# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_ba_sb55
_database_code_depnum_ccdc_archive 'CCDC 1530472'
_audit_update_record             
;
2017-03-17 deposited with the CCDC.
2017-04-05 downloaded from the CCDC.
;
_audit_creation_date             2016-04-05

_audit_block_code                ba_sb55
_audit_block_refno               2690
_audit_block_usercomment         'sb_dh16, irregular, yellow'


# start Validation Reply Form
_vrf_PLAT910_ba_sb55             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          14 Note
RESPONSE: limited by diffractometer.
;
# end Validation Reply Form

_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C45 H38 Cl N P2 Zr, C4 H10 O'
_chemical_formula_sum            'C49 H48 Cl N O P2 Zr'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         855.49
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_diffrn_ambient_temperature      120(1)
_chemical_oxdiff_formula         'C49 H48 Cl1 N1 O1 P2 Zr'
_chemical_oxdiff_usercomment     'sb_dh16, irregular, yellow'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration .

_space_group_name_Hall           '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.1149(2)
_cell_length_b                   12.1996(2)
_cell_length_c                   28.4817(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.1112(15)
_cell_angle_gamma                90
_cell_volume                     4208.73(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    20092
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      29.8050
_cell_measurement_theta_min      3.3080
_shelx_estimated_absorpt_T_max   0.957
_shelx_estimated_absorpt_T_min   0.957
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41p (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1776
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
13 -10 11 0.0358
-11 7 26 0.0455
11 -7 -26 0.0455
-7 -1 -36 0.0375
7 1 36 0.0375
-10 -14 3 0.0506
11 13 -3 0.0477
-15 8 -10 0.0325
-9 9 29 0.0407
-5 -3 38 0.0533
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.075
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
12.9930 -9.9964 11.0107 -0.0189 0.3075 0.9508
-10.9988 6.9978 25.9938 0.8216 0.0030 -0.5551
10.9988 -6.9978 -25.9938 -0.8216 -0.0030 0.5551
-6.9931 -1.0028 -36.0050 -0.8035 0.0121 -0.5863
6.9931 1.0028 36.0050 0.8035 -0.0121 0.5863
-9.9988 -14.0029 3.0017 -0.0783 0.9663 -0.2662
10.9983 13.0032 -3.0009 0.0531 -0.9349 0.3382
-14.9927 7.9959 -10.0107 0.0260 -0.1542 -1.0160
-8.9994 8.9996 28.9975 0.9086 -0.1292 -0.4646
-4.9999 -2.9999 37.9981 0.8856 0.4648 0.0251

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            106852
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.555
_diffrn_reflns_theta_min         3.175
_diffrn_ambient_environment      perfluoro
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     10.00  48.00   0.50   17.50    --   26.87  57.00-180.00   76
  2  ω     59.00  96.00   0.50   17.50    --   26.87  57.00-180.00   74
  3  ω      7.00  52.00   0.50   17.50    --   26.87  57.00 -30.00   90
  4  ω     55.00  96.00   0.50   17.50    --   26.87  57.00 -30.00   82
  5  ω    -20.00  69.00   0.50   17.50    --   26.87 -99.00 -60.00  178
  6  ω     -3.00  35.00   0.50   17.50    --   26.87  77.00-150.00   76
  7  ω     59.00  97.00   0.50   17.50    --   26.87  77.00-150.00   76
  8  ω    -18.00   9.00   0.50   17.50    --   26.87 -99.00   0.00   54
  9  ω     39.00  66.00   0.50   17.50    --   26.87 -99.00   0.00   54
 10  ω     -1.00  25.00   0.50   17.50    --   26.87  77.00  60.00   52
 11  ω    -42.00 -16.00   0.50   17.50    --   26.87 -57.00-180.00   52
 12  ω     -1.00  45.00   0.50   17.50    --   26.87 -57.00-180.00   92
 13  ω     -3.00  26.00   0.50   17.50    --   26.87  77.00 -60.00   58
 14  ω    -35.00   6.00   0.50   17.50    --   26.87 -77.00  90.00   82
 15  ω      6.00  37.00   0.50   17.50    --   26.87  77.00  90.00   62
 16  ω      6.00  31.00   0.50   17.50    --   26.87  57.00  30.00   50
 17  ω      3.00  30.00   0.50   17.50    --   26.87  38.00 -60.00   54
 18  ω     70.00  99.00   0.50   17.50    --   26.87  38.00 -60.00   58
 19  ω    -17.00  64.00   0.50   17.50    --   26.87 -99.00  30.00  162
 20  ω      3.00  99.00   0.50   17.50    --   26.87  38.00 150.00  192
 21  ω    -12.00  72.00   0.50   17.50    --   26.87-106.00 143.00  168
 22  ω    -17.00  16.00   0.50   17.50    --   26.87 -99.00-150.00   66
 23  ω     25.00  51.00   0.50   17.50    --   26.87 -99.00-150.00   52
 24  ω      1.00  90.00   0.50   17.50    --   26.87  38.00  90.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0085155000
_diffrn_orient_matrix_UB_12      0.0167111000
_diffrn_orient_matrix_UB_13      0.0235062000
_diffrn_orient_matrix_UB_21      -0.0213137000
_diffrn_orient_matrix_UB_22      -0.0526549000
_diffrn_orient_matrix_UB_23      0.0052705000
_diffrn_orient_matrix_UB_31      0.0538874000
_diffrn_orient_matrix_UB_32      -0.0181094000
_diffrn_orient_matrix_UB_33      0.0063207000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9920
_reflns_number_total             12873
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         1.816
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         12873
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0470
_refine_ls_restrained_S_all      1.051
_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)+(0.0521P)²+4.3808P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1204
_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 distances
 O51-C51 \\sim O51-C53
 with sigma of 0.005
 C51-C52 \\sim C53-C54
 with sigma of 0.005
 O51-C52 \\sim O51-C54
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O51, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C45(H45A,H45B), C51(H51A,H51B), C53(H53A,H53B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42),
  C43(H43), C44(H44)
4.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C54(H54A,H54B,H54C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.32814(2) 0.41200(2) 0.19809(2) 0.01564(6) Uani 1 1 d . . . . .
Cl Cl 0.28468(5) 0.23289(4) 0.23653(2) 0.02131(11) Uani 1 1 d . . . . .
P1 P 0.32556(5) 0.30319(5) 0.11811(2) 0.01768(12) Uani 1 1 d . . . . .
P2 P 0.09936(5) 0.43468(5) 0.19108(2) 0.01731(12) Uani 1 1 d . . . . .
N N 0.31222(15) 0.53512(15) 0.14715(7) 0.0176(4) Uani 1 1 d . . . . .
C1 C 0.45511(19) 0.34422(19) 0.14385(8) 0.0199(4) Uani 1 1 d . . . . .
H1 H 0.512(2) 0.286(2) 0.1470(10) 0.024 Uiso 1 1 d R . . . .
C2 C 0.49781(19) 0.4561(2) 0.14393(8) 0.0198(4) Uani 1 1 d . . . . .
C3 C 0.42932(19) 0.55064(19) 0.14468(8) 0.0191(4) Uani 1 1 d . . . . .
C4 C 0.4759(2) 0.6558(2) 0.14783(8) 0.0239(5) Uani 1 1 d . . . . .
H4 H 0.4288 0.7181 0.1478 0.029 Uiso 1 1 calc R . . . .
C5 C 0.5886(2) 0.6706(2) 0.15091(9) 0.0274(5) Uani 1 1 d . . . . .
H5 H 0.6193 0.7422 0.1519 0.033 Uiso 1 1 calc R . . . .
C6 C 0.6571(2) 0.5781(2) 0.15263(9) 0.0281(5) Uani 1 1 d . . . . .
H6 H 0.7347 0.5871 0.1561 0.034 Uiso 1 1 calc R . . . .
C7 C 0.6134(2) 0.4747(2) 0.14940(8) 0.0248(5) Uani 1 1 d . . . . .
H7 H 0.6618 0.4135 0.1509 0.030 Uiso 1 1 calc R . . . .
C8 C 0.30418(19) 0.35537(18) 0.05857(8) 0.0195(4) Uani 1 1 d . . . . .
C9 C 0.1962(2) 0.3758(2) 0.04262(8) 0.0215(5) Uani 1 1 d . . . . .
H9 H 0.1360 0.3643 0.0629 0.026 Uiso 1 1 calc R . . . .
C10 C 0.1771(2) 0.4127(2) -0.00289(9) 0.0255(5) Uani 1 1 d . . . . .
H10 H 0.1038 0.4265 -0.0137 0.031 Uiso 1 1 calc R . . . .
C11 C 0.2645(2) 0.4296(2) -0.03251(9) 0.0284(5) Uani 1 1 d . . . . .
H11 H 0.2510 0.4543 -0.0637 0.034 Uiso 1 1 calc R . . . .
C12 C 0.3725(2) 0.4103(2) -0.01666(9) 0.0298(6) Uani 1 1 d . . . . .
H12 H 0.4325 0.4221 -0.0370 0.036 Uiso 1 1 calc R . . . .
C13 C 0.3921(2) 0.3741(2) 0.02889(9) 0.0245(5) Uani 1 1 d . . . . .
H13 H 0.4656 0.3619 0.0398 0.029 Uiso 1 1 calc R . . . .
C14 C 0.33591(19) 0.15552(19) 0.10987(8) 0.0201(4) Uani 1 1 d . . . . .
C15 C 0.2789(2) 0.1064(2) 0.07237(9) 0.0265(5) Uani 1 1 d . . . . .
H15 H 0.2364 0.1504 0.0513 0.032 Uiso 1 1 calc R . . . .
C16 C 0.2837(2) -0.0062(2) 0.06565(9) 0.0301(6) Uani 1 1 d . . . . .
H16 H 0.2448 -0.0386 0.0399 0.036 Uiso 1 1 calc R . . . .
C17 C 0.3443(2) -0.0710(2) 0.09601(9) 0.0288(6) Uani 1 1 d . . . . .
H17 H 0.3482 -0.1479 0.0911 0.035 Uiso 1 1 calc R . . . .
C18 C 0.3998(2) -0.0235(2) 0.13384(9) 0.0281(5) Uani 1 1 d . . . . .
H18 H 0.4413 -0.0684 0.1549 0.034 Uiso 1 1 calc R . . . .
C19 C 0.3954(2) 0.0888(2) 0.14136(8) 0.0239(5) Uani 1 1 d . . . . .
H19 H 0.4326 0.1203 0.1678 0.029 Uiso 1 1 calc R . . . .
