C37 -178.2(2) . . . . ?
P2 C47 C48 C49 176.7(2) . . . . ?
P2 C47 C52 C51 -177.82(19) . . . . ?
P2 C53 C54 C55 -178.2(2) . . . . ?
P2 C53 C58 C57 177.5(2) . . . . ?
C59 C60 C61 C62 179.5(4) . . . . ?
C60 C61 C62 C63 -62.7(7) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3a
_database_code_depnum_ccdc_archive 'CCDC 1978290'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne
France
;
_audit_update_record             
;
2020-01-16 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_audit_creation_date             2019-11-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H78 N2 O4 P2 Zr, 3(C H2 Cl2)'
_chemical_formula_sum            'C63 H84 Cl6 N2 O4 P2 Zr'
_chemical_formula_weight         1299.18
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.3263(4)
_cell_length_b                   15.6278(5)
_cell_length_c                   16.7838(6)
_cell_angle_alpha                97.5780(16)
_cell_angle_beta                 94.7670(15)
_cell_angle_gamma                106.9900(15)
_cell_volume                     3286.27(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    115
_cell_measurement_theta_max      27.509
_cell_measurement_theta_min      2.428
_shelx_estimated_absorpt_T_max   0.863
_shelx_estimated_absorpt_T_min   0.797
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0528 before and 0.0460 after correction. The Ratio of minimum to maximum transmission is 0.9299. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            93582
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.601
_diffrn_reflns_theta_min         2.624
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       "φ and ω scans'"
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12199
_reflns_number_total             15091
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.855
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         15091
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0452
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0497P)²+6.5878P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1208
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(C13B)
3. Rigid body (RIGU) restrains
 C13B, C14B, C15B, C16B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C14, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C40, C41, C42, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C13B)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15B)=Sof(H15D)=
 Sof(H15E)=Sof(H15F)=Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(C13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
5.a Free rotating group:
 C13(C14,C15,C16), C13B(C14B,C15B,C16B)
5.b Ternary CH refined with riding coordinates:
 C55(H55), C58(H58)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C32(H32), C34(H34), C44(H44), C45(H45),
  C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
5.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C14B(H14D,H14E,H14F),
 C15B(H15D,H15E,H15F), C16B(H16D,H16E,H16F), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.83056(18) 0.35769(18) 0.78554(15) 0.0162(5) Uani 1 1 d . . . . .
H1A H 0.882623 0.409498 0.768785 0.019 Uiso 1 1 calc R . . . .
H1B H 0.858926 0.305586 0.781044 0.019 Uiso 1 1 calc R . . . .
C2 C 0.81186(19) 0.38297(17) 0.87248(15) 0.0151(5) Uani 1 1 d . . . . .
H2A H 0.876222 0.389485 0.909736 0.018 Uiso 1 1 calc R . . . .
H2B H 0.797297 0.441929 0.878990 0.018 Uiso 1 1 calc R . . . .
C3 C 0.51121(18) 0.28974(16) 0.60890(14) 0.0117(4) Uani 1 1 d . . . . .
C4 C 0.60894(18) 0.33244(16) 0.58336(14) 0.0137(5) Uani 1 1 d . . . . .
C5 C 0.61340(19) 0.36127(17) 0.50740(15) 0.0156(5) Uani 1 1 d . . . . .
H5 H 0.680348 0.390587 0.492068 0.019 Uiso 1 1 calc R . . . .
C6 C 0.52304(19) 0.34808(17) 0.45449(14) 0.0154(5) Uani 1 1 d . . . . .
C7 C 0.42615(19) 0.30282(17) 0.47982(15) 0.0151(5) Uani 1 1 d . . . . .
H7 H 0.363161 0.292400 0.444023 0.018 Uiso 1 1 calc R . . . .
C8 C 0.41690(18) 0.27244(16) 0.55389(14) 0.0130(5) Uani 1 1 d . . . . .
C9 C 0.30799(19) 0.22368(17) 0.57756(15) 0.0157(5) Uani 1 1 d . . . . .
C10 C 0.2842(2) 0.2828(2) 0.65022(16) 0.0230(6) Uani 1 1 d . . . . .
H10A H 0.282517 0.340836 0.634980 0.035 Uiso 1 1 calc GR . . . .
H10B H 0.339442 0.293798 0.696028 0.035 Uiso 1 1 calc GR . . . .
H10C H 0.215402 0.251315 0.665791 0.035 Uiso 1 1 calc GR . . . .
C11 C 0.3057(2) 0.13022(19) 0.59920(18) 0.0249(6) Uani 1 1 d . . . . .
H11A H 0.236100 0.100277 0.614331 0.037 Uiso 1 1 calc GR . . . .
H11B H 0.360372 0.138314 0.644784 0.037 Uiso 1 1 calc GR . . . .
H11C H 0.319133 0.092716 0.552211 0.037 Uiso 1 1 calc GR . . . .
C12 C 0.2185(2) 0.2071(2) 0.50781(16) 0.0215(5) Uani 1 1 d . . . . .
H12A H 0.151476 0.171996 0.523568 0.032 Uiso 1 1 calc GR . . . .
H12B H 0.234078 0.173346 0.459412 0.032 Uiso 1 1 calc GR . . . .
H12C H 0.213005 0.265473 0.496030 0.032 Uiso 1 1 calc GR . . . .
C13 C 0.5315(3) 0.3797(2) 0.3732(3) 0.0178(6) Uani 0.539(8) 1 d . U P A 1
C14 C 0.5652(6) 0.4841(2) 0.3885(3) 0.039(2) Uani 0.539(8) 1 d G U P A 1
H14A H 0.514193 0.504522 0.418588 0.058 Uiso 0.539(8) 1 calc GR . P A 1
H14B H 0.567426 0.506310 0.336545 0.058 Uiso 0.539(8) 1 calc GR . P A 1
H14C H 0.635561 0.507963 0.420195 0.058 Uiso 0.539(8) 1 calc GR . P A 1
C15 C 0.4263(3) 0.3451(4) 0.3162(5) 0.0287(17) Uani 0.539(8) 1 d G U P A 1
H15A H 0.401471 0.278690 0.307410 0.043 Uiso 0.539(8) 1 calc GR . P A 1
H15B H 0.437066 0.366161 0.264144 0.043 Uiso 0.539(8) 1 calc GR . P A 1
H15C H 0.373373 0.368575 0.340723 0.043 Uiso 0.539(8) 1 calc GR . P A 1
C16 C 0.6156(3) 0.3505(4) 0.3286(3) 0.0308(15) Uani 0.539(8) 1 d G U P A 1
H16A H 0.684831 0.376375 0.361716 0.046 Uiso 0.539(8) 1 calc GR . P A 1
H16B H 0.618656 0.372287 0.276493 0.046 Uiso 0.539(8) 1 calc GR . P A 1
H16C H 0.596834 0.284158 0.319358 0.046 Uiso 0.539(8) 1 calc GR . P A 1
C13B C 0.5241(4) 0.3911(3) 0.3764(3) 0.0178(6) Uani 0.461(8) 1 d . U P A 2
C14B C 0.4826(5) 0.4736(3) 0.3866(3) 0.0284(17) Uani 0.461(8) 1 d G U P A 2
H14D H 0.410286 0.454884 0.400650 0.043 Uiso 0.461(8) 1 calc GR . P A 2
H14E H 0.482734 0.498060 0.335768 0.043 Uiso 0.461(8) 1 calc GR . P A 2
H14F H 0.528313 0.520363 0.429961 0.043 Uiso 0.461(8) 1 calc GR . P A 2
C15B C 0.4525(6) 0.3207(4) 0.3060(5) 0.035(2) Uani 0.461(8) 1 d G U P A 2
H15D H 0.478174 0.267914 0.297489 0.053 Uiso 0.461(8) 1 calc GR . P A 2
H15E H 0.453938 0.347775 0.256473 0.053 Uiso 0.461(8) 1 calc GR . P A 2
H15F H 0.379821 0.301641 0.319211 0.053 Uiso 0.461(8) 1 calc GR . P A 2
C16B C 0.6361(4) 0.4226(6) 0.3517(4) 0.046(3) Uani 0.461(8) 1 d G U P A 2
H16D H 0.680089 0.474959 0.390902 0.069 Uiso 0.461(8) 1 calc GR . P A 2
H16E H 0.632170 0.439680 0.297667 0.069 Uiso 0.461(8) 1 calc GR . P A 2
H16F H 0.667478 0.373039 0.350745 0.069 Uiso 0.461(8) 1 calc GR . P A 2
C17 C 0.80532(19) 0.47329(17) 0.64236(15) 0.0165(5) Uani 1 1 d . . . . .
C18 C 0.7829(2) 0.53555(18) 0.70011(17) 0.0219(5) Uani 1 1 d . . . . .
H18 H 0.735685 0.514902 0.737861 0.026 Uiso 1 1 calc R . . . .
C19 C 0.8299(3) 0.6282(2) 0.7022(2) 0.0316(7) Uani 1 1 d . . . . .
H19 H 0.813984 0.670620 0.741087 0.038 Uiso 1 1 calc R . . . .
C20 C 0.8995(3) 0.6587(2) 0.6482(2) 0.0382(8) Uani 1 1 d . . . . .
H20 H 0.931851 0.721970 0.650298 0.046 Uiso 1 1 calc R . . . .
C21 C 0.9221(3) 0.5975(2) 0.5912(2) 0.0390(8) Uani 1 1 d . . . . .
H21 H 0.970056 0.618777 0.554089 0.047 Uiso 1 1 calc R . . . .
C22 C 0.8752(2) 0.5047(2) 0.58738(19) 0.0268(6) Uani 1 1 d . . . . .
H22 H 0.890693 0.462863 0.547593 0.032 Uiso 1 1 calc R . . . .
C23 C 0.80848(19) 0.29284(17) 0.58261(15) 0.0153(5) Uani 1 1 d . . . . .
C24 C 0.9181(2) 0.31424(19) 0.60378(16) 0.0193(5) Uani 1 1 d . . . . .
H24 H 0.953600 0.362307 0.646838 0.023 Uiso 1 1 calc R . . . .
C25 C 0.9752(2) 0.2655(2) 0.56211(17) 0.0226(6) Uani 1 1 d . . . . .
H25 H 1.049372 0.280448 0.576697 0.027 Uiso 1 1 calc R . . . .
C26 C 0.9239(2) 0.1951(2) 0.49925(17) 0.0234(6) Uani 1 1 d . . . . .
H26 H 0.962958 0.162056 0.470633 0.028 Uiso 1 1 calc R . . . .
C27 C 0.8154(2) 0.1731(2) 0.47826(17) 0.0240(6) Uani 1 1 d . . . . .
H27 H 0.780330 0.124509 0.435538 0.029 Uiso 1 1 calc R . . . .
C28 C 0.7577(2) 0.22176(18) 0.51941(16) 0.0184(5) Uani 1 1 d . . . . .
H28 H 0.683529 0.206527 0.504409 0.022 Uiso 1 1 calc R . . . .
C29 C 0.72432(19) 0.12603(16) 0.87260(14) 0.0142(5) Uani 1 1 d . . . . .
C30 C 0.64889(18) 0.10189(16) 0.80235(14) 0.0124(4) Uani 1 1 d . . . . .
C31 C 0.63810(18) 0.01922(16) 0.74910(14) 0.0131(5) Uani 1 1 d . . . . .
C32 C 0.6988(2) -0.03479(17) 0.77160(15) 0.0157(5) Uani 1 1 d . . . . .
H32 H 0.690479 -0.090161 0.736759 0.019 Uiso 1 1 calc R . . . .
C33 C 0.7717(2) -0.01282(17) 0.84243(15) 0.0168(5) Uani 1 1 d . . . . .
C34 C 0.7834(2) 0.06853(18) 0.89213(15) 0.0170(5) Uani 1 1 d . . . . .
H34 H 0.832157 0.085850 0.940326 0.020 Uiso 1 1 calc R . . . .
C35 C 0.5622(2) -0.00755(17) 0.66934(15) 0.0160(5) Uani 1 1 d . . . . .
C36 C 0.4471(2) -0.02251(19) 0.68798(18) 0.0236(6) Uani 1 1 d . . . . .
H36A H 0.399250 -0.037963 0.637028 0.035 Uiso 1 1 calc GR . . . .
H36B H 0.441671 0.033125 0.719349 0.035 Uiso 1 1 calc GR . . . .
H36C H 0.427337 -0.072180 0.719352 0.035 Uiso 1 1 calc GR . . . .
C37 C 0.5664(2) -0.09541(19) 0.61897(17) 0.0250(6) Uani 1 1 d . . . . .
H37A H 0.638677 -0.087915 0.606332 0.038 Uiso 1 1 calc GR . . . .
H37B H 0.518043 -0.109150 0.568475 0.038 Uiso 1 1 calc GR . . . .
H37C H 0.545280 -0.145330 0.649915 0.038 Uiso 1 1 calc GR . . . .
C38 C 0.5927(2) 0.06748(18) 0.61698(15) 0.0213(5) Uani 1 1 d . . . . .
H38A H 0.664520 0.074630 0.603546 0.032 Uiso 1 1 calc GR . . . .
H38B H 0.589904 0.124739 0.647093 0.032 Uiso 1 1 calc GR . . . .
H38C H 0.542996 0.050895 0.566950 0.032 Uiso 1 1 calc GR . . . .
C39 C 0.8391(2) -0.0732(2) 0.86557(18) 0.0252(6) Uani 1 1 d . U . . .
C40 C 0.8310(4) -0.1495(3) 0.7998(3) 0.0626(14) Uani 1 1 d . U . . .
H40A H 0.878595 -0.183168 0.816230 0.094 Uiso 1 1 calc GR . . . .
H40B H 0.850911 -0.125503 0.750327 0.094 Uiso 1 1 calc GR . . . .
H40C H 0.758026 -0.190114 0.789403 0.094 Uiso 1 1 calc GR . . . .
C41 C 0.9597(3) -0.0144(3) 0.8801(2) 0.0411(8) Uani 1 1 d . U . . .
H41A H 1.003032 -0.051703 0.896502 0.062 Uiso 1 1 calc GR . . . .
H41B H 0.970246 0.037606 0.922947 0.062 Uiso 1 1 calc GR . . . .
H41C H 0.980591 0.007171 0.829924 0.062 Uiso 1 1 calc GR . . . .
C42 C 0.8122(3) -0.1034(3) 0.9461(2) 0.0475(9) Uani 1 1 d . U . . .
H42A H 0.738655 -0.142507 0.939418 0.071 Uiso 1 1 calc GR . . . .
H42B H 0.821320 -0.050035 0.987133 0.071 Uiso 1 1 calc GR . . . .
H42C H 0.859361 -0.137114 0.963432 0.071 Uiso 1 1 calc GR . . . .
C43 C 0.64273(19) 0.20697(17) 1.00762(14) 0.0144(5) Uani 1 1 d . . . . .
C44 C 0.6119(2) 0.12231(18) 1.03296(16) 0.0218(5) Uani 1 1 d . . . . .
H44 H 0.637499 0.075153 1.009924 0.026 Uiso 1 1 calc R . . . .
C45 C 0.5440(3) 0.1070(2) 1.09170(18) 0.0291(6) Uani 1 1 d . . . . .
H45 H 0.523072 0.049437 1.108638 0.035 Uiso 1 1 calc R . . . .
C46 C 0.5067(2) 0.1762(2) 1.12571(17) 0.0278(6) Uani 1 1 d . . . . .
H46 H 0.460665 0.165833 1.166109 0.033 Uiso 1 1 calc R . . . .
C47 C 0.5366(2) 0.2598(2) 1.10076(17) 0.0255(6) Uani 1 1 d . . . . .
H47 H 0.510572 0.306647 1.123817 0.031 Uiso 1 1 calc R . . . .
C48 C 0.6048(2) 0.27583(18) 1.04196(15) 0.0194(5) Uani 1 1 d . . . . .
H48 H 0.625488 0.333566 1.025289 0.023 Uiso 1 1 calc R . . . .