C20 C 0.0818(2) 0.57623(18) 0.17033(8) 0.0202(4) Uani 1 1 d . . . . .
H20A H 0.0018 0.5926 0.1686 0.024 Uiso 1 1 calc R . . . .
H20B H 0.1154 0.6260 0.1941 0.024 Uiso 1 1 calc R . . . .
C21 C 0.13055(19) 0.60255(18) 0.12324(8) 0.0188(4) Uani 1 1 d . . . . .
C22 C 0.24367(19) 0.58928(18) 0.11431(8) 0.0184(4) Uani 1 1 d . . . . .
C23 C 0.2851(2) 0.6272(2) 0.07155(8) 0.0216(5) Uani 1 1 d . . . . .
H23 H 0.3617 0.6203 0.0657 0.026 Uiso 1 1 calc R . . . .
C24 C 0.2165(2) 0.6743(2) 0.03781(9) 0.0268(5) Uani 1 1 d . . . . .
H24 H 0.2464 0.7004 0.0093 0.032 Uiso 1 1 calc R . . . .
C25 C 0.1043(2) 0.6835(2) 0.04552(9) 0.0289(5) Uani 1 1 d . . . . .
H25 H 0.0564 0.7137 0.0221 0.035 Uiso 1 1 calc R . . . .
C26 C 0.0629(2) 0.6478(2) 0.08795(9) 0.0249(5) Uani 1 1 d . . . . .
H26 H -0.0141 0.6543 0.0932 0.030 Uiso 1 1 calc R . . . .
C27 C 0.02217(18) 0.34915(19) 0.14943(8) 0.0188(4) Uani 1 1 d . . . . .
C28 C -0.0648(2) 0.3898(2) 0.12164(9) 0.0254(5) Uani 1 1 d . . . . .
H28 H -0.0845 0.4651 0.1235 0.031 Uiso 1 1 calc R . . . .
C29 C -0.1226(2) 0.3206(2) 0.09126(10) 0.0326(6) Uani 1 1 d . . . . .
H29 H -0.1814 0.3488 0.0723 0.039 Uiso 1 1 calc R . . . .
C30 C -0.0949(2) 0.2108(2) 0.08842(10) 0.0321(6) Uani 1 1 d . . . . .
H30 H -0.1345 0.1639 0.0675 0.039 Uiso 1 1 calc R . . . .
C31 C -0.0095(2) 0.1694(2) 0.11611(9) 0.0270(5) Uani 1 1 d . . . . .
H31 H 0.0090 0.0938 0.1143 0.032 Uiso 1 1 calc R . . . .
C32 C 0.0492(2) 0.2380(2) 0.14649(9) 0.0228(5) Uani 1 1 d . . . . .
H32 H 0.1079 0.2093 0.1653 0.027 Uiso 1 1 calc R . . . .
C33 C 0.0111(2) 0.42727(19) 0.24261(8) 0.0208(4) Uani 1 1 d . . . . .
C34 C 0.0421(2) 0.3566(2) 0.27907(9) 0.0247(5) Uani 1 1 d . . . . .
H34 H 0.1071 0.3134 0.2767 0.030 Uiso 1 1 calc R . . . .
C35 C -0.0218(2) 0.3493(2) 0.31878(9) 0.0312(6) Uani 1 1 d . . . . .
H35 H 0.0010 0.3026 0.3439 0.037 Uiso 1 1 calc R . . . .
C36 C -0.1180(3) 0.4087(2) 0.32238(11) 0.0374(7) Uani 1 1 d . . . . .
H36 H -0.1618 0.4022 0.3496 0.045 Uiso 1 1 calc R . . . .
C37 C -0.1504(3) 0.4777(2) 0.28629(11) 0.0396(7) Uani 1 1 d . . . . .
H37 H -0.2167 0.5188 0.2886 0.047 Uiso 1 1 calc R . . . .
C38 C -0.0860(2) 0.4872(2) 0.24654(10) 0.0317(6) Uani 1 1 d . . . . .
H38 H -0.1086 0.5350 0.2218 0.038 Uiso 1 1 calc R . . . .
C39 C 0.38929(19) 0.5329(2) 0.26845(8) 0.0203(4) Uani 1 1 d . . . . .
C40 C 0.2832(2) 0.5061(2) 0.28511(8) 0.0236(5) Uani 1 1 d . . . . .
H40 H 0.2652 0.4315 0.2906 0.028 Uiso 1 1 calc R . . . .
C41 C 0.2040(2) 0.5874(2) 0.29371(9) 0.0280(5) Uani 1 1 d . . . . .
H41 H 0.1346 0.5676 0.3062 0.034 Uiso 1 1 calc R . . . .
C42 C 0.2265(2) 0.6961(2) 0.28411(10) 0.0299(6) Uani 1 1 d . . . . .
H42 H 0.1728 0.7511 0.2896 0.036 Uiso 1 1 calc R . . . .
C43 C 0.3296(2) 0.7239(2) 0.26614(9) 0.0273(5) Uani 1 1 d . . . . .
H43 H 0.3454 0.7984 0.2593 0.033 Uiso 1 1 calc R . . . .
C44 C 0.4081(2) 0.6456(2) 0.25829(8) 0.0227(5) Uani 1 1 d . . . . .
H44 H 0.4769 0.6670 0.2457 0.027 Uiso 1 1 calc R . . . .
C45 C 0.4651(2) 0.4469(2) 0.25486(8) 0.0224(5) Uani 1 1 d . . . . .
H45A H 0.4759 0.3880 0.2784 0.027 Uiso 1 1 calc R . . . .
H45B H 0.5360 0.4731 0.2423 0.027 Uiso 1 1 calc R . . . .
O51 O 0.2606(3) -0.0049(2) -0.05088(11) 0.0832(10) Uani 1 1 d D U . . .
C51 C 0.3694(5) -0.0199(5) -0.0628(3) 0.128(3) Uani 1 1 d D U . . .
H51A H 0.4162 0.0384 -0.0487 0.154 Uiso 1 1 calc R . . . .
H51B H 0.3768 -0.0174 -0.0974 0.154 Uiso 1 1 calc R . . . .
C52 C 0.4061(4) -0.1367(5) -0.0432(2) 0.110(2) Uani 1 1 d D U . . .
H52A H 0.3650 -0.1942 -0.0600 0.164 Uiso 1 1 calc GR . . . .
H52B H 0.3905 -0.1410 -0.0096 0.164 Uiso 1 1 calc GR . . . .
H52C H 0.4854 -0.1468 -0.0478 0.164 Uiso 1 1 calc GR . . . .
C53 C 0.2109(7) 0.0927(5) -0.0656(3) 0.160(3) Uani 1 1 d D U . . .
H53A H 0.2052 0.0954 -0.1003 0.192 Uiso 1 1 calc R . . . .
H53B H 0.2547 0.1565 -0.0545 0.192 Uiso 1 1 calc R . . . .
C54 C 0.0900(6) 0.0946(6) -0.0432(3) 0.192(4) Uani 1 1 d D U . . .
H54A H 0.0349 0.1116 -0.0678 0.287 Uiso 1 1 calc GR . . . .
H54B H 0.0876 0.1507 -0.0186 0.287 Uiso 1 1 calc GR . . . .
H54C H 0.0739 0.0227 -0.0296 0.287 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
Zr Cl 2.5045(6) . ?
Zr P1 2.6361(6) . ?
Zr P2 2.7888(6) . ?
Zr N 2.0947(19) . ?
Zr C1 2.351(2) . ?
Zr C2 2.649(2) . ?
Zr C3 2.598(2) . ?
Zr C39 2.585(2) . ?
Zr C40 2.795(2) . ?
Zr C45 2.333(2) . ?
P1 C1 1.791(2) . ?
P1 C8 1.825(2) . ?
P1 C14 1.821(2) . ?
P2 C20 1.836(2) . ?
P2 C27 1.824(2) . ?
P2 C33 1.835(2) . ?
N C3 1.434(3) . ?
N C22 1.404(3) . ?
C1 H1 0.99(3) . ?
C1 C2 1.460(3) . ?
C2 C3 1.421(3) . ?
C2 C7 1.424(3) . ?
C3 C4 1.404(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.378(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.401(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.370(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.399(3) . ?
C8 C13 1.391(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.387(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.382(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.396(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.387(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.396(3) . ?
C14 C19 1.400(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.388(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.374(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.386(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.388(3) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.510(3) . ?
C21 C22 1.408(3) . ?
C21 C26 1.398(3) . ?
C22 C23 1.404(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.383(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.386(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.388(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.397(3) . ?
C27 C32 1.397(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.389(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.384(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.384(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.390(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.396(3) . ?
C33 C38 1.391(4) . ?
C34 H34 0.9500 . ?
C34 C35 1.386(4) . ?
C35 H35 0.9500 . ?
C35 C36 1.378(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.380(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.392(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.417(3) . ?
C39 C44 1.424(3) . ?
C39 C45 1.452(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.405(4) . ?
C41 H41 0.9500 . ?
C41 C42 1.381(4) . ?
C42 H42 0.9500 . ?
C42 C43 1.401(4) . ?
C43 H43 0.9500 . ?
C43 C44 1.369(4) . ?
C44 H44 0.9500 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
O51 C51 1.380(5) . ?
O51 C53 1.395(5) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 C52 1.591(7) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.608(8) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 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
Cl Zr P1 86.521(19) . . ?
Cl Zr P2 84.309(19) . . ?
Cl Zr C2 127.15(5) . . ?
Cl Zr C3 158.36(6) . . ?
Cl Zr C39 102.63(6) . . ?
Cl Zr C40 85.67(5) . . ?
P1 Zr P2 89.594(19) . . ?
P1 Zr C2 66.13(5) . . ?
P1 Zr C40 166.90(5) . . ?
P2 Zr C40 79.17(5) . . ?
N Zr Cl 155.65(5) . . ?
N Zr P1 76.30(5) . . ?
N Zr P2 78.53(5) . . ?
N Zr C1 81.35(8) . . ?
N Zr C2 60.86(7) . . ?
N Zr C3 33.46(7) . . ?
N Zr C39 98.56(7) . . ?
N Zr C40 107.62(7) . . ?
N Zr C45 113.82(8) . . ?
C1 Zr Cl 97.25(6) . . ?
C1 Zr P1 41.59(6) . . ?
C1 Zr P2 130.52(6) . . ?
C1 Zr C2 33.27(8) . . ?
C1 Zr C3 61.45(8) . . ?
C1 Zr C39 121.92(8) . . ?
C1 Zr C40 150.28(8) . . ?
C2 Zr P2 136.01(5) . . ?
C2 Zr C40 126.86(7) . . ?
C3 Zr P1 79.61(5) . . ?
C3 Zr P2 111.90(5) . . ?
C3 Zr C2 31.41(7) . . ?
C3 Zr C40 110.74(7) . . ?
C39 Zr P1 162.86(6) . . ?
C39 Zr P2 105.57(5) . . ?
C39 Zr C2 96.98(7) . . ?
C39 Zr C3 87.19(7) . . ?
C39 Zr C40 30.23(7) . . ?
C45 Zr Cl 90.52(7) . . ?
C45 Zr P1 133.40(6) . . ?
C45 Zr P2 136.38(6) . . ?
C45 Zr C1 93.10(8) . . ?
C45 Zr C2 79.46(8) . . ?
C45 Zr C3 87.12(8) . . ?
C45 Zr C39 33.85(8) . . ?
C45 Zr C40 57.23(8) . . ?
C1 P1 Zr 60.66(8) . . ?
C1 P1 C8 112.97(11) . . ?
C1 P1 C14 105.50(11) . . ?
C8 P1 Zr 128.78(8) . . ?
C14 P1 Zr 127.57(8) . . ?
C14 P1 C8 103.54(10) . . ?
C20 P2 Zr 103.02(8) . . ?
C27 P2 Zr 119.09(8) . . ?
C27 P2 C20 105.89(11) . . ?
C27 P2 C33 101.10(11) . . ?
C33 P2 Zr 122.11(8) . . ?
C33 P2 C20 103.77(11) . . ?
C3 N Zr 92.91(13) . . ?
C22 N Zr 147.60(15) . . ?
C22 N C3 118.55(19) . . ?
Zr C1 H1 130.7(16) . . ?
P1 C1 Zr 77.75(9) . . ?
P1 C1 H1 116.0(16) . . ?
C2 C1 Zr 84.63(14) . . ?
C2 C1 P1 124.74(17) . . ?
C2 C1 H1 115.2(16) . . ?
C1 C2 Zr 62.10(12) . . ?
C3 C2 Zr 72.31(13) . . ?
C3 C2 C1 123.5(2) . . ?
C3 C2 C7 116.2(2) . . ?
C7 C2 Zr 137.82(16) . . ?
C7 C2 C1 119.8(2) . . ?
N C3 Zr 53.63(10) . . ?
C2 C3 Zr 76.28(13) . . ?
C2 C3 N 118.2(2) . . ?
C4 C3 Zr 138.68(17) . . ?
C4 C3 N 120.9(2) . . ?
C4 C3 C2 120.6(2) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 C3 121.3(2) . . ?
C5 C4 H4 119.3 . . ?
C4 C5 H5 120.6 . . ?
C4 C5 C6 118.8(2) . . ?
C6 C5 H5 120.6 . . ?
C5 C6 H6 119.6 . . ?
C7 C6 C5 120.8(2) . . ?
C7 C6 H6 119.6 . . ?
C2 C7 H7 118.9 . . ?
C6 C7 C2 122.1(2) . . ?
C6 C7 H7 118.9 . . ?
C9 C8 P1 118.61(18) . . ?
C13 C8 P1 121.69(18) . . ?
C13 C8 C9 119.7(2) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 119.9(2) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.2(2) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.1(2) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 C11 119.9(2) . . ?
C13 C12 H12 120.0 . . ?
C8 C13 H13 119.9 . . ?
C12 C13 C8 120.1(2) . . ?
C12 C13 H13 119.9 . . ?
C15 C14 P1 119.26(18) . . ?
C15 C14 C19 118.8(2) . . ?
C19 C14 P1 121.87(18) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.6(2) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.4(2) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 120.2 . . ?
C16 C17 C18 119.6(2) . . ?
C18 C17 H17 120.2 . . ?
C17 C18 H18 119.5 . . ?
C17 C18 C19 120.9(2) . . ?
C19 C18 H18 119.5 . . ?
C14 C19 H19 120.2 . . ?
C18 C19 C14 119.7(2) . . ?
C18 C19 H19 120.2 . . ?
P2 C20 H20A 108.2 . . ?
P2 C20 H20B 108.2 . . ?
H20A C20 H20B 107.4 . . ?
C21 C20 P2 116.15(16) . . ?
C21 C20 H20A 108.2 . . ?
C21 C20 H20B 108.2 . . ?
C22 C21 C20 122.3(2) . . ?
C26 C21 C20 119.2(2) . . ?
C26 C21 C22 118.3(2) . . ?
N C22 C21 119.9(2) . . ?
N C22 C23 121.1(2) . . ?
C23 C22 C21 118.9(2) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 C22 121.3(2) . . ?
C24 C23 H23 119.3 . . ?
C23 C24 H24 120.0 . . ?
C23 C24 C25 120.1(2) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 120.5 . . ?
C24 C25 C26 119.0(2) . . ?
C26 C25 H25 120.5 . . ?
C21 C26 H26 118.9 . . ?
C25 C26 C21 122.2(2) . . ?
C25 C26 H26 118.9 . . ?
C28 C27 P2 122.47(18) . . ?
C28 C27 C32 119.1(2) . . ?
C32 C27 P2 118.44(18) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 C27 120.2(2) . . ?
C29 C28 H28 119.9 . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.4(2) . . ?
C30 C29 H29 119.8 . . ?
C29 C30 H30 120.0 . . ?
C29 C30 C31 120.0(2) . . ?
C31 C30 H30 120.0 . . ?
C30 C31 H31 119.9 . . ?
C30 C31 C32 120.1(2) . . ?
C32 C31 H31 119.9 . . ?
C27 C32 H32 119.9 . . ?
C31 C32 C27 120.3(2) . . ?
C31 C32 H32 119.9 . . ?
C34 C33 P2 118.23(19) . . ?
C38 C33 P2 123.04(19) . . ?
C38 C33 C34 118.7(2) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 C33 120.0(2) . . ?
C35 C34 H34 120.0 . . ?
C34 C35 H35 119.5 . . ?
C36 C35 C34 120.9(3) . . ?
C36 C35 H35 119.5 . . ?
C35 C36 H36 120.2 . . ?
C35 C36 C37 119.6(3) . . ?
C37 C36 H36 120.2 . . ?
C36 C37 H37 120.0 . . ?
C36 C37 C38 120.0(3) . . ?
C38 C37 H37 120.0 . . ?
C33 C38 C37 120.7(3) . . ?
C33 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C40 C39 Zr 83.09(14) . . ?
C40 C39 C44 116.1(2) . . ?
C40 C39 C45 120.3(2) . . ?
C44 C39 Zr 115.98(15) . . ?
C44 C39 C45 122.6(2) . . ?
C45 C39 Zr 63.52(12) . . ?
Zr C40 H40 78.5 . . ?
C39 C40 Zr 66.68(12) . . ?
C39 C40 H40 119.3 . . ?
C41 C40 Zr 126.17(18) . . ?
C41 C40 C39 121.5(2) . . ?
C41 C40 H40 119.3 . . ?
C40 C41 H41 119.8 . . ?
C42 C41 C40 120.3(2) . . ?
C42 C41 H41 119.8 . . ?
C41 C42 H42 120.5 . . ?
C41 C42 C43 119.0(2) . . ?
C43 C42 H42 120.5 . . ?
C42 C43 H43 119.4 . . ?
C44 C43 C42 121.2(2) . . ?
C44 C43 H43 119.4 . . ?
C39 C44 H44 119.1 . . ?
C43 C44 C39 121.7(2) . . ?
C43 C44 H44 119.1 . . ?
Zr C45 H45A 114.9 . . ?
Zr C45 H45B 114.9 . . ?
C39 C45 Zr 82.64(13) . . ?
C39 C45 H45A 114.9 . . ?
C39 C45 H45B 114.9 . . ?
H45A C45 H45B 111.9 . . ?
C51 O51 C53 116.6(6) . . ?
O51 C51 H51A 110.3 . . ?
O51 C51 H51B 110.3 . . ?
O51 C51 C52 107.1(4) . . ?
H51A C51 H51B 108.5 . . ?
C52 C51 H51A 110.3 . . ?
C52 C51 H51B 110.3 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O51 C53 H53A 110.4 . . ?
O51 C53 H53B 110.4 . . ?
O51 C53 C54 106.5(6) . . ?
H53A C53 H53B 108.6 . . ?
C54 C53 H53A 110.4 . . ?
C54 C53 H53B 110.4 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 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 P1 C1 C2 -74.52(19) . . . . ?
Zr P1 C8 C9 -80.5(2) . . . . ?
Zr P1 C8 C13 100.2(2) . . . . ?
Zr P1 C14 C15 146.51(17) . . . . ?
Zr P1 C14 C19 -30.5(2) . . . . ?
Zr P2 C20 C21 61.30(18) . . . . ?
Zr P2 C27 C28 -138.57(18) . . . . ?
Zr P2 C27 C32 43.5(2) . . . . ?
Zr P2 C33 C34 -34.0(2) . . . . ?
Zr P2 C33 C38 147.27(19) . . . . ?
Zr N C3 C2 43.2(2) . . . . ?
Zr N C3 C4 -130.2(2) . . . . ?
Zr N C22 C21 33.5(4) . . . . ?
Zr N C22 C23 -144.0(2) . . . . ?
Zr C1 C2 C3 -40.3(2) . . . . ?
Zr C1 C2 C7 131.5(2) . . . . ?
Zr C2 C3 N -34.60(17) . . . . ?
Zr C2 C3 C4 138.9(2) . . . . ?
Zr C2 C7 C6 -95.7(3) . . . . ?
Zr C3 C4 C5 103.9(3) . . . . ?
Zr C39 C40 C41 -119.3(2) . . . . ?
Zr C39 C44 C43 97.9(2) . . . . ?
Zr C40 C41 C42 -79.9(3) . . . . ?
P1 C1 C2 Zr 71.07(16) . . . . ?
P1 C1 C2 C3 30.8(3) . . . . ?
P1 C1 C2 C7 -157.40(19) . . . . ?
P1 C8 C9 C10 -178.33(18) . . . . ?
P1 C8 C13 C12 177.9(2) . . . . ?
P1 C14 C15 C16 -178.9(2) . . . . ?
P1 C14 C19 C18 179.2(2) . . . . ?
P2 C20 C21 C22 -58.8(3) . . . . ?
P2 C20 C21 C26 125.1(2) . . . . ?
P2 C27 C28 C29 -178.5(2) . . . . ?
P2 C27 C32 C31 178.30(19) . . . . ?
P2 C33 C34 C35 179.47(19) . . . . ?
P2 C33 C38 C37 179.4(2) . . . . ?