C49 C 0.86771(19) 0.26469(17) 0.99662(15) 0.0155(5) Uani 1 1 d . . . . .
C50 C 0.8806(2) 0.3006(2) 1.07871(16) 0.0224(6) Uani 1 1 d . . . . .
H50 H 0.820535 0.302592 1.104771 0.027 Uiso 1 1 calc R . . . .
C51 C 0.9811(2) 0.3335(2) 1.12261(18) 0.0305(7) Uani 1 1 d . . . . .
H51 H 0.989460 0.357262 1.178699 0.037 Uiso 1 1 calc R . . . .
C52 C 1.0692(2) 0.3318(2) 1.08443(18) 0.0281(6) Uani 1 1 d . . . . .
H52 H 1.137800 0.354686 1.114453 0.034 Uiso 1 1 calc R . . . .
C53 C 1.0575(2) 0.2967(2) 1.00282(18) 0.0245(6) Uani 1 1 d . . . . .
H53 H 1.117982 0.295653 0.976968 0.029 Uiso 1 1 calc R . . . .
C54 C 0.9572(2) 0.26315(19) 0.95872(16) 0.0207(5) Uani 1 1 d . . . . .
H54 H 0.949280 0.239076 0.902741 0.025 Uiso 1 1 calc R . . . .
C55 C 0.5538(2) 0.46850(17) 0.89049(16) 0.0180(5) Uani 1 1 d . . . . .
H55 H 0.540864 0.432639 0.935809 0.022 Uiso 1 1 calc R . . . .
C56 C 0.4491(2) 0.47936(19) 0.85714(18) 0.0233(6) Uani 1 1 d . . . . .
H56A H 0.460542 0.515508 0.813348 0.035 Uiso 1 1 calc GR . . . .
H56B H 0.420968 0.510110 0.900528 0.035 Uiso 1 1 calc GR . . . .
H56C H 0.398512 0.419446 0.836089 0.035 Uiso 1 1 calc GR . . . .
C57 C 0.6356(2) 0.5597(2) 0.9235(2) 0.0302(7) Uani 1 1 d . . . . .
H57A H 0.701042 0.550195 0.945828 0.045 Uiso 1 1 calc GR . . . .
H57B H 0.608384 0.592309 0.966247 0.045 Uiso 1 1 calc GR . . . .
H57C H 0.650033 0.595500 0.879629 0.045 Uiso 1 1 calc GR . . . .
C58 C 0.3735(2) 0.2023(2) 0.8954(2) 0.0331(7) Uani 1 1 d . . . . .
H58 H 0.393501 0.227046 0.954559 0.040 Uiso 1 1 calc R . . . .
C59 C 0.2735(3) 0.2209(3) 0.8708(3) 0.0476(10) Uani 1 1 d . . . . .
H59A H 0.283607 0.286063 0.884453 0.071 Uiso 1 1 calc GR . . . .
H59B H 0.217525 0.187470 0.899561 0.071 Uiso 1 1 calc GR . . . .
H59C H 0.253302 0.201510 0.812282 0.071 Uiso 1 1 calc GR . . . .
C60 C 0.3654(3) 0.1039(2) 0.8861(3) 0.0445(9) Uani 1 1 d . . . . .
H60A H 0.343809 0.076204 0.828961 0.067 Uiso 1 1 calc GR . . . .
H60B H 0.312844 0.073429 0.918898 0.067 Uiso 1 1 calc GR . . . .
H60C H 0.434386 0.097610 0.904153 0.067 Uiso 1 1 calc GR . . . .
N1 N 0.72781(15) 0.33339(14) 0.73237(12) 0.0133(4) Uani 1 1 d . . . . .
N2 N 0.72170(16) 0.31276(14) 0.89344(12) 0.0131(4) Uani 1 1 d . . . . .
O1 O 0.50658(13) 0.26634(12) 0.68183(10) 0.0142(3) Uani 1 1 d . . . . .
O2 O 0.59032(13) 0.15446(11) 0.78763(10) 0.0139(3) Uani 1 1 d . . . . .
O3 O 0.59234(14) 0.41999(12) 0.82934(11) 0.0166(4) Uani 1 1 d . . . . .
O4 O 0.45618(14) 0.24958(12) 0.85591(11) 0.0188(4) Uani 1 1 d . . . . .
P2 P 0.73834(5) 0.23132(4) 0.93708(4) 0.01224(12) Uani 1 1 d . . . . .
P1 P 0.73522(5) 0.35435(4) 0.64182(4) 0.01162(12) Uani 1 1 d . . . . .
Zr Zr 0.57915(2) 0.28818(2) 0.79800(2) 0.01107(6) Uani 1 1 d . . . . .
C61 C 0.8998(3) 0.1146(2) 0.6944(2) 0.0368(8) Uani 1 1 d . . . . .
H61A H 0.849876 0.093037 0.733255 0.044 Uiso 1 1 calc R . . . .
H61B H 0.870841 0.152813 0.662394 0.044 Uiso 1 1 calc R . . . .
Cl1 Cl 1.02309(6) 0.18079(7) 0.74872(5) 0.0442(2) Uani 1 1 d . . . . .
Cl2 Cl 0.90906(12) 0.02142(7) 0.62945(7) 0.0682(3) Uani 1 1 d . . . . .
C62 C 0.8091(4) 0.1309(3) 0.2163(2) 0.0527(10) Uani 1 1 d . . . . .
H62A H 0.738243 0.090004 0.192148 0.063 Uiso 1 1 calc R . . . .
H62B H 0.851263 0.146405 0.171395 0.063 Uiso 1 1 calc R . . . .
Cl3 Cl 0.87054(10) 0.07353(9) 0.27776(7) 0.0629(3) Uani 1 1 d . . . . .
Cl4 Cl 0.79544(8) 0.23049(6) 0.26934(6) 0.0478(2) Uani 1 1 d . . . . .
C63 C 0.8189(6) 0.5299(7) 0.2168(5) 0.137(3) Uani 1 1 d . . . . .
H63A H 0.827275 0.591466 0.245770 0.164 Uiso 1 1 calc R . . . .
H63B H 0.742660 0.495517 0.210530 0.164 Uiso 1 1 calc R . . . .
Cl5 Cl 0.88333(8) 0.48004(7) 0.27649(8) 0.0583(3) Uani 1 1 d . . . . .
Cl6 Cl 0.85434(13) 0.54020(14) 0.12173(13) 0.1122(7) 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
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.521(3) . ?
C1 N1 1.490(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 N2 1.474(3) . ?
C3 C4 1.409(3) . ?
C3 C8 1.431(3) . ?
C3 O1 1.324(3) . ?
C4 C5 1.407(3) . ?
C4 P1 1.792(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.382(3) . ?
C6 C7 1.409(3) . ?
C6 C13 1.513(4) . ?
C6 C13B 1.550(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.390(3) . ?
C8 C9 1.541(3) . ?
C9 C10 1.543(4) . ?
C9 C11 1.543(4) . ?
C9 C12 1.538(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.5400 . ?
C13 C15 1.5403 . ?
C13 C16 1.5402 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C13B C14B 1.5394 . ?
C13B C15B 1.5406 . ?
C13B C16B 1.5400 . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C15B H15D 0.9800 . ?
C15B H15E 0.9800 . ?
C15B H15F 0.9800 . ?
C16B H16D 0.9800 . ?
C16B H16E 0.9800 . ?
C16B H16F 0.9800 . ?
C17 C18 1.395(4) . ?
C17 C22 1.399(4) . ?
C17 P1 1.819(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.394(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.381(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.377(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.392(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.404(3) . ?
C23 C28 1.396(4) . ?
C23 P1 1.823(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.390(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.388(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.387(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.392(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.417(3) . ?
C29 C34 1.408(3) . ?
C29 P2 1.797(2) . ?
C30 C31 1.433(3) . ?
C30 O2 1.320(3) . ?
C31 C32 1.394(3) . ?
C31 C35 1.540(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.407(3) . ?
C33 C34 1.385(4) . ?
C33 C39 1.543(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.548(4) . ?
C35 C37 1.533(3) . ?
C35 C38 1.538(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.487(4) . ?
C39 C41 1.580(5) . ?
C39 C42 1.526(5) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.400(4) . ?
C43 C48 1.396(4) . ?
C43 P2 1.804(2) . ?
C44 H44 0.9500 . ?
C44 C45 1.390(4) . ?
C45 H45 0.9500 . ?
C45 C46 1.392(4) . ?
C46 H46 0.9500 . ?
C46 C47 1.382(4) . ?
C47 H47 0.9500 . ?
C47 C48 1.394(4) . ?
C48 H48 0.9500 . ?
C49 C50 1.394(4) . ?
C49 C54 1.402(4) . ?
C49 P2 1.815(2) . ?
C50 H50 0.9500 . ?
C50 C51 1.390(4) . ?
C51 H51 0.9500 . ?
C51 C52 1.389(4) . ?
C52 H52 0.9500 . ?
C52 C53 1.385(4) . ?
C53 H53 0.9500 . ?
C53 C54 1.390(4) . ?
C54 H54 0.9500 . ?
C55 H55 1.0000 . ?
C55 C56 1.523(4) . ?
C55 C57 1.520(4) . ?
C55 O3 1.415(3) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58 1.0000 . ?
C58 C59 1.482(4) . ?
C58 C60 1.496(5) . ?
C58 O4 1.405(3) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
N1 P1 1.601(2) . ?
N1 Zr 2.321(2) . ?
N2 P2 1.609(2) . ?
N2 Zr 2.286(2) . ?
O1 Zr 2.0424(17) . ?
O2 Zr 2.1236(17) . ?
O3 Zr 2.0095(17) . ?
O4 Zr 1.9586(17) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 Cl1 1.763(3) . ?
C61 Cl2 1.741(4) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 Cl3 1.753(4) . ?
C62 Cl4 1.754(4) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 Cl5 1.673(7) . ?
C63 Cl6 1.716(7) . ?

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
H1A C1 H1B 108.4 . . ?
C2 C1 H1A 110.0 . . ?
C2 C1 H1B 110.0 . . ?
N1 C1 H1A 110.0 . . ?
N1 C1 H1B 110.0 . . ?
N1 C1 C2 108.35(19) . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N2 C2 C1 110.5(2) . . ?
N2 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C4 C3 C8 118.2(2) . . ?
O1 C3 C4 121.0(2) . . ?
O1 C3 C8 120.8(2) . . ?
C3 C4 P1 124.43(18) . . ?
C5 C4 C3 120.9(2) . . ?
C5 C4 P1 114.64(18) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 C4 121.8(2) . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C7 116.6(2) . . ?
C5 C6 C13 120.0(3) . . ?
C5 C6 C13B 122.8(3) . . ?
C7 C6 C13 123.3(3) . . ?
C7 C6 C13B 120.1(3) . . ?
C6 C7 H7 117.9 . . ?
C8 C7 C6 124.1(2) . . ?
C8 C7 H7 117.9 . . ?
C3 C8 C9 120.5(2) . . ?
C7 C8 C3 118.2(2) . . ?
C7 C8 C9 121.2(2) . . ?
C8 C9 C10 109.5(2) . . ?
C8 C9 C11 110.5(2) . . ?
C10 C9 C11 110.2(2) . . ?
C12 C9 C8 111.8(2) . . ?
C12 C9 C10 107.6(2) . . ?
C12 C9 C11 107.2(2) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C6 C13 C14 107.8(3) . . ?
C6 C13 C15 113.1(4) . . ?
C6 C13 C16 112.1(3) . . ?
C14 C13 C15 107.9 . . ?
C14 C13 C16 107.9 . . ?
C16 C13 C15 107.9 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14B C13B C6 111.8(3) . . ?
C14B C13B C15B 107.9 . . ?
C14B C13B C16B 107.9 . . ?
C15B C13B C6 109.6(4) . . ?
C16B C13B C6 111.7(3) . . ?
C16B C13B C15B 107.9 . . ?
C13B C14B H14D 109.5 . . ?
C13B C14B H14E 109.5 . . ?
C13B C14B H14F 109.5 . . ?
H14D C14B H14E 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C13B C15B H15D 109.5 . . ?
C13B C15B H15E 109.5 . . ?
C13B C15B H15F 109.5 . . ?
H15D C15B H15E 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
C13B C16B H16D 109.5 . . ?
C13B C16B H16E 109.5 . . ?
C13B C16B H16F 109.5 . . ?
H16D C16B H16E 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?
C18 C17 C22 119.5(2) . . ?
C18 C17 P1 116.2(2) . . ?
C22 C17 P1 124.2(2) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 C17 119.7(3) . . ?
C19 C18 H18 120.1 . . ?
C18 C19 H19 119.7 . . ?
C20 C19 C18 120.5(3) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 H20 120.0 . . ?
C21 C20 C19 119.9(3) . . ?
C21 C20 H20 120.0 . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C22 120.6(3) . . ?
C22 C21 H21 119.7 . . ?
C17 C22 H22 120.1 . . ?
C21 C22 C17 119.8(3) . . ?
C21 C22 H22 120.1 . . ?
C24 C23 P1 119.19(19) . . ?
C28 C23 C24 119.0(2) . . ?
C28 C23 P1 121.75(19) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.4(3) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 119.9 . . ?
C26 C25 C24 120.1(2) . . ?
C26 C25 H25 119.9 . . ?
C25 C26 H26 120.1 . . ?
C27 C26 C25 119.9(2) . . ?
C27 C26 H26 120.1 . . ?
C26 C27 H27 119.8 . . ?
C26 C27 C28 120.4(3) . . ?
C28 C27 H27 119.8 . . ?
C23 C28 H28 119.9 . . ?
C27 C28 C23 120.2(2) . . ?
C27 C28 H28 119.9 . . ?
C30 C29 P2 117.16(18) . . ?
C34 C29 C30 121.2(2) . . ?
C34 C29 P2 121.57(19) . . ?
C29 C30 C31 118.1(2) . . ?
O2 C30 C29 120.2(2) . . ?
O2 C30 C31 121.7(2) . . ?
C30 C31 C35 120.3(2) . . ?
C32 C31 C30 117.9(2) . . ?
C32 C31 C35 121.7(2) . . ?
C31 C32 H32 117.8 . . ?
C31 C32 C33 124.4(2) . . ?
C33 C32 H32 117.8 . . ?
C32 C33 C39 123.5(2) . . ?
C34 C33 C32 116.9(2) . . ?
C34 C33 C39 119.6(2) . . ?
C29 C34 H34 119.4 . . ?
C33 C34 C29 121.3(2) . . ?
C33 C34 H34 119.4 . . ?
C31 C35 C36 109.8(2) . . ?
C37 C35 C31 112.3(2) . . ?
C37 C35 C36 107.7(2) . . ?
C37 C35 C38 107.2(2) . . ?
C38 C35 C31 109.8(2) . . ?
C38 C35 C36 110.1(2) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C33 C39 C41 108.9(2) . . ?
C40 C39 C33 112.9(2) . . ?
C40 C39 C41 105.5(3) . . ?
C40 C39 C42 113.5(3) . . ?
C42 C39 C33 109.2(2) . . ?
C42 C39 C41 106.5(3) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 P2 121.11(19) . . ?
C48 C43 C44 119.4(2) . . ?
C48 C43 P2 119.30(19) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 C43 120.2(3) . . ?
C45 C44 H44 119.9 . . ?
C44 C45 H45 120.0 . . ?
C44 C45 C46 120.0(3) . . ?
C46 C45 H45 120.0 . . ?
C45 C46 H46 120.0 . . ?
C47 C46 C45 120.1(3) . . ?
C47 C46 H46 120.0 . . ?
C46 C47 H47 119.8 . . ?
C46 C47 C48 120.4(3) . . ?
C48 C47 H47 119.8 . . ?
C43 C48 H48 120.0 . . ?
C47 C48 C43 119.9(2) . . ?
C47 C48 H48 120.0 . . ?
C50 C49 C54 119.3(2) . . ?
C50 C49 P2 120.31(19) . . ?
C54 C49 P2 120.13(19) . . ?