N C3 C4 C5 172.5(2) . . . . ?
N C22 C23 C24 175.8(2) . . . . ?
C1 P1 C8 C9 -150.45(18) . . . . ?
C1 P1 C8 C13 30.2(2) . . . . ?
C1 P1 C14 C15 -148.8(2) . . . . ?
C1 P1 C14 C19 34.2(2) . . . . ?
C1 C2 C3 Zr 36.9(2) . . . . ?
C1 C2 C3 N 2.3(3) . . . . ?
C1 C2 C3 C4 175.8(2) . . . . ?
C1 C2 C7 C6 -175.9(2) . . . . ?
C2 C3 C4 C5 -0.9(4) . . . . ?
C3 N C22 C21 -161.6(2) . . . . ?
C3 N C22 C23 20.9(3) . . . . ?
C3 C2 C7 C6 -3.5(3) . . . . ?
C3 C4 C5 C6 -2.4(4) . . . . ?
C4 C5 C6 C7 2.6(4) . . . . ?
C5 C6 C7 C2 0.4(4) . . . . ?
C7 C2 C3 Zr -135.2(2) . . . . ?
C7 C2 C3 N -169.8(2) . . . . ?
C7 C2 C3 C4 3.7(3) . . . . ?
C8 P1 C1 Zr 122.83(9) . . . . ?
C8 P1 C1 C2 48.3(2) . . . . ?
C8 P1 C14 C15 -29.9(2) . . . . ?
C8 P1 C14 C19 153.1(2) . . . . ?
C8 C9 C10 C11 -0.1(4) . . . . ?
C9 C8 C13 C12 -1.5(4) . . . . ?
C9 C10 C11 C12 -0.5(4) . . . . ?
C10 C11 C12 C13 0.1(4) . . . . ?
C11 C12 C13 C8 0.9(4) . . . . ?
C13 C8 C9 C10 1.0(4) . . . . ?
C14 P1 C1 Zr -124.75(9) . . . . ?
C14 P1 C1 C2 160.74(19) . . . . ?
C14 P1 C8 C9 95.9(2) . . . . ?
C14 P1 C8 C13 -83.4(2) . . . . ?
C14 C15 C16 C17 0.3(4) . . . . ?
C15 C14 C19 C18 2.3(4) . . . . ?
C15 C16 C17 C18 0.8(4) . . . . ?
C16 C17 C18 C19 -0.4(4) . . . . ?
C17 C18 C19 C14 -1.2(4) . . . . ?
C19 C14 C15 C16 -1.8(4) . . . . ?
C20 P2 C27 C28 -23.3(2) . . . . ?
C20 P2 C27 C32 158.77(19) . . . . ?
C20 P2 C33 C34 -149.30(19) . . . . ?
C20 P2 C33 C38 32.0(2) . . . . ?
C20 C21 C22 N 9.6(3) . . . . ?
C20 C21 C22 C23 -172.8(2) . . . . ?
C20 C21 C26 C25 173.8(2) . . . . ?
C21 C22 C23 C24 -1.8(3) . . . . ?
C22 N C3 Zr -172.0(2) . . . . ?
C22 N C3 C2 -128.7(2) . . . . ?
C22 N C3 C4 57.8(3) . . . . ?
C22 C21 C26 C25 -2.5(4) . . . . ?
C22 C23 C24 C25 -0.9(4) . . . . ?
C23 C24 C25 C26 1.9(4) . . . . ?
C24 C25 C26 C21 -0.1(4) . . . . ?
C26 C21 C22 N -174.2(2) . . . . ?
C26 C21 C22 C23 3.4(3) . . . . ?
C27 P2 C20 C21 -64.48(19) . . . . ?
C27 P2 C33 C34 101.1(2) . . . . ?
C27 P2 C33 C38 -77.7(2) . . . . ?
C27 C28 C29 C30 0.3(4) . . . . ?
C28 C27 C32 C31 0.3(4) . . . . ?
C28 C29 C30 C31 0.3(4) . . . . ?
C29 C30 C31 C32 -0.6(4) . . . . ?
C30 C31 C32 C27 0.3(4) . . . . ?
C32 C27 C28 C29 -0.6(4) . . . . ?
C33 P2 C20 C21 -170.50(17) . . . . ?
C33 P2 C27 C28 84.6(2) . . . . ?
C33 P2 C27 C32 -93.3(2) . . . . ?
C33 C34 C35 C36 1.9(4) . . . . ?
C34 C33 C38 C37 0.7(4) . . . . ?
C34 C35 C36 C37 -1.0(4) . . . . ?
C35 C36 C37 C38 -0.1(5) . . . . ?
C36 C37 C38 C33 0.2(5) . . . . ?
C38 C33 C34 C35 -1.7(4) . . . . ?
C39 C40 C41 C42 2.8(4) . . . . ?
C40 C39 C44 C43 2.7(3) . . . . ?
C40 C39 C45 Zr 63.4(2) . . . . ?
C40 C41 C42 C43 -0.6(4) . . . . ?
C41 C42 C43 C44 -0.4(4) . . . . ?
C42 C43 C44 C39 -0.7(4) . . . . ?
C44 C39 C40 Zr 115.6(2) . . . . ?
C44 C39 C40 C41 -3.7(3) . . . . ?
C44 C39 C45 Zr -105.2(2) . . . . ?
C45 C39 C40 Zr -53.75(18) . . . . ?
C45 C39 C40 C41 -173.1(2) . . . . ?
C45 C39 C44 C43 171.8(2) . . . . ?
C51 O51 C53 C54 -174.8(6) . . . . ?
C53 O51 C51 C52 -179.0(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.146
_oxdiff_exptl_absorpt_empirical_full_min 0.901
_cell_oxdiff_length_a            12.1122(2)
_cell_oxdiff_length_b            12.2008(2)
_cell_oxdiff_length_c            28.4853(5)
_cell_oxdiff_angle_alpha         90.0316(15)
_cell_oxdiff_angle_beta          91.1040(15)
_cell_oxdiff_angle_gamma         90.0684(15)
_cell_oxdiff_volume              4208.73(13)
_cell_oxdiff_measurement_reflns_used 20092
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ba_ms34_sq
_database_code_depnum_ccdc_archive 'CCDC 1530475'
_audit_update_record             
;
2017-03-17 deposited with the CCDC.
2017-04-05 downloaded from the CCDC.
;
_audit_creation_date             2017-01-30

_audit_block_code                ba_ms34
_audit_block_refno               2438

_audit_creation_method           
;
Olex2 1.2
(compiled Mar  2 2017 14:00:58 for OlexSys, GUI svn.r5324)
;

# start Validation Reply Form
_vrf_CHEMW03_ba_ms34_sq          
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
RESPONSE: see _platon_squeeze_
;
_vrf_PLAT910_ba_ms34_sq          
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          24 Note
RESPONSE: limited by diffractometer
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C62 H69 B N P2 Zr'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         992.15
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            'dark yellow'
_diffrn_ambient_temperature      120(1)
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   17.3823(5)
_cell_length_b                   17.7265(5)
_cell_length_c                   21.7567(5)
_cell_angle_alpha                67.552(2)
_cell_angle_beta                 66.932(2)
_cell_angle_gamma                66.047(3)
_cell_volume                     5435.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    36614
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      30.4910
_cell_measurement_theta_min      3.0150
_shelx_estimated_absorpt_T_max   0.971
_shelx_estimated_absorpt_T_min   0.971
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2092
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
14 -8 -12 0.0926
-20 -18 -3 0.0456
-10 0 -28 0.0740
10 -17 -6 0.0899
9 5 30 0.0932
5 -10 -24 0.1044
-14 13 -3 0.1205
2 10 29 0.0640
20 20 6 0.0094
-7 -25 -8 0.0832
-1 22 5 0.1066
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.068
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
14.0185 -7.9868 -12.0022 0.3247 0.8739 0.3184
-20.0113 -18.0139 -2.9988 -0.9873 -0.0768 -0.0510
-10.0069 -0.0073 -27.9989 0.0415 -0.2215 0.9776
10.0180 -16.9891 -6.0023 -0.0871 1.0182 0.0271
9.0035 5.0057 29.9993 0.0358 -0.0071 -0.9960
5.0118 -9.9936 -24.0012 0.1591 0.6760 0.7231
-14.0192 12.9866 -2.9975 -0.0242 -0.9741 0.2485
1.9945 9.9992 29.0004 -0.0205 -0.4427 -0.9038
20.0101 20.0135 5.9990 1.0042 -0.0116 -0.0327
-6.9950 -25.0019 -8.0008 -0.7454 0.6862 0.0370
-1.0112 21.9958 5.0015 0.4789 -0.8591 0.0463

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            243662
_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         30.577
_diffrn_reflns_theta_min         2.595
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00   5.00   0.50   20.00    --   26.43 -79.00 -31.30   98
  2  ω     31.00  58.00   0.50   20.00    --   26.43 -79.00 -31.30   54
  3  ω      0.00  27.00   0.50   20.00    --   26.43 -79.00  45.44   54
  4  ω     33.00  58.00   0.50   20.00    --   26.43 -79.00  45.44   50
  5  ω    -38.00  58.00   0.50   20.00    --   26.43 -80.00  28.84  192
  6  ω    -44.00  58.00   0.50   20.00    --   26.43 -79.00 122.51  204
  7  ω     31.00  58.00   0.50   20.00    --   26.43 -80.00  76.22   54
  8  ω     -4.00  56.00   0.50   20.00    --   26.43  77.00  30.00  120
  9  ω     -4.00  54.00   0.50   20.00    --   26.43  77.00 -90.00  116
 10  ω     -4.00  32.00   0.50   20.00    --   26.43  77.00 150.00   72
 11  ω     69.00  95.00   0.50   20.00    --   26.43  77.00 150.00   52
 12  ω     14.00  95.00   0.50   20.00    --   26.43  57.00 -30.00  162
 13  ω     15.00  42.00   0.50   20.00    --   26.43  57.00  90.00   54
 14  ω     67.00  95.00   0.50   20.00    --   26.43  57.00-120.00   56
 15  ω     30.00  56.00   0.50   20.00    --   26.43 -77.00 -90.00   52
 16  ω      2.00  37.00   0.50   20.00    --   26.43  38.00 -30.00   70
 17  ω      7.00  58.00   0.50   20.00    --   26.43  77.00-180.00  102
 18  ω     70.00  97.00   0.50   20.00    --   26.43  77.00-180.00   54
 19  ω      2.00  99.00   0.50   20.00    --   26.43  38.00 120.00  194
 20  ω    -28.00  55.00   0.50   20.00    --   26.43 -77.00-120.00  166
 21  ω     24.00  56.00   0.50   20.00    --   26.43 -77.00 -60.00   64
 22  ω     60.00  86.00   0.50   20.00    --   26.43  77.00   0.00   52
 23  ω    -44.00  58.00   0.50   20.00    --   26.43 -80.00-162.10  204
 24  ω      1.00  99.00   0.50   20.00    --   26.43  38.00   0.00  196
 25  ω      5.00  95.00   0.50   20.00    --   26.43  57.00 120.00  180
 26  ω      1.00  99.00   0.50   20.00    --   26.43  38.00-120.00  196
 27  ω    -42.00  47.00   0.50   20.00    --   26.43 -57.00  90.00  178
 28  ω    -42.00  47.00   0.50   20.00    --   26.43 -57.00   0.00  178
 29  ω    -44.00  58.00   0.50   20.00    --   26.43 -80.00-162.10  204
 30  ω    -42.00 -17.00   0.50   20.00    --   26.43 -57.00 -90.00   50
 31  ω    -42.00  47.00   0.50   20.00    --   26.43 -57.00-150.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'Agilent Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0279539000
_diffrn_orient_matrix_UB_12      0.0256663000
_diffrn_orient_matrix_UB_13      -0.0114792000
_diffrn_orient_matrix_UB_21      0.0371615000
_diffrn_orient_matrix_UB_22      -0.0361274000
_diffrn_orient_matrix_UB_23      -0.0053629000
_diffrn_orient_matrix_UB_31      -0.0011867000
_diffrn_orient_matrix_UB_32      0.0098920000
_diffrn_orient_matrix_UB_33      -0.0344948000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent Agilent SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                23925
_reflns_number_total             33234
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 Structure factors included contributions from the .fab file,
 see _platon_squeeze_.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2016/6
_computing_structure_solution    'SIR2014 (Giacovazzo et al., 2014)'
_refine_diff_density_max         1.394
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1035
_refine_ls_number_reflns         33234
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0506
_refine_ls_restrained_S_all      1.040
_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)+(0.0580P)²+0.1560P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1247
_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
 C101, C102, C103, C104, C105, C106, C201, C202, C203, C204, C205
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C26(H26), C76(H76)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C57(H57A,H57B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23),
  C24(H24), C25(H25), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C53(H53), C54(H54), C55(H55),
  C56(H56), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65),
 C66(H66), C67(H67), C68(H68), C69(H69), C72(H72), C73(H73), C74(H74), C75(H75),
  C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C84(H84), C85(H85),
 C86(H86), C87(H87), C88(H88), C101(H101), C102(H102), C103(H103), C104(H104),
 C105(H105), C106(H106), C201(H201), C202(H202), C203(H203), C204(H204),
 C205(H205), C206(H206)
3.d Fitted hexagon refined as free rotating group:
 C101(C102,C103,C104,C105,C106), C201(C202,C203,C204,C205,C206)
3.e Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C90(H90A,H90B,
 H90C), C92(H92A,H92B,H92C), C94(H94A,H94B,H94C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Zr1 Zr 0.46549(2) 0.17451(2) 0.20588(2) 0.01956(5) Uani 1 1 d . . . . .
H H 0.5713(15) 0.0886(15) 0.2032(12) 0.043(7) Uiso 1 1 d . . . . .
H1 H 0.4080(14) 0.2964(14) 0.1481(11) 0.032(6) Uiso 1 1 d . . . . .
P1 P 0.48851(3) 0.10283(3) 0.10707(3) 0.02136(10) Uani 1 1 d . . . . .
P2 P 0.49073(3) 0.08283(3) 0.33087(3) 0.02170(11) Uani 1 1 d . . . . .
N1 N 0.36987(11) 0.12213(11) 0.23923(8) 0.0220(3) Uani 1 1 d . . . . .
C1 C 0.46397(13) 0.00089(13) 0.15173(10) 0.0225(4) Uani 1 1 d . . . . .
C2 C 0.38790(13) -0.00429(13) 0.20785(10) 0.0242(4) Uani 1 1 d . . . . .
C3 C 0.37141(15) -0.08276(14) 0.24024(11) 0.0299(5) Uani 1 1 d . . . . .
H3 H 0.320292 -0.086536 0.277963 0.036 Uiso 1 1 calc R . . . .
C4 C 0.42802(16) -0.15599(14) 0.21873(11) 0.0324(5) Uani 1 1 d . . . . .
H4 H 0.415633 -0.209087 0.241474 0.039 Uiso 1 1 calc R . . . .
C5 C 0.50252(15) -0.15052(14) 0.16384(11) 0.0308(5) Uani 1 1 d . . . . .
H5 H 0.541565 -0.200081 0.148708 0.037 Uiso 1 1 calc R . . . .
C6 C 0.52029(14) -0.07306(13) 0.13093(10) 0.0269(4) Uani 1 1 d . . . . .
H6 H 0.571820 -0.070182 0.093459 0.032 Uiso 1 1 calc R . . . .
C7 C 0.32440(13) 0.07186(14) 0.23507(11) 0.0268(4) Uani 1 1 d . . . . .
H7A H 0.286222 0.108517 0.204184 0.032 Uiso 1 1 calc R . . . .
H7B H 0.286588 0.051675 0.281688 0.032 Uiso 1 1 calc R . . . .
C8 C 0.41260(13) 0.16041(13) 0.05327(10) 0.0222(4) Uani 1 1 d . . . . .
C9 C 0.36059(13) 0.12161(14) 0.04762(10) 0.0258(4) Uani 1 1 d . . . . .
H9 H 0.362073 0.064331 0.073555 0.031 Uiso 1 1 calc R . . . .
C10 C 0.30665(14) 0.16755(14) 0.00372(11) 0.0288(5) Uani 1 1 d . . . . .
H10 H 0.271043 0.141437 0.000084 0.035 Uiso 1 1 calc R . . . .
C11 C 0.30445(14) 0.25038(15) -0.03444(11) 0.0303(5) Uani 1 1 d . . . . .
H11 H 0.268245 0.280763 -0.064839 0.036 Uiso 1 1 calc R . . . .
C12 C 0.35495(14) 0.28945(14) -0.02853(11) 0.0301(5) Uani 1 1 d . . . . .
H12 H 0.353048 0.346775 -0.054575 0.036 Uiso 1 1 calc R . . . .
C13 C 0.40858(14) 0.24463(14) 0.01565(10) 0.0278(4) Uani 1 1 d . . . . .
H13 H 0.442592 0.271824 0.020064 0.033 Uiso 1 1 calc R . . . .
C14 C 0.59522(13) 0.07671(13) 0.04307(10) 0.0235(4) Uani 1 1 d . . . . .
C15 C 0.60336(14) 0.09047(14) -0.02617(10) 0.0281(4) Uani 1 1 d . . . . .
H15 H 0.552395 0.113993 -0.041812 0.034 Uiso 1 1 calc R . . . .
C16 C 0.68627(15) 0.06982(15) -0.07288(11) 0.0335(5) Uani 1 1 d . . . . .
H16 H 0.691462 0.079543 -0.120212 0.040 Uiso 1 1 calc R . . . .
C17 C 0.76089(15) 0.03526(15) -0.05051(12) 0.0350(5) Uani 1 1 d . . . . .
H17 H 0.817197 0.021001 -0.082300 0.042 Uiso 1 1 calc R . . . .
C18 C 0.75297(15) 0.02154(16) 0.01877(12) 0.0358(5) Uani 1 1 d . . . . .
H18 H 0.803925 -0.001971 0.034424 0.043 Uiso 1 1 calc R . . . .
C19 C 0.67075(14) 0.04218(14) 0.06485(11) 0.0310(5) Uani 1 1 d . . . . .
H19 H 0.665775 0.032634 0.112106 0.037 Uiso 1 1 calc R . . . .
C20 C 0.38235(13) 0.08273(13) 0.38931(10) 0.0228(4) Uani 1 1 d . . . . .
C21 C 0.31252(13) 0.13599(12) 0.36037(10) 0.0219(4) Uani 1 1 d . . . . .
C22 C 0.22738(13) 0.14609(14) 0.40461(11) 0.0281(4) Uani 1 1 d . . . . .
H22 H 0.179121 0.183577 0.386716 0.034 Uiso 1 1 calc R . . . .
C23 C 0.21213(15) 0.10228(15) 0.47426(11) 0.0331(5) Uani 1 1 d . . . . .
H23 H 0.153715 0.110710 0.503603 0.040 Uiso 1 1 calc R . . . .
C24 C 0.28145(15) 0.04619(15) 0.50150(11) 0.0331(5) Uani 1 1 d . . . . .
H24 H 0.270606 0.014836 0.548883 0.040 Uiso 1 1 calc R . . . .
C25 C 0.36649(14) 0.03646(14) 0.45889(10) 0.0283(4) Uani 1 1 d . . . . .
H25 H 0.414284 -0.001878 0.477078 0.034 Uiso 1 1 calc R . . . .
C26 C 0.32964(13) 0.17833(12) 0.28460(10) 0.0216(4) Uani 1 1 d . . . . .
H26 H 0.280881 0.229963 0.271284 0.026 Uiso 1 1 calc R . . . .
C27 C 0.55601(13) -0.02966(13) 0.34351(10) 0.0241(4) Uani 1 1 d . . . . .
C28 C 0.61556(15) -0.06806(15) 0.38226(11) 0.0333(5) Uani 1 1 d . . . . .
H28 H 0.622109 -0.035937 0.405254 0.040 Uiso 1 1 calc R . . . .
C29 C 0.66578(17) -0.15322(17) 0.38771(13) 0.0434(6) Uani 1 1 d . . . . .
H29 H 0.707020 -0.178645 0.413865 0.052 Uiso 1 1 calc R . . . .
C30 C 0.65633(17) -0.20098(15) 0.35562(12) 0.0399(6) Uani 1 1 d . . . . .
H30 H 0.690828 -0.259204 0.359501 0.048 Uiso 1 1 calc R . . . .
C31 C 0.59669(16) -0.16396(15) 0.31793(13) 0.0383(6) Uani 1 1 d . . . . .
H31 H 0.589466 -0.196954 0.296074 0.046 Uiso 1 1 calc R . . . .
C32 C 0.54701(15) -0.07903(14) 0.31148(12) 0.0323(5) Uani 1 1 d . . . . .
H32 H 0.506278 -0.054066 0.284907 0.039 Uiso 1 1 calc R . . . .
C33 C 0.53628(14) 0.12793(13) 0.36634(11) 0.0271(4) Uani 1 1 d . . . . .