C49 C50 H50 119.9 . . ?
C51 C50 C49 120.3(3) . . ?
C51 C50 H50 119.9 . . ?
C50 C51 H51 120.0 . . ?
C52 C51 C50 120.0(3) . . ?
C52 C51 H51 120.0 . . ?
C51 C52 H52 119.8 . . ?
C53 C52 C51 120.3(3) . . ?
C53 C52 H52 119.8 . . ?
C52 C53 H53 120.0 . . ?
C52 C53 C54 120.0(3) . . ?
C54 C53 H53 120.0 . . ?
C49 C54 H54 119.9 . . ?
C53 C54 C49 120.2(3) . . ?
C53 C54 H54 119.9 . . ?
C56 C55 H55 108.3 . . ?
C57 C55 H55 108.3 . . ?
C57 C55 C56 111.6(2) . . ?
O3 C55 H55 108.3 . . ?
O3 C55 C56 109.9(2) . . ?
O3 C55 C57 110.2(2) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C59 C58 H58 106.5 . . ?
C59 C58 C60 114.7(3) . . ?
C60 C58 H58 106.5 . . ?
O4 C58 H58 106.5 . . ?
O4 C58 C59 111.3(3) . . ?
O4 C58 C60 110.7(3) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C1 N1 P1 115.72(16) . . ?
C1 N1 Zr 114.73(14) . . ?
P1 N1 Zr 129.01(11) . . ?
C2 N2 P2 121.62(16) . . ?
C2 N2 Zr 108.66(14) . . ?
P2 N2 Zr 120.62(11) . . ?
C3 O1 Zr 146.77(15) . . ?
C30 O2 Zr 147.36(15) . . ?
C55 O3 Zr 133.50(15) . . ?
C58 O4 Zr 166.37(18) . . ?
C29 P2 C43 106.92(11) . . ?
C29 P2 C49 106.79(11) . . ?
C43 P2 C49 106.34(11) . . ?
N2 P2 C29 116.83(11) . . ?
N2 P2 C43 108.29(11) . . ?
N2 P2 C49 111.11(11) . . ?
C4 P1 C17 105.87(11) . . ?
C4 P1 C23 106.77(11) . . ?
C17 P1 C23 104.51(12) . . ?
N1 P1 C4 113.69(11) . . ?
N1 P1 C17 110.80(11) . . ?
N1 P1 C23 114.45(11) . . ?
N2 Zr N1 73.89(7) . . ?
O1 Zr N1 80.87(7) . . ?
O1 Zr N2 153.69(7) . . ?
O1 Zr O2 92.67(7) . . ?
O2 Zr N1 90.65(7) . . ?
O2 Zr N2 80.49(7) . . ?
O3 Zr N1 87.85(7) . . ?
O3 Zr N2 87.05(7) . . ?
O3 Zr O1 99.46(7) . . ?
O3 Zr O2 167.37(7) . . ?
O4 Zr N1 178.42(7) . . ?
O4 Zr N2 104.57(7) . . ?
O4 Zr O1 100.62(7) . . ?
O4 Zr O2 88.74(7) . . ?
O4 Zr O3 92.43(7) . . ?
H61A C61 H61B 107.8 . . ?
Cl1 C61 H61A 109.1 . . ?
Cl1 C61 H61B 109.1 . . ?
Cl2 C61 H61A 109.1 . . ?
Cl2 C61 H61B 109.1 . . ?
Cl2 C61 Cl1 112.5(2) . . ?
H62A C62 H62B 107.8 . . ?
Cl3 C62 H62A 109.0 . . ?
Cl3 C62 H62B 109.0 . . ?
Cl3 C62 Cl4 112.9(2) . . ?
Cl4 C62 H62A 109.0 . . ?
Cl4 C62 H62B 109.0 . . ?
H63A C63 H63B 107.1 . . ?
Cl5 C63 H63A 107.7 . . ?
Cl5 C63 H63B 107.7 . . ?
Cl5 C63 Cl6 118.3(4) . . ?
Cl6 C63 H63A 107.7 . . ?
Cl6 C63 H63B 107.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 N2 P2 94.1(2) . . . . ?
C1 C2 N2 Zr -53.0(2) . . . . ?
C1 N1 P1 C4 -175.15(17) . . . . ?
C1 N1 P1 C17 -56.1(2) . . . . ?
C1 N1 P1 C23 61.8(2) . . . . ?
C2 C1 N1 P1 149.53(17) . . . . ?
C2 C1 N1 Zr -22.8(2) . . . . ?
C2 N2 P2 C29 -95.8(2) . . . . ?
C2 N2 P2 C43 143.54(18) . . . . ?
C2 N2 P2 C49 27.1(2) . . . . ?
C3 C4 C5 C6 -0.8(4) . . . . ?
C3 C4 P1 C17 -129.9(2) . . . . ?
C3 C4 P1 C23 119.1(2) . . . . ?
C3 C4 P1 N1 -8.0(3) . . . . ?
C3 C8 C9 C10 64.3(3) . . . . ?
C3 C8 C9 C11 -57.3(3) . . . . ?
C3 C8 C9 C12 -176.6(2) . . . . ?
C4 C3 C8 C7 -3.3(3) . . . . ?
C4 C3 C8 C9 178.4(2) . . . . ?
C4 C3 O1 Zr 23.0(4) . . . . ?
C4 C5 C6 C7 -1.1(4) . . . . ?
C4 C5 C6 C13 -179.7(3) . . . . ?
C4 C5 C6 C13B 170.8(3) . . . . ?
C5 C4 P1 C17 50.3(2) . . . . ?
C5 C4 P1 C23 -60.6(2) . . . . ?
C5 C4 P1 N1 172.18(18) . . . . ?
C5 C6 C7 C8 0.8(4) . . . . ?
C5 C6 C13 C14 -70.9(3) . . . . ?
C5 C6 C13 C15 169.9(3) . . . . ?
C5 C6 C13 C16 47.7(4) . . . . ?
C5 C6 C13B C14B -103.0(4) . . . . ?
C5 C6 C13B C15B 137.5(3) . . . . ?
C5 C6 C13B C16B 18.1(4) . . . . ?
C6 C7 C8 C3 1.4(4) . . . . ?
C6 C7 C8 C9 179.8(2) . . . . ?
C7 C6 C13 C14 110.6(3) . . . . ?
C7 C6 C13 C15 -8.6(4) . . . . ?
C7 C6 C13 C16 -130.8(3) . . . . ?
C7 C6 C13B C14B 68.7(5) . . . . ?
C7 C6 C13B C15B -50.8(4) . . . . ?
C7 C6 C13B C16B -170.3(4) . . . . ?
C7 C8 C9 C10 -114.0(3) . . . . ?
C7 C8 C9 C11 124.4(2) . . . . ?
C7 C8 C9 C12 5.1(3) . . . . ?
C8 C3 C4 C5 3.0(3) . . . . ?
C8 C3 C4 P1 -176.75(18) . . . . ?
C8 C3 O1 Zr -156.9(2) . . . . ?
C13 C6 C7 C8 179.3(3) . . . . ?
C13B C6 C7 C8 -171.4(3) . . . . ?
C17 C18 C19 C20 -0.8(4) . . . . ?
C18 C17 C22 C21 0.4(4) . . . . ?
C18 C17 P1 C4 83.3(2) . . . . ?
C18 C17 P1 C23 -164.14(19) . . . . ?
C18 C17 P1 N1 -40.4(2) . . . . ?
C18 C19 C20 C21 0.6(5) . . . . ?
C19 C20 C21 C22 0.0(5) . . . . ?
C20 C21 C22 C17 -0.5(5) . . . . ?
C22 C17 C18 C19 0.2(4) . . . . ?
C22 C17 P1 C4 -94.1(2) . . . . ?
C22 C17 P1 C23 18.5(3) . . . . ?
C22 C17 P1 N1 142.2(2) . . . . ?
C23 C24 C25 C26 -0.1(4) . . . . ?
C24 C23 C28 C27 0.0(4) . . . . ?
C24 C23 P1 C4 164.8(2) . . . . ?
C24 C23 P1 C17 52.9(2) . . . . ?
C24 C23 P1 N1 -68.5(2) . . . . ?
C24 C25 C26 C27 -0.3(4) . . . . ?
C25 C26 C27 C28 0.6(4) . . . . ?
C26 C27 C28 C23 -0.4(4) . . . . ?
C28 C23 C24 C25 0.3(4) . . . . ?
C28 C23 P1 C4 -18.6(2) . . . . ?
C28 C23 P1 C17 -130.5(2) . . . . ?
C28 C23 P1 N1 108.1(2) . . . . ?
C29 C30 C31 C32 3.1(3) . . . . ?
C29 C30 C31 C35 -176.4(2) . . . . ?
C29 C30 O2 Zr 32.3(4) . . . . ?
C30 C29 C34 C33 1.5(4) . . . . ?
C30 C29 P2 C43 87.6(2) . . . . ?
C30 C29 P2 C49 -158.84(18) . . . . ?
C30 C29 P2 N2 -33.8(2) . . . . ?
C30 C31 C32 C33 -1.3(4) . . . . ?
C30 C31 C35 C36 -63.3(3) . . . . ?
C30 C31 C35 C37 176.9(2) . . . . ?
C30 C31 C35 C38 57.8(3) . . . . ?
C31 C30 O2 Zr -148.3(2) . . . . ?
C31 C32 C33 C34 -0.5(4) . . . . ?
C31 C32 C33 C39 -179.2(2) . . . . ?
C32 C31 C35 C36 117.3(3) . . . . ?
C32 C31 C35 C37 -2.5(3) . . . . ?
C32 C31 C35 C38 -121.6(2) . . . . ?
C32 C33 C34 C29 0.4(4) . . . . ?
C32 C33 C39 C40 8.5(4) . . . . ?
C32 C33 C39 C41 125.3(3) . . . . ?
C32 C33 C39 C42 -118.8(3) . . . . ?
C34 C29 C30 C31 -3.2(3) . . . . ?
C34 C29 C30 O2 176.3(2) . . . . ?
C34 C29 P2 C43 -90.5(2) . . . . ?
C34 C29 P2 C49 23.0(2) . . . . ?
C34 C29 P2 N2 148.1(2) . . . . ?
C34 C33 C39 C40 -170.2(3) . . . . ?
C34 C33 C39 C41 -53.4(3) . . . . ?
C34 C33 C39 C42 62.5(4) . . . . ?
C35 C31 C32 C33 178.1(2) . . . . ?
C39 C33 C34 C29 179.2(2) . . . . ?
C43 C44 C45 C46 -0.2(4) . . . . ?
C44 C43 C48 C47 -0.2(4) . . . . ?
C44 C43 P2 C29 30.5(2) . . . . ?
C44 C43 P2 C49 -83.3(2) . . . . ?
C44 C43 P2 N2 157.2(2) . . . . ?
C44 C45 C46 C47 0.4(5) . . . . ?
C45 C46 C47 C48 -0.5(5) . . . . ?
C46 C47 C48 C43 0.4(4) . . . . ?
C48 C43 C44 C45 0.1(4) . . . . ?
C48 C43 P2 C29 -154.2(2) . . . . ?
C48 C43 P2 C49 91.9(2) . . . . ?
C48 C43 P2 N2 -27.5(2) . . . . ?
C49 C50 C51 C52 0.8(5) . . . . ?
C50 C49 C54 C53 0.3(4) . . . . ?
C50 C49 P2 C29 -138.6(2) . . . . ?
C50 C49 P2 C43 -24.6(2) . . . . ?
C50 C49 P2 N2 93.0(2) . . . . ?
C50 C51 C52 C53 -0.4(5) . . . . ?
C51 C52 C53 C54 0.0(5) . . . . ?
C52 C53 C54 C49 0.1(4) . . . . ?
C54 C49 C50 C51 -0.7(4) . . . . ?
C54 C49 P2 C29 47.9(2) . . . . ?
C54 C49 P2 C43 161.8(2) . . . . ?
C54 C49 P2 N2 -80.5(2) . . . . ?
C56 C55 O3 Zr -93.7(3) . . . . ?
C57 C55 O3 Zr 142.9(2) . . . . ?
C59 C58 O4 Zr -137.4(7) . . . . ?
C60 C58 O4 Zr -8.6(10) . . . . ?
N1 C1 C2 N2 49.9(3) . . . . ?
O1 C3 C4 C5 -176.9(2) . . . . ?
O1 C3 C4 P1 3.4(3) . . . . ?
O1 C3 C8 C7 176.6(2) . . . . ?
O1 C3 C8 C9 -1.7(3) . . . . ?
O2 C30 C31 C32 -176.4(2) . . . . ?
O2 C30 C31 C35 4.2(3) . . . . ?
P2 C29 C30 C31 178.61(17) . . . . ?
P2 C29 C30 O2 -1.9(3) . . . . ?
P2 C29 C34 C33 179.6(2) . . . . ?
P2 C43 C44 C45 175.3(2) . . . . ?
P2 C43 C48 C47 -175.5(2) . . . . ?
P2 C49 C50 C51 -174.3(2) . . . . ?
P2 C49 C54 C53 173.9(2) . . . . ?
P1 C4 C5 C6 179.0(2) . . . . ?
P1 C17 C18 C19 -177.3(2) . . . . ?
P1 C17 C22 C21 177.7(2) . . . . ?
P1 C23 C24 C25 176.9(2) . . . . ?
P1 C23 C28 C27 -176.6(2) . . . . ?
Zr N1 P1 C4 -4.11(19) . . . . ?
Zr N1 P1 C17 114.98(15) . . . . ?
Zr N1 P1 C23 -127.17(14) . . . . ?
Zr N2 P2 C29 47.47(16) . . . . ?
Zr N2 P2 C43 -73.24(14) . . . . ?
Zr N2 P2 C49 170.32(11) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3b
_database_code_depnum_ccdc_archive 'CCDC 1978288'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne
France
;
_audit_update_record             
;
2020-01-16 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_audit_creation_date             2019-10-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C64 H78 N2 O4 P2 Zr, 2(C H2 Cl2)'
_chemical_formula_sum            'C66 H82 Cl4 N2 O4 P2 Zr'
_chemical_formula_weight         1262.29
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.3206(9)
_cell_length_b                   13.3221(8)
_cell_length_c                   22.2555(13)
_cell_angle_alpha                104.471(3)
_cell_angle_beta                 102.628(3)
_cell_angle_gamma                101.728(3)
_cell_volume                     3589.9(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    115
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.61
_shelx_estimated_absorpt_T_max   0.909
_shelx_estimated_absorpt_T_min   0.909
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0830 before and 0.0680 after correction. The Ratio of minimum to maximum transmission is 0.8625. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            94359
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.577
_diffrn_reflns_theta_min         2.130
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       "φ and ω scans'"
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12337
_reflns_number_total             16522
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.845
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         16522
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0880
_refine_ls_restrained_S_all      1.179
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0825P)²+23.0599P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2468
_refine_ls_wR_factor_ref         0.2619
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Rigid body (RIGU) restrains
 C7, C7A, C8, C8A, C9, C9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: C7(0.54691) H7(0.54691) C7A(0.45309) H7A(0.45309) C8(0.54691)
 H8A(0.54691) H8B(0.54691) H8C(0.54691) C8A(0.45309) H8AA(0.45309)
 H8AB(0.45309) H8AC(0.45309) C9(0.54691) H9A(0.54691) H9B(0.54691) H9C(0.54691)
 C9A(0.45309) H9AA(0.45309) H9AB(0.45309) H9AC(0.45309) C10(0.63664)
 H10(0.63664) C10A(0.36336) H10A(0.36336) H11A(0.63664) H11B(0.63664)
 H11C(0.63664) H11D(0.36336) H11E(0.36336) H11F(0.36336) H12A(0.63664)
 H12B(0.63664) H12C(0.63664) H12D(0.36336) H12E(0.36336) H12F(0.36336)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C7A(H7A), C10(H10), C10A(H10A)
4.b Secondary CH2 refined with riding coordinates:
 C65(H65A,H65B), C66(H66A,H66B)
4.c Me refined with riding coordinates:
 C11(H11A,H11B,H11C), C11(H11D,H11E,H11F), C12(H12A,H12B,H12C), C12(H12D,H12E,
 H12F)
4.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C15(H15), C17(H17), C28(H28), C29(H29),
 C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C41(H41), C43(H43), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
 C60(H60), C61(H61), C62(H62), C63(H63), C64(H64)
4.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2654(4) 0.5627(4) 0.6161(2) 0.0183(10) Uani 1 1 d . . . . .