C34 C 0.61809(18) 0.13932(18) 0.32825(13) 0.0452(6) Uani 1 1 d . . . . .
H34 H 0.648373 0.121463 0.286769 0.054 Uiso 1 1 calc R . . . .
C35 C 0.6565(2) 0.1766(2) 0.34999(15) 0.0568(8) Uani 1 1 d . . . . .
H35 H 0.712591 0.183731 0.323769 0.068 Uiso 1 1 calc R . . . .
C36 C 0.6118(2) 0.20286(18) 0.41004(15) 0.0531(8) Uani 1 1 d . . . . .
H36 H 0.637466 0.228303 0.425195 0.064 Uiso 1 1 calc R . . . .
C37 C 0.53078(19) 0.19259(15) 0.44808(14) 0.0435(6) Uani 1 1 d . . . . .
H37 H 0.500585 0.210870 0.489371 0.052 Uiso 1 1 calc R . . . .
C38 C 0.49282(16) 0.15547(14) 0.42625(12) 0.0328(5) Uani 1 1 d . . . . .
H38 H 0.436509 0.148895 0.452648 0.039 Uiso 1 1 calc R . . . .
C39 C 0.45649(14) 0.31612(14) 0.22427(11) 0.0258(4) Uani 1 1 d . . . . .
H39A H 0.4744(15) 0.2530(15) 0.2603(12) 0.036(6) Uiso 1 1 d . . . . .
H39B H 0.5056(15) 0.3347(15) 0.2174(12) 0.035(6) Uiso 1 1 d . . . . .
C40 C 0.37069(15) 0.36838(15) 0.26529(11) 0.0324(5) Uani 1 1 d . . . . .
H40A H 0.321919 0.350722 0.269329 0.049 Uiso 1 1 calc GR . . . .
H40B H 0.360728 0.429366 0.241134 0.049 Uiso 1 1 calc GR . . . .
H40C H 0.374528 0.358482 0.311640 0.049 Uiso 1 1 calc GR . . . .
C41 C 0.56082(14) 0.27220(14) 0.10309(11) 0.0252(4) Uani 1 1 d . . . . .
H41A H 0.5815(17) 0.2100(18) 0.1186(13) 0.051(8) Uiso 1 1 d . . . . .
H41B H 0.5629(15) 0.2852(15) 0.0511(12) 0.034(6) Uiso 1 1 d . . . . .
C42 C 0.63463(15) 0.29857(16) 0.10331(12) 0.0345(5) Uani 1 1 d . . . . .
H42A H 0.641134 0.277741 0.150247 0.052 Uiso 1 1 calc GR . . . .
H42B H 0.620132 0.361112 0.088278 0.052 Uiso 1 1 calc GR . . . .
H42C H 0.689731 0.273683 0.071559 0.052 Uiso 1 1 calc GR . . . .
C43 C 0.42868(16) 0.42390(14) 0.10291(11) 0.0298(5) Uani 1 1 d . . . . .
H43A H 0.3724(16) 0.4525(15) 0.1299(12) 0.036 Uiso 1 1 d R . . . .
H43B H 0.4713(15) 0.4555(15) 0.1003(12) 0.036 Uiso 1 1 d R . . . .
C44 C 0.42227(17) 0.44095(15) 0.03014(11) 0.0381(6) Uani 1 1 d . . . . .
H44A H 0.479534 0.414274 0.001451 0.057 Uiso 1 1 calc GR . . . .
H44B H 0.404387 0.502808 0.009057 0.057 Uiso 1 1 calc GR . . . .
H44C H 0.378777 0.416636 0.033454 0.057 Uiso 1 1 calc GR . . . .
B1 B 0.46191(16) 0.32525(15) 0.14353(11) 0.0241(5) Uani 1 1 d . . . . .
Zr51 Zr 0.82293(2) 0.54230(2) 0.29186(2) 0.02026(5) Uani 1 1 d . . . . .
HA H 0.9076(15) 0.4395(14) 0.2939(11) 0.036(6) Uiso 1 1 d . . . . .
H51 H 0.7012(15) 0.5984(14) 0.3493(11) 0.033(6) Uiso 1 1 d . . . . .
P51 P 0.89516(3) 0.51796(3) 0.39090(3) 0.02119(10) Uani 1 1 d . . . . .
P52 P 0.91734(3) 0.51533(3) 0.16648(3) 0.02145(11) Uani 1 1 d . . . . .
N51 N 0.87981(11) 0.63356(11) 0.25902(8) 0.0228(3) Uani 1 1 d . . . . .
C51 C 1.00108(13) 0.53937(13) 0.34676(10) 0.0224(4) Uani 1 1 d . . . . .
C52 C 1.00850(13) 0.61279(13) 0.29112(10) 0.0228(4) Uani 1 1 d . . . . .
C53 C 1.09031(14) 0.62678(14) 0.25891(10) 0.0276(4) Uani 1 1 d . . . . .
H53 H 1.095803 0.676294 0.221548 0.033 Uiso 1 1 calc R . . . .
C54 C 1.16382(14) 0.56994(15) 0.28027(11) 0.0311(5) Uani 1 1 d . . . . .
H54 H 1.219067 0.580294 0.257397 0.037 Uiso 1 1 calc R . . . .
C55 C 1.15617(14) 0.49805(15) 0.33508(11) 0.0292(5) Uani 1 1 d . . . . .
H55 H 1.206104 0.459121 0.350241 0.035 Uiso 1 1 calc R . . . .
C56 C 1.07565(13) 0.48306(13) 0.36773(10) 0.0251(4) Uani 1 1 d . . . . .
H56 H 1.070982 0.433448 0.405167 0.030 Uiso 1 1 calc R . . . .
C57 C 0.93203(14) 0.67623(13) 0.26376(11) 0.0265(4) Uani 1 1 d . . . . .
H57A H 0.894678 0.714188 0.294839 0.032 Uiso 1 1 calc R . . . .
H57B H 0.954282 0.712270 0.217325 0.032 Uiso 1 1 calc R . . . .
C58 C 0.83662(13) 0.59224(13) 0.44601(9) 0.0225(4) Uani 1 1 d . . . . .
C59 C 0.87677(14) 0.64008(13) 0.45401(10) 0.0251(4) Uani 1 1 d . . . . .
H59 H 0.936140 0.637009 0.428770 0.030 Uiso 1 1 calc R . . . .
C60 C 0.83021(15) 0.69272(14) 0.49904(11) 0.0286(5) Uani 1 1 d . . . . .
H60 H 0.857686 0.725906 0.503988 0.034 Uiso 1 1 calc R . . . .
C61 C 0.74448(15) 0.69654(14) 0.53627(10) 0.0298(5) Uani 1 1 d . . . . .
H61 H 0.713277 0.731691 0.567440 0.036 Uiso 1 1 calc R . . . .
C62 C 0.70351(15) 0.64950(15) 0.52855(11) 0.0308(5) Uani 1 1 d . . . . .
H62 H 0.644215 0.652623 0.554107 0.037 Uiso 1 1 calc R . . . .
C63 C 0.74945(14) 0.59756(14) 0.48320(10) 0.0267(4) Uani 1 1 d . . . . .
H63 H 0.721226 0.565583 0.477596 0.032 Uiso 1 1 calc R . . . .
C64 C 0.91981(13) 0.41387(13) 0.45386(10) 0.0238(4) Uani 1 1 d . . . . .
C65 C 0.90303(14) 0.40467(14) 0.52385(10) 0.0277(4) Uani 1 1 d . . . . .
H65 H 0.877655 0.454136 0.540696 0.033 Uiso 1 1 calc R . . . .
C66 C 0.92290(15) 0.32387(15) 0.56967(11) 0.0322(5) Uani 1 1 d . . . . .
H66 H 0.910693 0.318615 0.617421 0.039 Uiso 1 1 calc R . . . .
C67 C 0.96027(15) 0.25147(15) 0.54584(12) 0.0334(5) Uani 1 1 d . . . . .
H67 H 0.974230 0.196430 0.577036 0.040 Uiso 1 1 calc R . . . .
C68 C 0.97743(15) 0.25944(15) 0.47583(12) 0.0338(5) Uani 1 1 d . . . . .
H68 H 1.002801 0.209717 0.459314 0.041 Uiso 1 1 calc R . . . .
C69 C 0.95745(14) 0.34015(14) 0.43006(11) 0.0300(5) Uani 1 1 d . . . . .
H69 H 0.969439 0.345244 0.382369 0.036 Uiso 1 1 calc R . . . .
C70 C 0.92013(12) 0.62044(13) 0.10838(10) 0.0219(4) Uani 1 1 d . . . . .
C71 C 0.86701(12) 0.68938(13) 0.13795(10) 0.0215(4) Uani 1 1 d . . . . .
C72 C 0.85766(14) 0.77210(14) 0.09387(11) 0.0269(4) Uani 1 1 d . . . . .
H72 H 0.819802 0.819753 0.112036 0.032 Uiso 1 1 calc R . . . .
C73 C 0.90281(14) 0.78576(14) 0.02393(11) 0.0301(5) Uani 1 1 d . . . . .
H73 H 0.895146 0.842559 -0.005160 0.036 Uiso 1 1 calc R . . . .
C74 C 0.95890(14) 0.71761(15) -0.00393(11) 0.0303(5) Uani 1 1 d . . . . .
H74 H 0.991060 0.727522 -0.051519 0.036 Uiso 1 1 calc R . . . .
C75 C 0.96765(13) 0.63470(14) 0.03835(10) 0.0265(4) Uani 1 1 d . . . . .
H75 H 1.005973 0.587527 0.019706 0.032 Uiso 1 1 calc R . . . .
C76 C 0.82301(13) 0.67393(13) 0.21396(10) 0.0229(4) Uani 1 1 d . . . . .
H76 H 0.770971 0.722470 0.227654 0.027 Uiso 1 1 calc R . . . .
C77 C 0.86991(13) 0.47217(13) 0.13083(10) 0.0248(4) Uani 1 1 d . . . . .
C78 C 0.85842(16) 0.39216(16) 0.16732(12) 0.0352(5) Uani 1 1 d . . . . .
H78 H 0.876695 0.361796 0.208306 0.042 Uiso 1 1 calc R . . . .
C79 C 0.82049(17) 0.35593(18) 0.14459(14) 0.0453(6) Uani 1 1 d . . . . .
H79 H 0.813347 0.300946 0.169736 0.054 Uiso 1 1 calc R . . . .
C80 C 0.79309(15) 0.40044(18) 0.08502(13) 0.0427(6) Uani 1 1 d . . . . .