C2 C 0.3493(4) 0.6422(4) 0.6124(2) 0.0187(10) Uani 1 1 d . . . . .
C3 C 0.3392(4) 0.6726(4) 0.5568(3) 0.0225(11) Uani 1 1 d . . . . .
H3 H 0.397033 0.724086 0.553625 0.027 Uiso 1 1 calc R . . . .
C4 C 0.2457(5) 0.6292(5) 0.5052(3) 0.0239(11) Uani 1 1 d . . . . .
H4 H 0.238808 0.653439 0.468165 0.029 Uiso 1 1 calc R . . . .
C5 C 0.1634(5) 0.5505(5) 0.5085(3) 0.0245(11) Uani 1 1 d . . . . .
H5 H 0.100498 0.518868 0.473142 0.029 Uiso 1 1 calc R . . . .
C6 C 0.1726(4) 0.5178(4) 0.5632(3) 0.0215(11) Uani 1 1 d . . . . .
H6 H 0.115370 0.464133 0.565206 0.026 Uiso 1 1 calc R . . . .
C7 C 0.4575(14) 0.7557(12) 0.8612(7) 0.041(3) Uani 0.5469 1 d . U P A 1
H7 H 0.533476 0.800407 0.875419 0.050 Uiso 0.5469 1 calc R . P A 1
C7A C 0.4100(14) 0.7095(16) 0.8638(8) 0.042(4) Uani 0.4531 1 d . U P A 2
H7A H 0.383498 0.647164 0.878952 0.051 Uiso 0.4531 1 calc R . P A 2
C8 C 0.387(3) 0.823(2) 0.8435(10) 0.099(9) Uani 0.5469 1 d . U P A 1
H8A H 0.390436 0.831894 0.801529 0.148 Uiso 0.5469 1 calc GR . P A 1
H8B H 0.411297 0.893677 0.876572 0.148 Uiso 0.5469 1 calc GR . P A 1
H8C H 0.313537 0.787686 0.840757 0.148 Uiso 0.5469 1 calc GR . P A 1
C8A C 0.3188(19) 0.748(2) 0.8437(11) 0.078(8) Uani 0.4531 1 d . U P A 2
H8AA H 0.337475 0.801495 0.821501 0.117 Uiso 0.4531 1 calc GR . P A 2
H8AB H 0.297913 0.782326 0.881673 0.117 Uiso 0.4531 1 calc GR . P A 2
H8AC H 0.259098 0.688003 0.814065 0.117 Uiso 0.4531 1 calc GR . P A 2
C9 C 0.4361(16) 0.7124(13) 0.9146(6) 0.056(4) Uani 0.5469 1 d . U P A 1
H9A H 0.359333 0.678861 0.904571 0.084 Uiso 0.5469 1 calc GR . P A 1
H9B H 0.459690 0.771560 0.955391 0.084 Uiso 0.5469 1 calc GR . P A 1
H9C H 0.475392 0.658621 0.918784 0.084 Uiso 0.5469 1 calc GR . P A 1
C9A C 0.5038(16) 0.7833(16) 0.9170(9) 0.056(5) Uani 0.4531 1 d . U P A 2
H9AA H 0.553497 0.742520 0.930258 0.084 Uiso 0.4531 1 calc GR . P A 2
H9AB H 0.479960 0.816284 0.953934 0.084 Uiso 0.4531 1 calc GR . P A 2
H9AC H 0.540021 0.839767 0.901938 0.084 Uiso 0.4531 1 calc GR . P A 2
C10 C 0.5174(9) 0.3631(8) 0.6513(5) 0.032(2) Uani 0.6366 1 d . . P B 3
H10 H 0.453567 0.309405 0.652075 0.038 Uiso 0.6366 1 calc R . P B 3
C10A C 0.5772(15) 0.4126(14) 0.6498(8) 0.029(4) Uani 0.3634 1 d . . P B 4
H10A H 0.639842 0.467660 0.648880 0.035 Uiso 0.3634 1 calc R . P B 4
C11 C 0.6139(6) 0.3618(6) 0.7015(4) 0.0422(16) Uani 1 1 d . . . . .
H11A H 0.626334 0.290326 0.690371 0.063 Uiso 0.6366 1 calc R . P B 3
H11B H 0.676855 0.415932 0.702634 0.063 Uiso 0.6366 1 calc R . P B 3
H11C H 0.600913 0.378407 0.744153 0.063 Uiso 0.6366 1 calc R . P B 3
H11D H 0.667325 0.325127 0.690798 0.063 Uiso 0.3634 1 calc R . P B 4
H11E H 0.645526 0.418014 0.743504 0.063 Uiso 0.3634 1 calc R . P B 4
H11F H 0.552473 0.309521 0.703772 0.063 Uiso 0.3634 1 calc R . P B 4
C12 C 0.5292(8) 0.3341(7) 0.5848(4) 0.058(2) Uani 1 1 d . . . . .
H12A H 0.541649 0.262614 0.573764 0.087 Uiso 0.6366 1 calc R . P B 3
H12B H 0.463794 0.333314 0.553987 0.087 Uiso 0.6366 1 calc R . P B 3
H12C H 0.589994 0.387383 0.582681 0.087 Uiso 0.6366 1 calc R . P B 3
H12D H 0.581868 0.297679 0.572342 0.087 Uiso 0.3634 1 calc R . P B 4
H12E H 0.466770 0.280786 0.585006 0.087 Uiso 0.3634 1 calc R . P B 4
H12F H 0.507012 0.371643 0.553655 0.087 Uiso 0.3634 1 calc R . P B 4
C13 C 0.3326(5) 0.4332(4) 0.7955(3) 0.0233(11) Uani 1 1 d . . . . .
C14 C 0.2354(5) 0.4580(5) 0.7745(3) 0.0243(11) Uani 1 1 d . . . . .
C15 C 0.1647(5) 0.4666(5) 0.8119(3) 0.0275(12) Uani 1 1 d . . . . .
H15 H 0.100564 0.484845 0.796653 0.033 Uiso 1 1 calc R . . . .
C16 C 0.1879(5) 0.4483(5) 0.8718(3) 0.0275(12) Uani 1 1 d . . . . .
C17 C 0.2782(5) 0.4126(5) 0.8881(3) 0.0268(12) Uani 1 1 d . . . . .
H17 H 0.291202 0.393817 0.927027 0.032 Uiso 1 1 calc R . . . .
C18 C 0.3508(5) 0.4021(5) 0.8527(3) 0.0259(12) Uani 1 1 d . . . . .
C19 C 0.4433(5) 0.3527(5) 0.8705(3) 0.0321(14) Uani 1 1 d . . . . .
C20 C 0.4269(7) 0.2500(6) 0.8144(4) 0.0429(17) Uani 1 1 d . . . . .
H20A H 0.487573 0.219696 0.823550 0.064 Uiso 1 1 calc GR . . . .
H20B H 0.421879 0.268192 0.774045 0.064 Uiso 1 1 calc GR . . . .
H20C H 0.360756 0.197006 0.810152 0.064 Uiso 1 1 calc GR . . . .
C21 C 0.4452(7) 0.3199(7) 0.9325(3) 0.0471(19) Uani 1 1 d . . . . .
H21A H 0.460428 0.384430 0.969494 0.071 Uiso 1 1 calc GR . . . .
H21B H 0.500906 0.282715 0.940204 0.071 Uiso 1 1 calc GR . . . .
H21C H 0.375540 0.271572 0.927220 0.071 Uiso 1 1 calc GR . . . .
C22 C 0.5511(6) 0.4327(6) 0.8828(3) 0.0409(16) Uani 1 1 d . . . . .
H22A H 0.555968 0.448830 0.842781 0.061 Uiso 1 1 calc GR . . . .
H22B H 0.608840 0.401341 0.897326 0.061 Uiso 1 1 calc GR . . . .
H22C H 0.557627 0.499338 0.916342 0.061 Uiso 1 1 calc GR . . . .
C23 C 0.1170(5) 0.4634(6) 0.9173(3) 0.0342(14) Uani 1 1 d . . . . .
C24 C 0.0240(9) 0.5037(11) 0.8910(5) 0.084(4) Uani 1 1 d . . . . .
H24A H 0.050777 0.571055 0.882097 0.125 Uiso 1 1 calc GR . . . .
H24B H -0.016032 0.516705 0.922904 0.125 Uiso 1 1 calc GR . . . .
H24C H -0.023153 0.449623 0.850865 0.125 Uiso 1 1 calc GR . . . .
C25 C 0.0782(8) 0.3585(7) 0.9324(5) 0.059(2) Uani 1 1 d . . . . .
H25A H 0.038328 0.300893 0.891996 0.088 Uiso 1 1 calc GR . . . .
H25B H 0.031631 0.368842 0.960615 0.088 Uiso 1 1 calc GR . . . .
H25C H 0.139963 0.338634 0.954270 0.088 Uiso 1 1 calc GR . . . .
C26 C 0.1861(8) 0.5477(8) 0.9824(4) 0.063(2) Uani 1 1 d . . . . .
H26A H 0.242452 0.519623 1.002779 0.095 Uiso 1 1 calc GR . . . .
H26B H 0.140932 0.562581 1.011057 0.095 Uiso 1 1 calc GR . . . .
H26C H 0.218554 0.614400 0.974591 0.095 Uiso 1 1 calc GR . . . .
C27 C 0.0705(5) 0.4848(5) 0.6785(3) 0.0264(12) Uani 1 1 d . . . . .
C28 C 0.0715(5) 0.5921(5) 0.6918(3) 0.0332(14) Uani 1 1 d . . . . .
H28 H 0.136948 0.646512 0.703526 0.040 Uiso 1 1 calc R . . . .
C29 C -0.0250(6) 0.6194(6) 0.6879(4) 0.0423(16) Uani 1 1 d . . . . .
H29 H -0.025216 0.692847 0.695966 0.051 Uiso 1 1 calc R . . . .
C30 C -0.1188(6) 0.5421(7) 0.6725(3) 0.0438(18) Uani 1 1 d . . . . .
H30 H -0.183800 0.561885 0.669846 0.053 Uiso 1 1 calc R . . . .
C31 C -0.1200(5) 0.4377(7) 0.6611(3) 0.0403(16) Uani 1 1 d . . . . .
H31 H -0.185664 0.384789 0.651842 0.048 Uiso 1 1 calc R . . . .
C32 C -0.0253(5) 0.4058(6) 0.6627(3) 0.0327(13) Uani 1 1 d . . . . .
H32 H -0.026783 0.331786 0.653114 0.039 Uiso 1 1 calc R . . . .
C33 C 0.1775(4) 0.3141(5) 0.6469(3) 0.0243(11) Uani 1 1 d . . . . .
C34 C 0.2195(5) 0.2887(5) 0.5952(3) 0.0293(12) Uani 1 1 d . . . . .
H34 H 0.257318 0.344609 0.582505 0.035 Uiso 1 1 calc R . . . .
C35 C 0.2064(6) 0.1811(5) 0.5617(3) 0.0373(15) Uani 1 1 d . . . . .
H35 H 0.234630 0.164216 0.525895 0.045 Uiso 1 1 calc R . . . .
C36 C 0.1535(6) 0.0997(5) 0.5798(4) 0.0410(16) Uani 1 1 d . . . . .
H36 H 0.144939 0.026771 0.556549 0.049 Uiso 1 1 calc R . . . .
C37 C 0.1124(6) 0.1232(6) 0.6319(4) 0.0461(18) Uani 1 1 d . . . . .
H37 H 0.075323 0.066409 0.644191 0.055 Uiso 1 1 calc R . . . .
C38 C 0.1251(5) 0.2303(5) 0.6665(3) 0.0363(14) Uani 1 1 d . . . . .
H38 H 0.098547 0.246479 0.703070 0.044 Uiso 1 1 calc R . . . .
C39 C 0.6599(4) 0.7676(4) 0.7889(3) 0.0228(11) Uani 1 1 d . . . . .
C40 C 0.6165(4) 0.8395(4) 0.7617(3) 0.0220(11) Uani 1 1 d . . . . .
C41 C 0.6463(5) 0.9499(5) 0.7934(3) 0.0304(13) Uani 1 1 d . . . . .
H41 H 0.614486 0.996098 0.774050 0.036 Uiso 1 1 calc R . . . .
C42 C 0.7221(5) 0.9924(5) 0.8532(3) 0.0326(14) Uani 1 1 d . . . . .
C43 C 0.7712(5) 0.9225(5) 0.8767(3) 0.0316(13) Uani 1 1 d . . . . .
H43 H 0.826820 0.952151 0.916305 0.038 Uiso 1 1 calc R . . . .
C44 C 0.7452(4) 0.8112(5) 0.8466(3) 0.0239(11) Uani 1 1 d . . . . .
C45 C 0.8085(5) 0.7409(5) 0.8746(3) 0.0376(15) Uani 1 1 d . . . . .
C46 C 0.8494(7) 0.6783(7) 0.8216(4) 0.055(2) Uani 1 1 d . . . . .
H46A H 0.898373 0.729097 0.808893 0.083 Uiso 1 1 calc GR . . . .
H46B H 0.788657 0.635316 0.783867 0.083 Uiso 1 1 calc GR . . . .
H46C H 0.887091 0.630427 0.838069 0.083 Uiso 1 1 calc GR . . . .
C47 C 0.7344(7) 0.6604(8) 0.8955(5) 0.067(3) Uani 1 1 d . . . . .
H47A H 0.773234 0.612197 0.910602 0.100 Uiso 1 1 calc GR . . . .
H47B H 0.672197 0.617896 0.858598 0.100 Uiso 1 1 calc GR . . . .
H47C H 0.710364 0.699763 0.930607 0.100 Uiso 1 1 calc GR . . . .
C48 C 0.9049(7) 0.8057(6) 0.9323(4) 0.057(2) Uani 1 1 d . . . . .
H48A H 0.880425 0.839885 0.968695 0.085 Uiso 1 1 calc GR . . . .
H48B H 0.949744 0.861357 0.920548 0.085 Uiso 1 1 calc GR . . . .
H48C H 0.946450 0.757654 0.944819 0.085 Uiso 1 1 calc GR . . . .
C49 C 0.7470(6) 1.1127(6) 0.8896(4) 0.0434(17) Uani 1 1 d . . . . .
C50 C 0.7570(9) 1.1827(7) 0.8466(5) 0.071(3) Uani 1 1 d . . . . .
H50A H 0.775313 1.258565 0.872551 0.107 Uiso 1 1 calc GR . . . .
H50B H 0.688846 1.164542 0.813220 0.107 Uiso 1 1 calc GR . . . .
H50C H 0.813270 1.170757 0.826003 0.107 Uiso 1 1 calc GR . . . .
C51 C 0.6555(7) 1.1297(7) 0.9179(5) 0.067(3) Uani 1 1 d . . . . .
H51A H 0.650195 1.088713 0.948502 0.101 Uiso 1 1 calc GR . . . .
H51B H 0.588376 1.104983 0.882911 0.101 Uiso 1 1 calc GR . . . .
H51C H 0.668790 1.206542 0.940391 0.101 Uiso 1 1 calc GR . . . .
C52 C 0.8507(6) 1.1515(6) 0.9453(4) 0.056(2) Uani 1 1 d . . . . .
H52A H 0.863565 1.228215 0.967765 0.083 Uiso 1 1 calc GR . . . .
H52B H 0.910614 1.140608 0.928022 0.083 Uiso 1 1 calc GR . . . .
H52C H 0.844045 1.110321 0.975801 0.083 Uiso 1 1 calc GR . . . .
C53 C 0.4919(4) 0.8928(4) 0.6588(3) 0.0258(12) Uani 1 1 d . . . . .
C54 C 0.4150(5) 0.9248(5) 0.6852(3) 0.0340(14) Uani 1 1 d . . . . .
H54 H 0.384941 0.886201 0.710497 0.041 Uiso 1 1 calc R . . . .
C55 C 0.3807(6) 1.0125(5) 0.6755(4) 0.0444(18) Uani 1 1 d . . . . .
H55 H 0.327325 1.033348 0.693925 0.053 Uiso 1 1 calc R . . . .
C56 C 0.4235(7) 1.0688(6) 0.6395(5) 0.064(3) Uani 1 1 d . . . . .
H56 H 0.400664 1.129558 0.633462 0.076 Uiso 1 1 calc R . . . .
C57 C 0.5008(7) 1.0377(7) 0.6116(5) 0.061(2) Uani 1 1 d . . . . .
H57 H 0.530674 1.077092 0.586584 0.074 Uiso 1 1 calc R . . . .
C58 C 0.5342(5) 0.9484(5) 0.6205(4) 0.0407(16) Uani 1 1 d . . . . .
H58 H 0.585504 0.925574 0.600678 0.049 Uiso 1 1 calc R . . . .
C59 C 0.6294(5) 0.7497(5) 0.6337(3) 0.0248(11) Uani 1 1 d . . . . .
C60 C 0.7299(5) 0.8220(5) 0.6461(3) 0.0335(14) Uani 1 1 d . . . . .
H60 H 0.747919 0.891412 0.676822 0.040 Uiso 1 1 calc R . . . .
C61 C 0.8019(5) 0.7938(6) 0.6144(4) 0.0377(15) Uani 1 1 d . . . . .
H61 H 0.870299 0.842633 0.624207 0.045 Uiso 1 1 calc R . . . .
C62 C 0.7752(5) 0.6944(6) 0.5683(3) 0.0375(15) Uani 1 1 d . . . . .
H62 H 0.824465 0.676064 0.545307 0.045 Uiso 1 1 calc R . . . .
C63 C 0.6762(5) 0.6206(6) 0.5553(3) 0.0350(14) Uani 1 1 d . . . . .
H63 H 0.658209 0.551683 0.524071 0.042 Uiso 1 1 calc R . . . .
C64 C 0.6047(5) 0.6494(5) 0.5886(3) 0.0277(12) Uani 1 1 d . . . . .
H64 H 0.537575 0.599314 0.580238 0.033 Uiso 1 1 calc R . . . .
N1 N 0.2849(4) 0.5327(4) 0.6731(2) 0.0204(9) Uani 1 1 d . . . . .
N2 N 0.4396(3) 0.6815(4) 0.6674(2) 0.0198(9) Uani 1 1 d . . . . .
O1 O 0.3995(3) 0.4377(3) 0.75964(18) 0.0222(8) Uani 1 1 d . . . . .
O2 O 0.6211(3) 0.6625(3) 0.75806(18) 0.0226(8) Uani 1 1 d . . . . .
O3 O 0.4452(4) 0.6667(4) 0.8087(2) 0.0333(10) Uani 1 1 d . . . . .
O4 O 0.4997(3) 0.4650(3) 0.66724(19) 0.0252(8) Uani 1 1 d . . . . .
P1 P 0.19762(11) 0.45307(11) 0.69178(7) 0.0205(3) Uani 1 1 d . . . . .
P2 P 0.53807(11) 0.78408(11) 0.67912(7) 0.0208(3) Uani 1 1 d . . . . .
Zr Zr 0.45966(4) 0.57215(4) 0.73012(2) 0.01943(14) Uani 1 1 d . . . . .
C65 C 0.1729(10) 0.9133(11) 0.4170(6) 0.090(4) Uani 1 1 d . . . . .
H65A H 0.162752 0.986295 0.422416 0.108 Uiso 1 1 calc R . . . .
H65B H 0.108674 0.867340 0.421881 0.108 Uiso 1 1 calc R . . . .
Cl1 Cl 0.2816(2) 0.9213(3) 0.47713(15) 0.0872(8) Uani 1 1 d . . . . .
Cl2 Cl 0.1823(3) 0.8615(3) 0.33898(14) 0.0925(10) Uani 1 1 d . . . . .
C66 C 0.1356(7) 0.7913(7) 0.5936(4) 0.0493(19) Uani 1 1 d . . . . .
H66A H 0.205190 0.825543 0.588536 0.059 Uiso 1 1 calc R . . . .
H66B H 0.134725 0.716671 0.593365 0.059 Uiso 1 1 calc R . . . .
Cl3 Cl 0.12248(17) 0.86366(15) 0.66844(10) 0.0505(5) Uani 1 1 d . . . . .
Cl4 Cl 0.03196(15) 0.78772(17) 0.52826(11) 0.0519(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
C1 C2 1.408(7) . ?
C1 C6 1.408(7) . ?
C1 N1 1.410(6) . ?
C2 C3 1.384(7) . ?
C2 N2 1.413(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.398(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.384(8) . ?
C5 H5 0.9500 . ?
C5 C6 1.382(8) . ?
C6 H6 0.9500 . ?
C7 H7 1.0000 . ?
C7 C8 1.48(2) . ?
C7 C9 1.501(19) . ?
C7 O3 1.393(14) . ?
C7A H7A 1.0000 . ?
C7A C8A 1.44(3) . ?
C7A C9A 1.48(3) . ?
C7A O3 1.436(14) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.514(13) . ?
C10 C12 1.485(12) . ?
C10 O4 1.398(10) . ?
C10A H10A 1.0000 . ?
C10A C11 1.517(19) . ?
C10A C12 1.471(19) . ?
C10A O4 1.428(16) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C11 H11D 0.9800 . ?
C11 H11E 0.9800 . ?
C11 H11F 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12 H12D 0.9800 . ?
C12 H12E 0.9800 . ?
C12 H12F 0.9800 . ?
C13 C14 1.410(8) . ?
C13 C18 1.420(8) . ?
C13 O1 1.323(6) . ?
C14 C15 1.391(8) . ?
C14 P1 1.779(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.394(8) . ?
C16 C17 1.391(8) . ?
C16 C23 1.534(8) . ?
C17 H17 0.9500 . ?
C17 C18 1.382(8) . ?
C18 C19 1.534(8) . ?
C19 C20 1.543(9) . ?
C19 C21 1.546(8) . ?
C19 C22 1.527(10) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.509(11) . ?
C23 C25 1.533(10) . ?
C23 C26 1.546(11) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.382(9) . ?
C27 C32 1.391(9) . ?
C27 P1 1.808(6) . ?
C28 H28 0.9500 . ?
C28 C29 1.396(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.361(11) . ?
C30 H30 0.9500 . ?
C30 C31 1.346(11) . ?
C31 H31 0.9500 . ?
C31 C32 1.406(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.384(8) . ?
C33 C38 1.408(8) . ?
C33 P1 1.804(6) . ?
C34 H34 0.9500 . ?
C34 C35 1.397(9) . ?
C35 H35 0.9500 . ?
C35 C36 1.367(10) . ?
C36 H36 0.9500 . ?
C36 C37 1.380(11) . ?
C37 H37 0.9500 . ?
C37 C38 1.398(10) . ?
C38 H38 0.9500 . ?
C39 C40 1.407(8) . ?
C39 C44 1.414(8) . ?
C39 O2 1.330(7) . ?
C40 C41 1.394(8) . ?
C40 P2 1.783(5) . ?
C41 H41 0.9500 . ?
C41 C42 1.382(9) . ?
C42 C43 1.384(9) . ?
C42 C49 1.533(9) . ?
C43 H43 0.9500 . ?
C43 C44 1.399(8) . ?
C44 C45 1.536(8) . ?
C45 C46 1.536(10) . ?
C45 C47 1.537(11) . ?
C45 C48 1.522(9) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.501(12) . ?
C49 C51 1.521(12) . ?
C49 C52 1.534(10) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.376(9) . ?
C53 C58 1.395(9) . ?
C53 P2 1.802(6) . ?
C54 H54 0.9500 . ?
C54 C55 1.385(9) . ?
C55 H55 0.9500 . ?
C55 C56 1.362(12) . ?
C56 H56 0.9500 . ?
C56 C57 1.394(14) . ?
C57 H57 0.9500 . ?
C57 C58 1.395(10) . ?
C58 H58 0.9500 . ?
C59 C60 1.406(8) . ?
C59 C64 1.381(8) . ?
C59 P2 1.801(6) . ?
C60 H60 0.9500 . ?
C60 C61 1.366(9) . ?
C61 H61 0.9500 . ?
C61 C62 1.379(10) . ?
C62 H62 0.9500 . ?
C62 C63 1.398(10) . ?
C63 H63 0.9500 . ?
C63 C64 1.384(8) . ?
C64 H64 0.9500 . ?
N1 P1 1.606(4) . ?
N1 Zr 2.277(4) . ?
N2 P2 1.612(5) . ?
N2 Zr 2.270(4) . ?
O1 Zr 2.125(4) . ?
O2 Zr 2.110(4) . ?
O3 Zr 1.956(4) . ?
O4 Zr 1.979(4) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C65 Cl1 1.708(13) . ?
C65 Cl2 1.743(12) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C66 Cl3 1.769(7) . ?
C66 Cl4 1.756(8) . ?

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
C2 C1 C6 118.7(5) . . ?
C2 C1 N1 115.4(5) . . ?
C6 C1 N1 125.8(5) . . ?
C1 C2 N2 114.7(4) . . ?
C3 C2 C1 119.3(5) . . ?
C3 C2 N2 126.0(5) . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.5(5) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.2(5) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.2(5) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 H6 119.5 . . ?
C5 C6 C1 121.1(5) . . ?
C5 C6 H6 119.5 . . ?
C8 C7 H7 108.5 . . ?
C8 C7 C9 113.3(14) . . ?
C9 C7 H7 108.5 . . ?
O3 C7 H7 108.5 . . ?
O3 C7 C8 111.5(14) . . ?
O3 C7 C9 106.5(12) . . ?
C8A C7A H7A 106.3 . . ?
C8A C7A C9A 118.9(18) . . ?
C9A C7A H7A 106.3 . . ?
O3 C7A H7A 106.3 . . ?
O3 C7A C8A 109.5(15) . . ?
O3 C7A C9A 108.9(14) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7A C8A H8AA 109.5 . . ?
C7A C8A H8AB 109.5 . . ?
C7A C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7A C9A H9AA 109.5 . . ?
C7A C9A H9AB 109.5 . . ?
C7A C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
C11 C10 H10 108.3 . . ?
C12 C10 H10 108.3 . . ?
C12 C10 C11 112.7(8) . . ?
O4 C10 H10 108.3 . . ?
O4 C10 C11 109.5(8) . . ?
O4 C10 C12 109.7(7) . . ?
C11 C10A H10A 109.0 . . ?
C12 C10A H10A 109.0 . . ?
C12 C10A C11 113.4(12) . . ?
O4 C10A H10A 109.0 . . ?
O4 C10A C11 107.7(11) . . ?
O4 C10A C12 108.8(13) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
C10A C11 H11D 109.5 . . ?
C10A C11 H11E 109.5 . . ?
C10A C11 H11F 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
H11D C11 H11E 109.5 . . ?
H11D C11 H11F 109.5 . . ?
H11E C11 H11F 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
C10A C12 H12D 109.5 . . ?
C10A C12 H12E 109.5 . . ?
C10A C12 H12F 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
H12D C12 H12E 109.5 . . ?
H12D C12 H12F 109.5 . . ?
H12E C12 H12F 109.5 . . ?
C14 C13 C18 118.0(5) . . ?
O1 C13 C14 117.6(5) . . ?
O1 C13 C18 124.3(5) . . ?
C13 C14 P1 115.5(4) . . ?
C15 C14 C13 122.2(5) . . ?
C15 C14 P1 121.3(4) . . ?
C14 C15 H15 120.0 . . ?
C14 C15 C16 119.9(5) . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C23 122.6(5) . . ?
C17 C16 C15 116.6(5) . . ?
C17 C16 C23 120.8(5) . . ?
C16 C17 H17 117.2 . . ?
C18 C17 C16 125.6(5) . . ?
C18 C17 H17 117.2 . . ?
C13 C18 C19 120.3(5) . . ?
C17 C18 C13 116.9(5) . . ?
C17 C18 C19 122.7(5) . . ?
C18 C19 C20 108.1(5) . . ?
C18 C19 C21 111.7(5) . . ?
C20 C19 C21 107.9(6) . . ?
C22 C19 C18 111.1(5) . . ?
C22 C19 C20 110.8(5) . . ?
C22 C19 C21 107.3(6) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C16 C23 C26 108.2(6) . . ?
C24 C23 C16 112.5(6) . . ?
C24 C23 C25 111.0(7) . . ?
C24 C23 C26 108.0(7) . . ?
C25 C23 C16 110.4(6) . . ?
C25 C23 C26 106.5(7) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C32 120.2(6) . . ?
C28 C27 P1 117.9(5) . . ?
C32 C27 P1 121.5(5) . . ?
C27 C28 H28 120.5 . . ?
C27 C28 C29 119.1(6) . . ?
C29 C28 H28 120.5 . . ?
C28 C29 H29 119.6 . . ?
C30 C29 C28 120.8(7) . . ?
C30 C29 H29 119.6 . . ?
C29 C30 H30 119.8 . . ?
C31 C30 C29 120.5(6) . . ?
C31 C30 H30 119.8 . . ?
C30 C31 H31 119.5 . . ?
C30 C31 C32 120.9(7) . . ?
C32 C31 H31 119.5 . . ?
C27 C32 C31 118.6(6) . . ?
C27 C32 H32 120.7 . . ?
C31 C32 H32 120.7 . . ?
C34 C33 C38 119.2(6) . . ?
C34 C33 P1 120.2(4) . . ?
C38 C33 P1 120.5(5) . . ?
C33 C34 H34 120.0 . . ?
C33 C34 C35 120.1(6) . . ?
C35 C34 H34 120.0 . . ?
C34 C35 H35 119.6 . . ?
C36 C35 C34 120.8(6) . . ?
C36 C35 H35 119.6 . . ?
C35 C36 H36 119.9 . . ?
C35 C36 C37 120.1(6) . . ?
C37 C36 H36 119.9 . . ?
C36 C37 H37 119.9 . . ?
C36 C37 C38 120.2(6) . . ?
C38 C37 H37 119.9 . . ?
C33 C38 H38 120.2 . . ?
C37 C38 C33 119.6(6) . . ?
C37 C38 H38 120.2 . . ?
C40 C39 C44 118.2(5) . . ?
O2 C39 C40 118.5(5) . . ?
O2 C39 C44 123.3(5) . . ?
C39 C40 P2 115.6(4) . . ?
C41 C40 C39 122.1(5) . . ?
C41 C40 P2 121.6(4) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 C40 120.1(6) . . ?
C42 C41 H41 120.0 . . ?
C41 C42 C43 117.2(5) . . ?
C41 C42 C49 119.1(6) . . ?
C43 C42 C49 123.7(6) . . ?
C42 C43 H43 117.5 . . ?
C42 C43 C44 124.9(6) . . ?
C44 C43 H43 117.5 . . ?
C39 C44 C45 122.0(5) . . ?
C43 C44 C39 116.9(5) . . ?
C43 C44 C45 121.1(5) . . ?
C44 C45 C47 109.3(6) . . ?
C46 C45 C44 108.5(6) . . ?
C46 C45 C47 109.0(7) . . ?
C48 C45 C44 113.3(6) . . ?
C48 C45 C46 107.8(6) . . ?
C48 C45 C47 108.8(7) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C42 C49 C52 111.7(6) . . ?
C50 C49 C42 112.9(7) . . ?
C50 C49 C51 107.6(8) . . ?
C50 C49 C52 108.0(7) . . ?
C51 C49 C42 108.1(6) . . ?
C51 C49 C52 108.3(7) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49 C51 H51A 109.5 . . ?