H80 H 0.767397 0.375772 0.069221 0.051 Uiso 1 1 calc R . . . .
C81 C 0.80302(15) 0.47964(17) 0.04909(13) 0.0389(6) Uani 1 1 d . . . . .
H81 H 0.783652 0.510087 0.008594 0.047 Uiso 1 1 calc R . . . .
C82 C 0.84138(14) 0.51608(15) 0.07145(11) 0.0305(5) Uani 1 1 d . . . . .
H82 H 0.848117 0.571166 0.046067 0.037 Uiso 1 1 calc R . . . .
C83 C 1.03158(13) 0.44861(13) 0.15390(10) 0.0228(4) Uani 1 1 d . . . . .
C84 C 1.06965(14) 0.38781(15) 0.11682(11) 0.0316(5) Uani 1 1 d . . . . .
H84 H 1.036652 0.381532 0.094076 0.038 Uiso 1 1 calc R . . . .
C85 C 1.15571(15) 0.33588(16) 0.11256(12) 0.0396(6) Uani 1 1 d . . . . .
H85 H 1.180850 0.294145 0.087213 0.047 Uiso 1 1 calc R . . . .
C86 C 1.20472(15) 0.34434(16) 0.14464(12) 0.0367(5) Uani 1 1 d . . . . .
H86 H 1.263366 0.308421 0.141891 0.044 Uiso 1 1 calc R . . . .
C87 C 1.16789(14) 0.40559(16) 0.18095(12) 0.0349(5) Uani 1 1 d . . . . .
H87 H 1.201724 0.412277 0.202736 0.042 Uiso 1 1 calc R . . . .
C88 C 1.08215(14) 0.45729(15) 0.18585(12) 0.0311(5) Uani 1 1 d . . . . .
H88 H 1.057485 0.499024 0.211146 0.037 Uiso 1 1 calc R . . . .
C89 C 0.67757(14) 0.55443(15) 0.27247(11) 0.0269(4) Uani 1 1 d . . . . .
H89A H 0.7425(14) 0.5383(13) 0.2384(11) 0.026(6) Uiso 1 1 d . . . . .
H89B H 0.6582(16) 0.5043(16) 0.2811(12) 0.042(7) Uiso 1 1 d . . . . .
C90 C 0.62576(15) 0.63950(15) 0.23291(11) 0.0336(5) Uani 1 1 d . . . . .
H90A H 0.643893 0.686088 0.231140 0.050 Uiso 1 1 calc GR . . . .
H90B H 0.562954 0.649551 0.256580 0.050 Uiso 1 1 calc GR . . . .
H90C H 0.637248 0.637358 0.185675 0.050 Uiso 1 1 calc GR . . . .
C91 C 0.72025(15) 0.44986(14) 0.39276(11) 0.0283(4) Uani 1 1 d . . . . .
H91A H 0.7841(16) 0.4314(15) 0.3789(12) 0.036(7) Uiso 1 1 d . . . . .
H91B H 0.7062(17) 0.4477(16) 0.4434(14) 0.048(8) Uiso 1 1 d . . . . .
C92 C 0.69625(17) 0.37857(16) 0.38732(13) 0.0382(5) Uani 1 1 d . . . . .
H92A H 0.722014 0.372872 0.339781 0.057 Uiso 1 1 calc GR . . . .
H92B H 0.632323 0.393081 0.399483 0.057 Uiso 1 1 calc GR . . . .
H92C H 0.719125 0.324328 0.419214 0.057 Uiso 1 1 calc GR . . . .
C93 C 0.56610(15) 0.58026(17) 0.39549(11) 0.0323(5) Uani 1 1 d . . . . .
H93A H 0.5373(15) 0.6374(15) 0.3666(12) 0.032(6) Uiso 1 1 d . . . . .
H93B H 0.5394(18) 0.5338(18) 0.3993(14) 0.059(8) Uiso 1 1 d . . . . .
C94 C 0.54876(15) 0.58741(18) 0.46818(12) 0.0414(6) Uani 1 1 d . . . . .
H94A H 0.575399 0.628684 0.464683 0.062 Uiso 1 1 calc GR . . . .
H94B H 0.574440 0.531311 0.496797 0.062 Uiso 1 1 calc GR . . . .
H94C H 0.485389 0.606807 0.489450 0.062 Uiso 1 1 calc GR . . . .
B51 B 0.66778(16) 0.54744(16) 0.35373(12) 0.0265(5) Uani 1 1 d . . . . .
C101 C 0.72142(8) 0.35021(10) 0.91102(9) 0.0409(6) Uani 1 1 d . U . . .
H101 H 0.665602 0.382768 0.903236 0.049 Uiso 1 1 calc R . . . .
C102 C 0.77417(11) 0.39076(8) 0.91240(9) 0.0394(6) Uani 1 1 d G U . . .
H102 H 0.754412 0.451041 0.905567 0.047 Uiso 1 1 calc R . . . .
C103 C 0.85584(10) 0.34312(11) 0.92378(9) 0.0463(6) Uani 1 1 d G U . . .
H103 H 0.891897 0.370842 0.924729 0.056 Uiso 1 1 calc R . . . .
C104 C 0.88476(9) 0.25493(11) 0.93378(10) 0.0549(7) Uani 1 1 d G U . . .
H104 H 0.940573 0.222368 0.941560 0.066 Uiso 1 1 calc R . . . .
C105 C 0.83200(12) 0.21437(8) 0.93240(10) 0.0583(8) Uani 1 1 d G U . . .
H105 H 0.851764 0.154093 0.939229 0.070 Uiso 1 1 calc R . . . .
C106 C 0.75033(11) 0.26201(10) 0.92101(10) 0.0492(7) Uani 1 1 d G U . . .
H106 H 0.714279 0.234292 0.920068 0.059 Uiso 1 1 calc R . . . .
C201 C 0.34203(12) 0.73064(11) 0.41840(11) 0.0529(7) Uani 1 1 d . U . . .
H201 H 0.374662 0.675964 0.409985 0.063 Uiso 1 1 calc R . . . .
C202 C 0.25093(12) 0.75602(14) 0.43715(13) 0.0784(11) Uani 1 1 d G U . . .
H202 H 0.221290 0.718678 0.441549 0.094 Uiso 1 1 calc R . . . .
C203 C 0.20319(10) 0.83602(16) 0.44946(16) 0.1187(19) Uani 1 1 d G U . . .
H203 H 0.140919 0.853364 0.462277 0.142 Uiso 1 1 calc R . . . .
C204 C 0.24655(15) 0.89066(12) 0.44303(14) 0.0968(14) Uani 1 1 d G U . . .
H204 H 0.213918 0.945337 0.451441 0.116 Uiso 1 1 calc R . . . .
C205 C 0.33765(15) 0.86528(13) 0.42428(11) 0.0619(8) Uani 1 1 d G U . . .
H205 H 0.367289 0.902625 0.419877 0.074 Uiso 1 1 calc R . . . .
C206 C 0.38540(10) 0.78528(13) 0.41196(10) 0.0557(7) Uani 1 1 d G . . . .
H206 H 0.447662 0.767939 0.399149 0.067 Uiso 1 1 calc R . . . .


_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
Zr1 H 1.85(2) . ?
Zr1 H1 2.10(2) . ?
Zr1 P1 2.7195(5) . ?
Zr1 P2 2.6849(5) . ?
Zr1 N1 1.9862(17) . ?
Zr1 C26 2.3029(19) . ?
Zr1 C39 2.624(2) . ?
Zr1 H39A 2.22(2) . ?
Zr1 C41 2.686(2) . ?
Zr1 H41A 2.28(3) . ?
Zr1 B1 2.479(2) . ?
P1 C1 1.831(2) . ?
P1 C8 1.8322(19) . ?
P1 C14 1.834(2) . ?
P2 C20 1.814(2) . ?
P2 C27 1.824(2) . ?
P2 C33 1.824(2) . ?
N1 C7 1.455(2) . ?
N1 C26 1.449(2) . ?
C1 C2 1.413(3) . ?
C1 C6 1.395(3) . ?
C2 C3 1.389(3) . ?
C2 C7 1.510(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.392(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.384(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.383(3) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.401(3) . ?
C8 C13 1.389(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.394(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.377(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.385(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.393(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(3) . ?
C14 C19 1.392(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.397(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.384(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.391(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.384(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.406(3) . ?
C20 C25 1.396(3) . ?
C21 C22 1.396(3) . ?
C21 C26 1.490(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.387(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.389(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.384(3) . ?
C25 H25 0.9500 . ?
C26 H26 1.0000 . ?
C27 C28 1.385(3) . ?
C27 C32 1.392(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.389(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.373(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.371(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.382(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.390(3) . ?
C33 C38 1.387(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.396(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.379(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.372(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.389(3) . ?
C38 H38 0.9500 . ?
C39 H39A 1.10(2) . ?
C39 H39B 0.98(2) . ?
C39 C40 1.531(3) . ?
C39 B1 1.669(3) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.97(3) . ?
C41 H41B 1.05(2) . ?
C41 C42 1.536(3) . ?
C41 B1 1.658(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.97(2) . ?
C43 H43B 1.07(2) . ?
C43 C44 1.535(3) . ?
C43 B1 1.604(3) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
B1 H1 1.19(2) . ?
Zr51 HA 1.82(2) . ?
Zr51 H51 2.05(2) . ?
Zr51 P51 2.7160(5) . ?
Zr51 P52 2.6858(5) . ?
Zr51 N51 1.9919(17) . ?
Zr51 C76 2.302(2) . ?
Zr51 C89 2.633(2) . ?
Zr51 H89A 2.17(2) . ?
Zr51 C91 2.692(2) . ?
Zr51 H91A 2.27(2) . ?
Zr51 B51 2.478(2) . ?
P51 C51 1.833(2) . ?
P51 C58 1.835(2) . ?
P51 C64 1.831(2) . ?
P52 C70 1.816(2) . ?
P52 C77 1.826(2) . ?
P52 C83 1.825(2) . ?
N51 C57 1.448(2) . ?
N51 C76 1.448(2) . ?
C51 C52 1.410(3) . ?
C51 C56 1.396(3) . ?
C52 C53 1.396(3) . ?
C52 C57 1.510(3) . ?
C53 H53 0.9500 . ?
C53 C54 1.388(3) . ?
C54 H54 0.9500 . ?
C54 C55 1.384(3) . ?
C55 H55 0.9500 . ?
C55 C56 1.383(3) . ?
C56 H56 0.9500 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C59 1.388(3) . ?
C58 C63 1.393(3) . ?
C59 H59 0.9500 . ?