C49 C51 H51B 109.5 . . ?
C49 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C49 C52 H52A 109.5 . . ?
C49 C52 H52B 109.5 . . ?
C49 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C54 C53 C58 119.2(6) . . ?
C54 C53 P2 117.6(5) . . ?
C58 C53 P2 123.1(5) . . ?
C53 C54 H54 119.5 . . ?
C53 C54 C55 121.1(7) . . ?
C55 C54 H54 119.5 . . ?
C54 C55 H55 120.0 . . ?
C56 C55 C54 120.0(7) . . ?
C56 C55 H55 120.0 . . ?
C55 C56 H56 119.9 . . ?
C55 C56 C57 120.2(7) . . ?
C57 C56 H56 119.9 . . ?
C56 C57 H57 120.1 . . ?
C56 C57 C58 119.8(8) . . ?
C58 C57 H57 120.1 . . ?
C53 C58 C57 119.6(7) . . ?
C53 C58 H58 120.2 . . ?
C57 C58 H58 120.2 . . ?
C60 C59 P2 120.7(5) . . ?
C64 C59 C60 118.6(6) . . ?
C64 C59 P2 120.7(4) . . ?
C59 C60 H60 119.6 . . ?
C61 C60 C59 120.9(6) . . ?
C61 C60 H60 119.6 . . ?
C60 C61 H61 120.0 . . ?
C60 C61 C62 120.0(6) . . ?
C62 C61 H61 120.0 . . ?
C61 C62 H62 119.8 . . ?
C61 C62 C63 120.4(6) . . ?
C63 C62 H62 119.8 . . ?
C62 C63 H63 120.5 . . ?
C64 C63 C62 119.0(6) . . ?
C64 C63 H63 120.5 . . ?
C59 C64 C63 121.1(6) . . ?
C59 C64 H64 119.4 . . ?
C63 C64 H64 119.4 . . ?
C1 N1 P1 124.6(4) . . ?
C1 N1 Zr 116.0(3) . . ?
P1 N1 Zr 118.0(2) . . ?
C2 N2 P2 123.8(4) . . ?
C2 N2 Zr 116.2(3) . . ?
P2 N2 Zr 118.7(2) . . ?
C13 O1 Zr 125.9(3) . . ?
C39 O2 Zr 126.5(3) . . ?
C7 O3 Zr 163.2(8) . . ?
C7A O3 Zr 163.5(9) . . ?
C10 O4 Zr 145.8(5) . . ?
C10A O4 Zr 149.9(8) . . ?
C14 P1 C27 105.6(3) . . ?
C14 P1 C33 104.7(3) . . ?
C33 P1 C27 109.1(3) . . ?
N1 P1 C14 113.4(3) . . ?
N1 P1 C27 112.0(3) . . ?
N1 P1 C33 111.5(3) . . ?
C40 P2 C53 105.4(3) . . ?
C40 P2 C59 105.7(3) . . ?
C59 P2 C53 109.2(3) . . ?
N2 P2 C40 112.7(3) . . ?
N2 P2 C53 111.5(2) . . ?
N2 P2 C59 111.9(3) . . ?
N2 Zr N1 69.83(16) . . ?
O1 Zr N1 82.03(15) . . ?
O1 Zr N2 151.56(16) . . ?
O2 Zr N1 152.31(15) . . ?
O2 Zr N2 82.48(15) . . ?
O2 Zr O1 125.63(15) . . ?
O3 Zr N1 95.04(17) . . ?
O3 Zr N2 97.56(18) . . ?
O3 Zr O1 88.72(17) . . ?
O3 Zr O2 87.66(17) . . ?
O3 Zr O4 164.94(17) . . ?
O4 Zr N1 96.81(17) . . ?
O4 Zr N2 95.24(16) . . ?
O4 Zr O1 83.76(15) . . ?
O4 Zr O2 86.16(16) . . ?
H65A C65 H65B 107.6 . . ?
Cl1 C65 H65A 108.7 . . ?
Cl1 C65 H65B 108.7 . . ?
Cl1 C65 Cl2 114.3(7) . . ?
Cl2 C65 H65A 108.7 . . ?
Cl2 C65 H65B 108.7 . . ?
H66A C66 H66B 108.0 . . ?
Cl3 C66 H66A 109.3 . . ?
Cl3 C66 H66B 109.3 . . ?
Cl4 C66 H66A 109.3 . . ?
Cl4 C66 H66B 109.3 . . ?
Cl4 C66 Cl3 111.5(4) . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT602_3b                  
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info  
RESPONSE: the residual electron density is very diffuse and does 
not allow to locate additional solvent molecules. The crystal 
could have lost some solvent molecules while retaining its structure. 
Applying the squeeze procedure did not significantly improve the resolution 
indices.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_2cp
_database_code_depnum_ccdc_archive 'CCDC 1978289'
loop_
_audit_author_name
_audit_author_address
'Philippe Richard'
;Universite de Bourgogne
France
;
_audit_update_record             
;
2020-01-16 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_audit_creation_date             2019-11-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C138 H160 N4 O4 P4 Zr2'
_chemical_formula_sum            'C138 H160 N4 O4 P4 Zr2'
_chemical_formula_weight         2245.01
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.9665(10)
_cell_length_b                   27.0540(17)
_cell_length_c                   18.9109(12)
_cell_angle_alpha                90
_cell_angle_beta                 116.2737(18)
_cell_angle_gamma                90
_cell_volume                     7783.6(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9563
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.431
_cell_measurement_theta_min      2.781
_shelx_estimated_absorpt_T_max   0.938
_shelx_estimated_absorpt_T_min   0.934
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0608 before and 0.0551 after correction. The Ratio of minimum to maximum transmission is 0.9358. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.958
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            199749
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.581
_diffrn_reflns_theta_min         2.692
_diffrn_ambient_temperature      100
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Mo'
_diffrn_measurement_method       "φ and ω scans'"
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-90C'
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13604
_reflns_number_total             17921
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         17921
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0567
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0925P)²+12.7337P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1749
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C56(H56A,H56B), C63(H63A,H63B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
 C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C34(H34), C45(H45), C46(H46),
  C47(H47), C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54),
 C55(H55), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C65(H65), C66(H66),
  C67(H67), C68(H68), C69(H69)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.60834(18) 0.47342(10) 0.46545(15) 0.0218(5) Uani 1 1 d . . . . .
H1A H 0.622146 0.494717 0.512032 0.026 Uiso 1 1 calc R . . . .
H1B H 0.654122 0.447480 0.481063 0.026 Uiso 1 1 calc R . . . .
C2 C 0.52023(18) 0.44883(11) 0.44314(17) 0.0269(6) Uani 1 1 d . . . . .
H2A H 0.498933 0.434326 0.389775 0.032 Uiso 1 1 calc R . . . .
H2B H 0.477174 0.474128 0.441247 0.032 Uiso 1 1 calc R . . . .
C3 C 0.52529(18) 0.40844(10) 0.50107(16) 0.0228(5) Uani 1 1 d . . . . .
H3A H 0.538140 0.376708 0.482239 0.027 Uiso 1 1 calc R . . . .
H3B H 0.575390 0.415817 0.552664 0.027 Uiso 1 1 calc R . . . .
C4 C 0.70728(18) 0.65699(10) 0.45418(16) 0.0222(5) Uani 1 1 d . . . . .
C5 C 0.68717(18) 0.67350(10) 0.51474(16) 0.0236(5) Uani 1 1 d . . . . .
C6 C 0.71315(19) 0.71996(10) 0.54914(17) 0.0269(6) Uani 1 1 d . . . . .
H6 H 0.698870 0.730063 0.590186 0.032 Uiso 1 1 calc R . . . .
C7 C 0.7596(2) 0.75136(11) 0.52376(18) 0.0302(6) Uani 1 1 d . . . . .
C8 C 0.7836(2) 0.73370(11) 0.46665(17) 0.0292(6) Uani 1 1 d . . . . .
H8 H 0.817624 0.754715 0.450705 0.035 Uiso 1 1 calc R . . . .
C9 C 0.76079(19) 0.68727(10) 0.43152(17) 0.0257(6) Uani 1 1 d . . . . .
C10 C 0.79504(19) 0.66871(11) 0.37315(17) 0.0275(6) Uani 1 1 d . . . . .
C11 C 0.7190(2) 0.65995(12) 0.29208(17) 0.0308(6) Uani 1 1 d . . . . .
H11A H 0.676320 0.637532 0.296970 0.046 Uiso 1 1 calc GR . . . .
H11B H 0.741377 0.645156 0.257209 0.046 Uiso 1 1 calc GR . . . .
H11C H 0.690437 0.691515 0.269893 0.046 Uiso 1 1 calc GR . . . .
C12 C 0.8450(2) 0.62036(13) 0.4045(2) 0.0386(7) Uani 1 1 d . . . . .
H12A H 0.804755 0.595232 0.407038 0.058 Uiso 1 1 calc GR . . . .
H12B H 0.892761 0.625795 0.457382 0.058 Uiso 1 1 calc GR . . . .
H12C H 0.869632 0.609054 0.369194 0.058 Uiso 1 1 calc GR . . . .
C13 C 0.8574(2) 0.70609(14) 0.3634(2) 0.0430(8) Uani 1 1 d . . . . .
H13A H 0.907508 0.712175 0.414669 0.065 Uiso 1 1 calc GR . . . .
H13B H 0.826046 0.737172 0.342471 0.065 Uiso 1 1 calc GR . . . .
H13C H 0.878650 0.692825 0.326682 0.065 Uiso 1 1 calc GR . . . .
C14 C 0.7844(3) 0.80437(12) 0.5556(2) 0.0410(8) Uani 1 1 d . . . . .
C15 C 0.7546(4) 0.81705(15) 0.6178(3) 0.0625(12) Uani 1 1 d . . . . .
H15A H 0.690592 0.813448 0.595606 0.094 Uiso 1 1 calc GR . . . .
H15B H 0.770953 0.851233 0.635262 0.094 Uiso 1 1 calc GR . . . .
H15C H 0.782783 0.794679 0.662873 0.094 Uiso 1 1 calc GR . . . .
C16 C 0.7374(4) 0.84121(14) 0.4855(3) 0.0605(12) Uani 1 1 d . . . . .
H16A H 0.673606 0.837432 0.464500 0.091 Uiso 1 1 calc GR . . . .
H16B H 0.755272 0.834088 0.443811 0.091 Uiso 1 1 calc GR . . . .
H16C H 0.754033 0.875171 0.504196 0.091 Uiso 1 1 calc GR . . . .
C17 C 0.8819(3) 0.81296(18) 0.5879(3) 0.0727(14) Uani 1 1 d . . . . .
H17A H 0.913212 0.790994 0.632943 0.109 Uiso 1 1 calc GR . . . .
H17B H 0.895339 0.847429 0.604957 0.109 Uiso 1 1 calc GR . . . .
H17C H 0.900683 0.806054 0.546753 0.109 Uiso 1 1 calc GR . . . .
C18 C 0.6086(2) 0.66237(10) 0.61981(18) 0.0285(6) Uani 1 1 d . . . . .
C19 C 0.5448(2) 0.69933(11) 0.5876(2) 0.0349(7) Uani 1 1 d . . . . .
H19 H 0.514475 0.703256 0.531962 0.042 Uiso 1 1 calc R . . . .
C20 C 0.5258(3) 0.73031(13) 0.6366(3) 0.0482(10) Uani 1 1 d . . . . .
H20 H 0.482356 0.755337 0.614765 0.058 Uiso 1 1 calc R . . . .
C21 C 0.5706(3) 0.72438(16) 0.7171(3) 0.0608(12) Uani 1 1 d . . . . .
H21 H 0.558337 0.745954 0.750693 0.073 Uiso 1 1 calc R . . . .
C22 C 0.6319(3) 0.68821(18) 0.7495(2) 0.0573(11) Uani 1 1 d . . . . .
H22 H 0.661009 0.684361 0.805205 0.069 Uiso 1 1 calc R . . . .
C23 C 0.6525(2) 0.65665(14) 0.70142(19) 0.0409(8) Uani 1 1 d . . . . .
H23 H 0.695766 0.631643 0.724110 0.049 Uiso 1 1 calc R . . . .
C24 C 0.73130(19) 0.59098(11) 0.61696(16) 0.0264(6) Uani 1 1 d . . . . .
C25 C 0.7191(2) 0.54807(12) 0.65059(19) 0.0352(7) Uani 1 1 d . . . . .
H25 H 0.661137 0.536192 0.635444 0.042 Uiso 1 1 calc R . . . .
C26 C 0.7895(2) 0.52223(14) 0.7057(2) 0.0449(9) Uani 1 1 d . . . . .
H26 H 0.779812 0.492421 0.727244 0.054 Uiso 1 1 calc R . . . .
C27 C 0.8742(2) 0.53959(16) 0.7297(2) 0.0519(10) Uani 1 1 d . . . . .
H27 H 0.922814 0.522191 0.768412 0.062 Uiso 1 1 calc R . . . .
C28 C 0.8874(2) 0.58233(15) 0.6968(3) 0.0548(11) Uani 1 1 d . . . . .
H28 H 0.945419 0.594347 0.713015 0.066 Uiso 1 1 calc R . . . .
C29 C 0.8167(2) 0.60812(14) 0.6403(2) 0.0436(8) Uani 1 1 d . . . . .
H29 H 0.826634 0.637380 0.617634 0.052 Uiso 1 1 calc R . . . .
C30 C 0.61334(18) 0.54508(9) 0.23861(15) 0.0211(5) Uani 1 1 d . . . . .
C31 C 0.68094(18) 0.51293(10) 0.28808(15) 0.0214(5) Uani 1 1 d . . . . .
C32 C 0.74581(18) 0.49703(10) 0.26664(15) 0.0226(5) Uani 1 1 d . . . . .
H32 H 0.791895 0.476441 0.301722 0.027 Uiso 1 1 calc R . . . .
C33 C 0.74445(18) 0.51055(11) 0.19564(16) 0.0243(6) Uani 1 1 d . . . . .
C34 C 0.67216(19) 0.53852(10) 0.14429(16) 0.0249(6) Uani 1 1 d . . . . .
H34 H 0.668253 0.546143 0.093800 0.030 Uiso 1 1 calc R . . . .
C35 C 0.60567(18) 0.55593(9) 0.16191(15) 0.0214(5) Uani 1 1 d . . . . .
C36 C 0.52587(19) 0.58343(10) 0.10025(16) 0.0242(6) Uani 1 1 d . . . . .
C37 C 0.5229(2) 0.63694(11) 0.12568(17) 0.0300(6) Uani 1 1 d . . . . .
H37A H 0.521984 0.637123 0.177122 0.045 Uiso 1 1 calc GR . . . .
H37B H 0.469880 0.653179 0.086596 0.045 Uiso 1 1 calc GR . . . .
H37C H 0.575024 0.654711 0.129576 0.045 Uiso 1 1 calc GR . . . .
C38 C 0.4417(2) 0.55632(12) 0.08899(17) 0.0305(6) Uani 1 1 d . . . . .
H38A H 0.438589 0.554747 0.139486 0.046 Uiso 1 1 calc GR . . . .
H38B H 0.442246 0.522725 0.069846 0.046 Uiso 1 1 calc GR . . . .
H38C H 0.390364 0.574176 0.050451 0.046 Uiso 1 1 calc GR . . . .
C39 C 0.5268(2) 0.58484(12) 0.01916(17) 0.0321(7) Uani 1 1 d . . . . .
H39A H 0.526336 0.550998 0.000506 0.048 Uiso 1 1 calc GR . . . .
H39B H 0.579837 0.601906 0.023937 0.048 Uiso 1 1 calc GR . . . .
H39C H 0.474656 0.602510 -0.018556 0.048 Uiso 1 1 calc GR . . . .
C40 C 0.81444(19) 0.49364(12) 0.17046(17) 0.0309(6) Uani 1 1 d . . . . .
C41 C 0.8563(3) 0.53836(15) 0.1517(3) 0.0522(10) Uani 1 1 d . . . . .
H41A H 0.886102 0.558539 0.199309 0.078 Uiso 1 1 calc GR . . . .
H41B H 0.810646 0.558099 0.110384 0.078 Uiso 1 1 calc GR . . . .
H41C H 0.899123 0.527241 0.133439 0.078 Uiso 1 1 calc GR . . . .
C42 C 0.7709(2) 0.46061(16) 0.0977(2) 0.0482(9) Uani 1 1 d . . . . .
H42A H 0.744047 0.432007 0.110380 0.072 Uiso 1 1 calc GR . . . .
H42B H 0.815250 0.449244 0.081457 0.072 Uiso 1 1 calc GR . . . .
H42C H 0.725451 0.479421 0.054658 0.072 Uiso 1 1 calc GR . . . .
C43 C 0.8868(2) 0.46300(17) 0.2344(2) 0.0490(9) Uani 1 1 d . . . . .
H43A H 0.860917 0.433318 0.245299 0.073 Uiso 1 1 calc GR . . . .
H43B H 0.915361 0.482735 0.282574 0.073 Uiso 1 1 calc GR . . . .
H43C H 0.930353 0.453316 0.216108 0.073 Uiso 1 1 calc GR . . . .
C44 C 0.78810(19) 0.47210(11) 0.44283(16) 0.0265(6) Uani 1 1 d . . . . .
C45 C 0.8218(2) 0.50729(12) 0.50242(17) 0.0315(6) Uani 1 1 d . . . . .
H45 H 0.784874 0.532833 0.505253 0.038 Uiso 1 1 calc R . . . .
C46 C 0.9093(2) 0.50515(16) 0.5578(2) 0.0462(9) Uani 1 1 d . . . . .
H46 H 0.932217 0.529531 0.598003 0.055 Uiso 1 1 calc R . . . .
C47 C 0.9634(2) 0.46778(17) 0.5548(2) 0.0528(10) Uani 1 1 d . . . . .
H47 H 1.023063 0.466203 0.593114 0.063 Uiso 1 1 calc R . . . .
C48 C 0.9298(2) 0.43280(16) 0.4958(3) 0.0508(10) Uani 1 1 d . . . . .
H48 H 0.966834 0.407105 0.493621 0.061 Uiso 1 1 calc R . . . .
C49 C 0.8428(2) 0.43462(13) 0.4395(2) 0.0357(7) Uani 1 1 d . . . . .
H49 H 0.820499 0.410442 0.398986 0.043 Uiso 1 1 calc R . . . .
C50 C 0.6430(2) 0.41783(10) 0.32775(18) 0.0273(6) Uani 1 1 d . . . . .
C51 C 0.5960(2) 0.41128(12) 0.2467(2) 0.0378(7) Uani 1 1 d . . . . .
H51 H 0.579200 0.439191 0.212709 0.045 Uiso 1 1 calc R . . . .
C52 C 0.5736(3) 0.36408(14) 0.2154(2) 0.0541(10) Uani 1 1 d . . . . .
H52 H 0.541584 0.359631 0.159980 0.065 Uiso 1 1 calc R . . . .
C53 C 0.5983(3) 0.32345(14) 0.2652(3) 0.0580(11) Uani 1 1 d . . . . .
H53 H 0.585212 0.291104 0.243537 0.070 Uiso 1 1 calc R . . . .
C54 C 0.6415(3) 0.32947(13) 0.3459(3) 0.0497(9) Uani 1 1 d . . . . .
H54 H 0.655537 0.301465 0.379619 0.060 Uiso 1 1 calc R . . . .
C55 C 0.6643(2) 0.37638(12) 0.3777(2) 0.0371(7) Uani 1 1 d . . . . .
H55 H 0.694426 0.380582 0.433297 0.044 Uiso 1 1 calc R . . . .
C56 C 0.49502(19) 0.65894(10) 0.31015(16) 0.0249(6) Uani 1 1 d . . . . .
H56A H 0.540353 0.674735 0.298158 0.030 Uiso 1 1 calc R . . . .
H56B H 0.444263 0.652032 0.258763 0.030 Uiso 1 1 calc R . . . .
C57 C 0.4656(2) 0.69695(11) 0.34890(18) 0.0330(7) Uani 1 1 d . . . . .
C58 C 0.3821(3) 0.69456(13) 0.3477(2) 0.0462(9) Uani 1 1 d . . . . .
H58 H 0.344306 0.667725 0.321413 0.055 Uiso 1 1 calc R . . . .
C59 C 0.3532(3) 0.73019(15) 0.3836(3) 0.0561(10) Uani 1 1 d . . . . .
H59 H 0.296302 0.727581 0.381294 0.067 Uiso 1 1 calc R . . . .
C60 C 0.4074(3) 0.76977(14) 0.4231(2) 0.0532(10) Uani 1 1 d . . . . .
H60 H 0.387672 0.794467 0.447263 0.064 Uiso 1 1 calc R . . . .
C61 C 0.4896(3) 0.77240(12) 0.4264(2) 0.0450(9) Uani 1 1 d . . . . .
H61 H 0.527241 0.798966 0.454010 0.054 Uiso 1 1 calc R . . . .
C62 C 0.5191(2) 0.73716(11) 0.39035(19) 0.0363(7) Uani 1 1 d . . . . .
H62 H 0.576445 0.740172 0.393645 0.044 Uiso 1 1 calc R . . . .
C63 C 0.40830(19) 0.55445(10) 0.32092(16) 0.0251(6) Uani 1 1 d . . . . .
H63A H 0.407097 0.530621 0.360163 0.030 Uiso 1 1 calc R . . . .
H63B H 0.372906 0.583337 0.321746 0.030 Uiso 1 1 calc R . . . .
C64 C 0.3611(2) 0.53092(12) 0.24202(18) 0.0327(7) Uani 1 1 d . . . . .
C65 C 0.2916(2) 0.55376(15) 0.1797(2) 0.0449(8) Uani 1 1 d . . . . .
H65 H 0.274786 0.586196 0.186770 0.054 Uiso 1 1 calc R . . . .
C66 C 0.2459(3) 0.53042(18) 0.1074(2) 0.0556(10) Uani 1 1 d . . . . .
H66 H 0.198136 0.546895 0.066212 0.067 Uiso 1 1 calc R . . . .
C67 C 0.2691(3) 0.48380(17) 0.0949(2) 0.0570(11) Uani 1 1 d . . . . .
H67 H 0.237085 0.467628 0.045806 0.068 Uiso 1 1 calc R . . . .
C68 C 0.3407(3) 0.46047(15) 0.1558(2) 0.0507(10) Uani 1 1 d . . . . .
H68 H 0.358382 0.428482 0.147749 0.061 Uiso 1 1 calc R . . . .
C69 C 0.3849(2) 0.48361(12) 0.22644(19) 0.0379(7) Uani 1 1 d . . . . .
H69 H 0.433712 0.467315 0.266796 0.045 Uiso 1 1 calc R . . . .
N1 N 0.55540(15) 0.59816(8) 0.48651(13) 0.0198(4) Uani 1 1 d . . . . .
N2 N 0.61304(15) 0.50408(8) 0.40167(12) 0.0199(4) Uani 1 1 d . . . . .
O1 O 0.67693(12) 0.61306(7) 0.42218(11) 0.0225(4) Uani 1 1 d . . . . .
O2 O 0.55912(12) 0.56426(7) 0.26461(11) 0.0212(4) Uani 1 1 d . . . . .
P1 P 0.63816(5) 0.62840(2) 0.55295(4) 0.02113(15) Uani 1 1 d . . . . .
P2 P 0.67562(4) 0.47937(2) 0.36735(4) 0.01915(14) Uani 1 1 d . . . . .
Zr Zr 0.55232(2) 0.58135(2) 0.36667(2) 0.01863(8) 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
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.516(4) . ?
C1 N2 1.495(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.523(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 N1 1.499(3) 3_666 ?
C4 C5 1.405(4) . ?
C4 C9 1.422(4) . ?
C4 O1 1.330(3) . ?
C5 C6 1.394(4) . ?
C5 P1 1.798(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.381(4) . ?
C7 C8 1.396(4) . ?
C7 C14 1.540(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.393(4) . ?
C9 C10 1.541(4) . ?
C10 C11 1.523(4) . ?
C10 C12 1.529(4) . ?
C10 C13 1.533(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.511(5) . ?
C14 C16 1.566(6) . ?
C14 C17 1.506(6) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.399(5) . ?
C18 C23 1.394(4) . ?
C18 P1 1.805(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.390(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.378(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.361(7) . ?
C22 H22 0.9500 . ?
C22 C23 1.400(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(4) . ?
C24 C29 1.394(4) . ?
C24 P1 1.815(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.378(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.385(5) . ?
C27 H27 0.9500 . ?
C27 C28 1.377(5) . ?
C28 H28 0.9500 . ?
C28 C29 1.390(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.413(4) . ?
C30 C35 1.428(3) . ?
C30 O2 1.326(3) . ?
C31 C32 1.399(4) . ?
C31 P2 1.789(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.382(4) . ?
C33 C34 1.402(4) . ?
C33 C40 1.532(4) . ?
C34 H34 0.9500 . ?
C34 C35 1.392(4) . ?
C35 C36 1.533(4) . ?
C36 C37 1.533(4) . ?
C36 C38 1.535(4) . ?
C36 C39 1.541(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.522(5) . ?
C40 C42 1.529(5) . ?
C40 C43 1.530(5) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.390(4) . ?
C44 C49 1.394(4) . ?
C44 P2 1.818(3) . ?
C45 H45 0.9500 . ?
C45 C46 1.389(5) . ?
C46 H46 0.9500 . ?
C46 C47 1.382(6) . ?
C47 H47 0.9500 . ?
C47 C48 1.380(6) . ?
C48 H48 0.9500 . ?
C48 C49 1.387(5) . ?
C49 H49 0.9500 . ?
C50 C51 1.391(4) . ?
C50 C55 1.407(4) . ?
C50 P2 1.809(3) . ?
C51 H51 0.9500 . ?
C51 C52 1.388(5) . ?
C52 H52 0.9500 . ?
C52 C53 1.387(6) . ?
C53 H53 0.9500 . ?
C53 C54 1.379(6) . ?
C54 H54 0.9500 . ?
C54 C55 1.384(5) . ?
C55 H55 0.9500 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C57 1.472(4) . ?
C56 Zr 2.361(3) . ?
C57 C58 1.409(5) . ?
C57 C62 1.411(5) . ?
C58 H58 0.9500 . ?
C58 C59 1.387(5) . ?
C59 H59 0.9500 . ?
C59 C60 1.393(6) . ?
C60 H60 0.9500 . ?
C60 C61 1.370(6) . ?
C61 H61 0.9500 . ?
C61 C62 1.388(5) . ?
C62 H62 0.9500 . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.488(4) . ?
C63 Zr 2.319(3) . ?
C64 C65 1.390(5) . ?
C64 C69 1.412(5) . ?
C65 H65 0.9500 . ?
C65 C66 1.390(5) . ?
C66 H66 0.9500 . ?
C66 C67 1.372(6) . ?
C67 H67 0.9500 . ?
C67 C68 1.400(6) . ?
C68 H68 0.9500 . ?
C68 C69 1.361(5) . ?
C69 H69 0.9500 . ?
N1 P1 1.630(2) . ?
N1 Zr 2.289(2) . ?
N2 P2 1.614(2) . ?
N2 Zr 2.295(2) . ?
O1 Zr 2.0840(19) . ?
O2 Zr 2.0370(18) . ?

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
H1A C1 H1B 107.6 . . ?
C2 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
N2 C1 H1A 108.6 . . ?
N2 C1 H1B 108.6 . . ?
N2 C1 C2 114.7(2) . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C1 C2 C3 112.3(2) . . ?
H2A C2 H2B 107.9 . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
C2 C3 H3A 108.4 . . ?
C2 C3 H3B 108.4 . . ?
H3A C3 H3B 107.4 . . ?
N1 C3 C2 115.7(2) 3_666 . ?
N1 C3 H3A 108.4 3_666 . ?
N1 C3 H3B 108.4 3_666 . ?
C5 C4 C9 118.7(2) . . ?
O1 C4 C5 118.0(2) . . ?
O1 C4 C9 123.2(2) . . ?
C4 C5 P1 115.7(2) . . ?
C6 C5 C4 121.8(2) . . ?
C6 C5 P1 122.1(2) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.2(3) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 C8 117.7(3) . . ?
C6 C7 C14 122.4(3) . . ?
C8 C7 C14 119.9(3) . . ?
C7 C8 H8 117.9 . . ?
C9 C8 C7 124.3(3) . . ?
C9 C8 H8 117.9 . . ?
C4 C9 C10 121.4(2) . . ?
C8 C9 C4 117.1(2) . . ?
C8 C9 C10 121.5(2) . . ?
C11 C10 C9 110.6(2) . . ?
C11 C10 C12 109.5(3) . . ?
C11 C10 C13 107.7(3) . . ?
C12 C10 C9 108.7(2) . . ?
C12 C10 C13 108.5(3) . . ?
C13 C10 C9 111.8(2) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C14 C16 108.2(3) . . ?
C15 C14 C7 112.8(3) . . ?
C15 C14 C16 107.1(3) . . ?
C17 C14 C7 111.3(3) . . ?
C17 C14 C15 109.7(4) . . ?
C17 C14 C16 107.5(4) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 P1 117.4(2) . . ?
C23 C18 C19 119.5(3) . . ?
C23 C18 P1 122.8(3) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 C18 120.2(3) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 120.3 . . ?
C21 C20 C19 119.3(4) . . ?
C21 C20 H20 120.3 . . ?
C20 C21 H21 119.4 . . ?
C22 C21 C20 121.3(3) . . ?
C22 C21 H21 119.4 . . ?
C21 C22 H22 119.8 . . ?
C21 C22 C23 120.5(4) . . ?
C23 C22 H22 119.8 . . ?
C18 C23 C22 119.2(4) . . ?
C18 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C25 C24 C29 118.7(3) . . ?
C25 C24 P1 120.8(2) . . ?
C29 C24 P1 120.1(2) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 C24 121.2(3) . . ?
C26 C25 H25 119.4 . . ?
C25 C26 H26 119.9 . . ?
C25 C26 C27 120.2(3) . . ?
C27 C26 H26 119.9 . . ?
C26 C27 H27 120.4 . . ?
C28 C27 C26 119.3(3) . . ?
C28 C27 H27 120.4 . . ?
C27 C28 H28 119.6 . . ?
C27 C28 C29 120.8(3) . . ?
C29 C28 H28 119.6 . . ?
C24 C29 H29 120.1 . . ?
C28 C29 C24 119.9(3) . . ?
C28 C29 H29 120.1 . . ?
C31 C30 C35 118.8(2) . . ?
O2 C30 C31 119.2(2) . . ?
O2 C30 C35 122.0(2) . . ?
C30 C31 P2 122.7(2) . . ?
C32 C31 C30 120.6(2) . . ?
C32 C31 P2 115.1(2) . . ?
C31 C32 H32 119.2 . . ?
C33 C32 C31 121.6(2) . . ?
C33 C32 H32 119.2 . . ?
C32 C33 C34 116.7(2) . . ?
C32 C33 C40 122.8(3) . . ?
C34 C33 C40 120.5(2) . . ?
C33 C34 H34 117.6 . . ?
C35 C34 C33 124.7(2) . . ?
C35 C34 H34 117.6 . . ?
C30 C35 C36 121.7(2) . . ?
C34 C35 C30 117.0(2) . . ?
C34 C35 C36 121.2(2) . . ?
C35 C36 C37 111.1(2) . . ?
C35 C36 C38 109.2(2) . . ?
C35 C36 C39 112.0(2) . . ?
C37 C36 C38 109.7(2) . . ?
C37 C36 C39 107.7(2) . . ?
C38 C36 C39 107.0(2) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C40 C33 109.9(3) . . ?
C41 C40 C42 110.2(3) . . ?
C41 C40 C43 108.7(3) . . ?
C42 C40 C33 108.8(3) . . ?
C42 C40 C43 107.1(3) . . ?
C43 C40 C33 112.2(2) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 C44 C49 119.4(3) . . ?
C45 C44 P2 118.3(2) . . ?
C49 C44 P2 122.1(2) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 C44 120.1(3) . . ?
C46 C45 H45 120.0 . . ?
C45 C46 H46 119.8 . . ?
C47 C46 C45 120.5(4) . . ?
C47 C46 H46 119.8 . . ?
C46 C47 H47 120.3 . . ?
C48 C47 C46 119.4(3) . . ?
C48 C47 H47 120.3 . . ?
C47 C48 H48 119.5 . . ?
C47 C48 C49 120.9(4) . . ?
C49 C48 H48 119.5 . . ?
C44 C49 H49 120.2 . . ?
C48 C49 C44 119.7(3) . . ?
C48 C49 H49 120.2 . . ?
C51 C50 C55 119.4(3) . . ?
C51 C50 P2 119.6(2) . . ?
C55 C50 P2 121.0(2) . . ?
C50 C51 H51 119.9 . . ?
C52 C51 C50 120.2(3) . . ?
C52 C51 H51 119.9 . . ?
C51 C52 H52 120.1 . . ?
C53 C52 C51 119.7(4) . . ?
C53 C52 H52 120.1 . . ?
C52 C53 H53 119.6 . . ?
C54 C53 C52 120.8(3) . . ?
C54 C53 H53 119.6 . . ?
C53 C54 H54 120.0 . . ?
C53 C54 C55 119.9(4) . . ?
C55 C54 H54 120.0 . . ?
C50 C55 H55 120.0 . . ?
C54 C55 C50 120.0(3) . . ?
C54 C55 H55 120.0 . . ?
H56A C56 H56B 106.4 . . ?
C57 C56 H56A 106.3 . . ?
C57 C56 H56B 106.3 . . ?
C57 C56 Zr 123.93(18) . . ?
Zr C56 H56A 106.3 . . ?
Zr C56 H56B 106.3 . . ?
C58 C57 C56 121.3(3) . . ?
C58 C57 C62 116.1(3) . . ?
C62 C57 C56 122.6(3) . . ?
C57 C58 H58 119.0 . . ?
C59 C58 C57 122.0(4) . . ?
C59 C58 H58 119.0 . . ?
C58 C59 H59 119.8 . . ?
C58 C59 C60 120.3(4) . . ?
C60 C59 H59 119.8 . . ?
C59 C60 H60 120.6 . . ?
C61 C60 C59 118.7(3) . . ?
C61 C60 H60 120.6 . . ?
C60 C61 H61 119.2 . . ?
C60 C61 C62 121.6(4) . . ?
C62 C61 H61 119.2 . . ?
C57 C62 H62 119.4 . . ?
C61 C62 C57 121.2(3) . . ?
C61 C62 H62 119.4 . . ?
H63A C63 H63B 106.8 . . ?
C64 C63 H63A 107.0 . . ?
C64 C63 H63B 107.0 . . ?
C64 C63 Zr 121.25(19) . . ?
Zr C63 H63A 107.0 . . ?
Zr C63 H63B 107.0 . . ?
C65 C64 C63 122.5(3) . . ?
C65 C64 C69 116.1(3) . . ?
C69 C64 C63 121.3(3) . . ?
C64 C65 H65 119.1 . . ?
C64 C65 C66 121.8(4) . . ?
C66 C65 H65 119.1 . . ?
C65 C66 H66 119.7 . . ?
C67 C66 C65 120.6(4) . . ?
C67 C66 H66 119.7 . . ?
C66 C67 H67 120.5 . . ?
C66 C67 C68 118.9(4) . . ?
C68 C67 H67 120.5 . . ?
C67 C68 H68 120.0 . . ?
C69 C68 C67 120.0(4) . . ?
C69 C68 H68 120.0 . . ?
C64 C69 H69 118.8 . . ?
C68 C69 C64 122.5(4) . . ?
C68 C69 H69 118.8 . . ?
C3 N1 P1 118.29(17) 3_666 . ?
C3 N1 Zr 120.62(16) 3_666 . ?
P1 N1 Zr 119.81(11) . . ?
C1 N2 P2 111.98(17) . . ?
C1 N2 Zr 124.11(16) . . ?
P2 N2 Zr 123.54(11) . . ?
C4 O1 Zr 134.38(17) . . ?
C30 O2 Zr 141.24(17) . . ?
C5 P1 C18 104.93(13) . . ?
C5 P1 C24 103.03(13) . . ?
C18 P1 C24 104.28(14) . . ?
N1 P1 C5 115.12(12) . . ?
N1 P1 C18 112.57(13) . . ?
N1 P1 C24 115.64(13) . . ?
C31 P2 C44 106.74(13) . . ?
C31 P2 C50 103.88(13) . . ?
C50 P2 C44 104.35(14) . . ?
N2 P2 C31 114.39(12) . . ?
N2 P2 C44 112.20(12) . . ?
N2 P2 C50 114.36(12) . . ?
C63 Zr C56 87.45(10) . . ?
N1 Zr C56 95.50(9) . . ?
N1 Zr C63 89.44(9) . . ?
N1 Zr N2 94.87(8) . . ?
N2 Zr C56 169.38(8) . . ?
N2 Zr C63 94.93(9) . . ?
O1 Zr C56 89.12(9) . . ?
O1 Zr C63 169.63(8) . . ?
O1 Zr N1 81.15(7) . . ?
O1 Zr N2 90.23(8) . . ?
O2 Zr C56 87.56(8) . . ?
O2 Zr C63 93.87(9) . . ?
O2 Zr N1 175.59(8) . . ?
O2 Zr N2 81.96(7) . . ?
O2 Zr O1 95.76(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 N1 147.2(2) . . . 3_666 ?
C1 N2 P2 C31 177.70(17) . . . . ?
C1 N2 P2 C44 -60.5(2) . . . . ?
C1 N2 P2 C50 58.1(2) . . . . ?
C2 C1 N2 P2 -110.4(2) . . . . ?
C2 C1 N2 Zr 76.5(3) . . . . ?
C3 N1 P1 C5 -134.58(19) 3_666 . . . ?
C3 N1 P1 C18 -14.4(2) 3_666 . . . ?
C3 N1 P1 C24 105.3(2) 3_666 . . . ?
C4 C5 C6 C7 0.3(5) . . . . ?
C4 C5 P1 C18 -173.3(2) . . . . ?
C4 C5 P1 C24 77.8(2) . . . . ?
C4 C5 P1 N1 -49.0(3) . . . . ?
C4 C9 C10 C11 64.9(4) . . . . ?
C4 C9 C10 C12 -55.4(4) . . . . ?
C4 C9 C10 C13 -175.2(3) . . . . ?
C5 C4 C9 C8 -5.5(4) . . . . ?
C5 C4 C9 C10 172.2(3) . . . . ?
C5 C4 O1 Zr 56.8(3) . . . . ?
C5 C6 C7 C8 -3.8(5) . . . . ?
C5 C6 C7 C14 175.7(3) . . . . ?
C6 C5 P1 C18 14.0(3) . . . . ?
C6 C5 P1 C24 -94.8(3) . . . . ?
C6 C5 P1 N1 138.3(2) . . . . ?
C6 C7 C8 C9 2.6(5) . . . . ?
C6 C7 C14 C15 1.4(5) . . . . ?
C6 C7 C14 C16 -117.0(4) . . . . ?
C6 C7 C14 C17 125.1(4) . . . . ?
C7 C8 C9 C4 2.1(5) . . . . ?
C7 C8 C9 C10 -175.6(3) . . . . ?
C8 C7 C14 C15 -179.1(4) . . . . ?
C8 C7 C14 C16 62.5(4) . . . . ?
C8 C7 C14 C17 -55.4(5) . . . . ?
C8 C9 C10 C11 -117.5(3) . . . . ?
C8 C9 C10 C12 122.1(3) . . . . ?
C8 C9 C10 C13 2.4(4) . . . . ?
C9 C4 C5 C6 4.4(4) . . . . ?
C9 C4 C5 P1 -168.2(2) . . . . ?
C9 C4 O1 Zr -125.0(3) . . . . ?
C14 C7 C8 C9 -176.9(3) . . . . ?
C18 C19 C20 C21 0.3(5) . . . . ?
C19 C18 C23 C22 -0.2(5) . . . . ?
C19 C18 P1 C5 64.3(3) . . . . ?
C19 C18 P1 C24 172.2(2) . . . . ?
C19 C18 P1 N1 -61.7(3) . . . . ?
C19 C20 C21 C22 -1.2(6) . . . . ?
C20 C21 C22 C23 1.4(6) . . . . ?
C21 C22 C23 C18 -0.7(6) . . . . ?
C23 C18 C19 C20 0.4(5) . . . . ?
C23 C18 P1 C5 -109.1(3) . . . . ?
C23 C18 P1 C24 -1.1(3) . . . . ?
C23 C18 P1 N1 125.0(3) . . . . ?
C24 C25 C26 C27 1.4(6) . . . . ?
C25 C24 C29 C28 -0.5(5) . . . . ?
C25 C24 P1 C5 -172.1(3) . . . . ?
C25 C24 P1 C18 78.5(3) . . . . ?
C25 C24 P1 N1 -45.6(3) . . . . ?
C25 C26 C27 C28 -1.2(7) . . . . ?
C26 C27 C28 C29 0.2(7) . . . . ?
C27 C28 C29 C24 0.7(7) . . . . ?
C29 C24 C25 C26 -0.5(5) . . . . ?
C29 C24 P1 C5 15.4(3) . . . . ?
C29 C24 P1 C18 -93.9(3) . . . . ?
C29 C24 P1 N1 141.9(3) . . . . ?
C30 C31 C32 C33 -2.4(4) . . . . ?
C30 C31 P2 C44 -149.3(2) . . . . ?
C30 C31 P2 C50 100.8(2) . . . . ?
C30 C31 P2 N2 -24.6(3) . . . . ?
C30 C35 C36 C37 66.8(3) . . . . ?
C30 C35 C36 C38 -54.3(3) . . . . ?
C30 C35 C36 C39 -172.6(2) . . . . ?
C31 C30 C35 C34 -7.3(4) . . . . ?
C31 C30 C35 C36 169.9(2) . . . . ?
C31 C30 O2 Zr 24.1(4) . . . . ?
C31 C32 C33 C34 -3.7(4) . . . . ?
C31 C32 C33 C40 -179.9(3) . . . . ?
C32 C31 P2 C44 44.8(2) . . . . ?
C32 C31 P2 C50 -65.1(2) . . . . ?
C32 C31 P2 N2 169.50(19) . . . . ?
C32 C33 C34 C35 4.2(4) . . . . ?
C32 C33 C40 C41 -124.1(3) . . . . ?
C32 C33 C40 C42 115.2(3) . . . . ?
C32 C33 C40 C43 -3.0(4) . . . . ?
C33 C34 C35 C30 1.3(4) . . . . ?
C33 C34 C35 C36 -176.0(3) . . . . ?
C34 C33 C40 C41 59.8(4) . . . . ?
C34 C33 C40 C42 -60.9(4) . . . . ?
C34 C33 C40 C43 -179.1(3) . . . . ?
C34 C35 C36 C37 -116.0(3) . . . . ?
C34 C35 C36 C38 122.9(3) . . . . ?
C34 C35 C36 C39 4.5(4) . . . . ?
C35 C30 C31 C32 8.0(4) . . . . ?
C35 C30 C31 P2 -157.1(2) . . . . ?
C35 C30 O2 Zr -155.9(2) . . . . ?
C40 C33 C34 C35 -179.4(3) . . . . ?
C44 C45 C46 C47 -0.8(5) . . . . ?
C45 C44 C49 C48 0.2(5) . . . . ?
C45 C44 P2 C31 92.7(2) . . . . ?
C45 C44 P2 C50 -157.7(2) . . . . ?
C45 C44 P2 N2 -33.3(3) . . . . ?
C45 C46 C47 C48 0.6(6) . . . . ?
C46 C47 C48 C49 0.0(6) . . . . ?
C47 C48 C49 C44 -0.4(5) . . . . ?
C49 C44 C45 C46 0.4(4) . . . . ?
C49 C44 P2 C31 -82.7(3) . . . . ?
C49 C44 P2 C50 26.9(3) . . . . ?
C49 C44 P2 N2 151.2(2) . . . . ?
C50 C51 C52 C53 0.1(6) . . . . ?
C51 C50 C55 C54 2.4(5) . . . . ?
C51 C50 P2 C31 -25.6(3) . . . . ?
C51 C50 P2 C44 -137.3(3) . . . . ?
C51 C50 P2 N2 99.7(3) . . . . ?
C51 C52 C53 C54 2.8(7) . . . . ?
C52 C53 C54 C55 -3.0(7) . . . . ?
C53 C54 C55 C50 0.4(6) . . . . ?
C55 C50 C51 C52 -2.6(5) . . . . ?
C55 C50 P2 C31 154.4(2) . . . . ?
C55 C50 P2 C44 42.8(3) . . . . ?
C55 C50 P2 N2 -80.2(3) . . . . ?
C56 C57 C58 C59 -179.7(3) . . . . ?
C56 C57 C62 C61 -179.9(3) . . . . ?
C57 C58 C59 C60 -0.5(6) . . . . ?
C58 C57 C62 C61 -1.0(4) . . . . ?
C58 C59 C60 C61 -0.7(6) . . . . ?
C59 C60 C61 C62 1.1(6) . . . . ?
C60 C61 C62 C57 -0.2(5) . . . . ?
C62 C57 C58 C59 1.3(5) . . . . ?
C63 C64 C65 C66 -177.3(3) . . . . ?
C63 C64 C69 C68 177.4(3) . . . . ?
C64 C65 C66 C67 -0.8(6) . . . . ?
C65 C64 C69 C68 -2.6(5) . . . . ?
C65 C66 C67 C68 -1.2(6) . . . . ?
C66 C67 C68 C69 1.3(6) . . . . ?
C67 C68 C69 C64 0.6(6) . . . . ?
C69 C64 C65 C66 2.6(5) . . . . ?
N2 C1 C2 C3 165.6(2) . . . . ?
O1 C4 C5 C6 -177.2(3) . . . . ?
O1 C4 C5 P1 10.1(3) . . . . ?
O1 C4 C9 C8 176.3(3) . . . . ?
O1 C4 C9 C10 -6.1(4) . . . . ?
O2 C30 C31 C32 -171.9(2) . . . . ?
O2 C30 C31 P2 22.9(3) . . . . ?
O2 C30 C35 C34 172.6(2) . . . . ?
O2 C30 C35 C36 -10.1(4) . . . . ?
P1 C5 C6 C7 172.5(2) . . . . ?
P1 C18 C19 C20 -173.2(2) . . . . ?
P1 C18 C23 C22 173.0(3) . . . . ?
P1 C24 C25 C26 -173.1(3) . . . . ?
P1 C24 C29 C28 172.1(3) . . . . ?
P2 C31 C32 C33 163.9(2) . . . . ?
P2 C44 C45 C46 -175.2(3) . . . . ?
P2 C44 C49 C48 175.6(3) . . . . ?
P2 C50 C51 C52 177.4(3) . . . . ?
P2 C50 C55 C54 -177.7(3) . . . . ?
Zr C56 C57 C58 -80.8(4) . . . . ?
Zr C56 C57 C62 98.1(3) . . . . ?
Zr C63 C64 C65 -110.9(3) . . . . ?
Zr C63 C64 C69 69.2(3) . . . . ?
Zr N1 P1 C5 32.58(18) . . . . ?
Zr N1 P1 C18 152.77(13) . . . . ?
Zr N1 P1 C24 -87.51(15) . . . . ?
Zr N2 P2 C31 -9.11(19) . . . . ?
Zr N2 P2 C44 112.67(15) . . . . ?
Zr N2 P2 C50 -128.74(15) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.804 -0.763 2666.6 39.0 ?


_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