C59 C60 1.396(3) . ?
C60 H60 0.9500 . ?
C60 C61 1.377(3) . ?
C61 H61 0.9500 . ?
C61 C62 1.383(3) . ?
C62 H62 0.9500 . ?
C62 C63 1.392(3) . ?
C63 H63 0.9500 . ?
C64 C65 1.390(3) . ?
C64 C69 1.400(3) . ?
C65 H65 0.9500 . ?
C65 C66 1.394(3) . ?
C66 H66 0.9500 . ?
C66 C67 1.380(3) . ?
C67 H67 0.9500 . ?
C67 C68 1.394(3) . ?
C68 H68 0.9500 . ?
C68 C69 1.392(3) . ?
C69 H69 0.9500 . ?
C70 C71 1.407(3) . ?
C70 C75 1.399(3) . ?
C71 C72 1.397(3) . ?
C71 C76 1.493(3) . ?
C72 H72 0.9500 . ?
C72 C73 1.388(3) . ?
C73 H73 0.9500 . ?
C73 C74 1.385(3) . ?
C74 H74 0.9500 . ?
C74 C75 1.387(3) . ?
C75 H75 0.9500 . ?
C76 H76 1.0000 . ?
C77 C78 1.388(3) . ?
C77 C82 1.393(3) . ?
C78 H78 0.9500 . ?
C78 C79 1.390(3) . ?
C79 H79 0.9500 . ?
C79 C80 1.388(4) . ?
C80 H80 0.9500 . ?
C80 C81 1.365(4) . ?
C81 H81 0.9500 . ?
C81 C82 1.394(3) . ?
C82 H82 0.9500 . ?
C83 C84 1.385(3) . ?
C83 C88 1.396(3) . ?
C84 H84 0.9500 . ?
C84 C85 1.390(3) . ?
C85 H85 0.9500 . ?
C85 C86 1.373(3) . ?
C86 H86 0.9500 . ?
C86 C87 1.381(3) . ?
C87 H87 0.9500 . ?
C87 C88 1.383(3) . ?
C88 H88 0.9500 . ?
C89 H89A 1.07(2) . ?
C89 H89B 1.00(3) . ?
C89 C90 1.529(3) . ?
C89 B51 1.669(3) . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
C91 H91A 0.97(2) . ?
C91 H91B 1.02(3) . ?
C91 C92 1.538(3) . ?
C91 B51 1.658(3) . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C93 H93A 1.01(2) . ?
C93 H93B 1.06(3) . ?
C93 C94 1.535(3) . ?
C93 B51 1.612(3) . ?
C94 H94A 0.9800 . ?
C94 H94B 0.9800 . ?
C94 H94C 0.9800 . ?
B51 H51 1.21(2) . ?
C101 H101 0.9500 . ?
C101 C102 1.3900 . ?
C101 C106 1.3900 . ?
C102 H102 0.9500 . ?
C102 C103 1.3900 . ?
C103 H103 0.9500 . ?
C103 C104 1.3900 . ?
C104 H104 0.9500 . ?
C104 C105 1.3900 . ?
C105 H105 0.9500 . ?
C105 C106 1.3900 . ?
C106 H106 0.9500 . ?
C201 H201 0.9500 . ?
C201 C202 1.3900 . ?
C201 C206 1.3900 . ?
C202 H202 0.9500 . ?
C202 C203 1.3900 . ?
C203 H203 0.9500 . ?
C203 C204 1.3900 . ?
C204 H204 0.9500 . ?
C204 C205 1.3900 . ?
C205 H205 0.9500 . ?
C205 C206 1.3900 . ?
C206 H206 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H Zr1 H1 141.2(10) . . ?
H Zr1 H39A 101.7(10) . . ?
H Zr1 H41A 65.3(10) . . ?
H1 Zr1 H39A 81.3(9) . . ?
H1 Zr1 H41A 76.3(9) . . ?
P1 Zr1 H 74.8(7) . . ?
P1 Zr1 H1 91.0(6) . . ?
P1 Zr1 H39A 162.6(6) . . ?
P1 Zr1 H41A 75.4(7) . . ?
P2 Zr1 H 65.7(7) . . ?
P2 Zr1 H1 144.4(6) . . ?
P2 Zr1 P1 123.441(17) . . ?
P2 Zr1 H39A 67.8(6) . . ?
P2 Zr1 C41 127.46(5) . . ?
P2 Zr1 H41A 118.0(7) . . ?
N1 Zr1 H 108.9(8) . . ?
N1 Zr1 H1 100.5(6) . . ?
N1 Zr1 P1 72.92(5) . . ?
N1 Zr1 P2 83.29(5) . . ?
N1 Zr1 C26 38.62(6) . . ?
N1 Zr1 C39 127.43(7) . . ?
N1 Zr1 H39A 123.7(6) . . ?
N1 Zr1 C41 149.10(6) . . ?
N1 Zr1 H41A 148.1(7) . . ?
N1 Zr1 B1 128.34(7) . . ?
C26 Zr1 H 130.2(7) . . ?
C26 Zr1 H1 88.5(6) . . ?
C26 Zr1 P1 109.71(5) . . ?
C26 Zr1 P2 72.43(5) . . ?
C26 Zr1 C39 90.09(7) . . ?
C26 Zr1 H39A 85.8(6) . . ?
C26 Zr1 C41 143.69(7) . . ?
C26 Zr1 H41A 164.2(7) . . ?
C26 Zr1 B1 106.62(7) . . ?
C39 Zr1 H 116.5(8) . . ?
C39 Zr1 H1 57.4(6) . . ?
C39 Zr1 P1 142.81(5) . . ?
C39 Zr1 P2 92.03(5) . . ?
C39 Zr1 H39A 24.4(6) . . ?
C39 Zr1 C41 62.18(7) . . ?
C39 Zr1 H41A 78.1(7) . . ?
H39A Zr1 H41A 87.6(9) . . ?
C41 Zr1 H 85.1(7) . . ?
C41 Zr1 H1 57.5(6) . . ?
C41 Zr1 P1 85.18(5) . . ?
C41 Zr1 H39A 77.5(6) . . ?
C41 Zr1 H41A 20.6(7) . . ?
B1 Zr1 H 120.4(8) . . ?
B1 Zr1 H1 28.7(6) . . ?
B1 Zr1 P1 104.90(5) . . ?
B1 Zr1 P2 129.40(5) . . ?
B1 Zr1 C39 38.06(7) . . ?
B1 Zr1 H39A 61.7(6) . . ?
B1 Zr1 C41 37.17(7) . . ?
B1 Zr1 H41A 57.7(7) . . ?
C1 P1 Zr1 107.38(6) . . ?
C1 P1 C8 102.89(9) . . ?
C1 P1 C14 104.84(9) . . ?
C8 P1 Zr1 116.14(6) . . ?
C8 P1 C14 102.72(9) . . ?
C14 P1 Zr1 120.97(6) . . ?
C20 P2 Zr1 105.45(6) . . ?
C20 P2 C27 105.17(9) . . ?
C20 P2 C33 105.99(10) . . ?
C27 P2 Zr1 119.31(6) . . ?
C33 P2 Zr1 115.32(7) . . ?
C33 P2 C27 104.47(9) . . ?
C7 N1 Zr1 153.88(13) . . ?
C26 N1 Zr1 82.59(11) . . ?
C26 N1 C7 122.80(16) . . ?
C2 C1 P1 120.64(15) . . ?
C6 C1 P1 120.47(16) . . ?
C6 C1 C2 118.90(19) . . ?
C1 C2 C7 122.60(18) . . ?
C3 C2 C1 118.91(19) . . ?
C3 C2 C7 118.48(19) . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.6(2) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.2(2) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.2(2) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 H6 119.4 . . ?
C5 C6 C1 121.2(2) . . ?
C5 C6 H6 119.4 . . ?
N1 C7 C2 111.64(16) . . ?
N1 C7 H7A 109.3 . . ?
N1 C7 H7B 109.3 . . ?
C2 C7 H7A 109.3 . . ?
C2 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C9 C8 P1 122.16(16) . . ?
C13 C8 P1 118.50(15) . . ?
C13 C8 C9 119.32(18) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 C8 119.6(2) . . ?
C10 C9 H9 120.2 . . ?
C9 C10 H10 119.7 . . ?
C11 C10 C9 120.7(2) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.04(19) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0(2) . . ?
C13 C12 H12 120.0 . . ?
C8 C13 C12 120.4(2) . . ?
C8 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 P1 122.50(16) . . ?
C15 C14 C19 118.93(19) . . ?
C19 C14 P1 118.57(15) . . ?
C14 C15 H15 119.9 . . ?
C14 C15 C16 120.2(2) . . ?
C16 C15 H15 119.9 . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.3(2) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 120.2 . . ?
C16 C17 C18 119.6(2) . . ?
C18 C17 H17 120.2 . . ?
C17 C18 H18 120.1 . . ?
C19 C18 C17 119.9(2) . . ?
C19 C18 H18 120.1 . . ?
C14 C19 H19 119.5 . . ?
C18 C19 C14 121.0(2) . . ?
C18 C19 H19 119.5 . . ?
C21 C20 P2 115.11(15) . . ?
C25 C20 P2 124.09(16) . . ?
C25 C20 C21 120.76(19) . . ?
C20 C21 C26 120.57(17) . . ?
C22 C21 C20 117.80(18) . . ?
C22 C21 C26 121.62(18) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 C21 121.1(2) . . ?
C23 C22 H22 119.5 . . ?
C22 C23 H23 119.7 . . ?
C22 C23 C24 120.6(2) . . ?
C24 C23 H23 119.7 . . ?
C23 C24 H24 120.3 . . ?
C25 C24 C23 119.3(2) . . ?
C25 C24 H24 120.3 . . ?
C20 C25 H25 119.9 . . ?
C24 C25 C20 120.3(2) . . ?
C24 C25 H25 119.9 . . ?
Zr1 C26 H26 114.5 . . ?
N1 C26 Zr1 58.79(9) . . ?
N1 C26 C21 116.32(16) . . ?
N1 C26 H26 114.5 . . ?
C21 C26 Zr1 125.92(13) . . ?
C21 C26 H26 114.5 . . ?
C28 C27 P2 123.25(16) . . ?
C28 C27 C32 118.25(19) . . ?
C32 C27 P2 118.49(15) . . ?
C27 C28 H28 119.8 . . ?
C27 C28 C29 120.5(2) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 H29 119.7 . . ?
C30 C29 C28 120.6(2) . . ?
C30 C29 H29 119.7 . . ?
C29 C30 H30 120.3 . . ?
C31 C30 C29 119.5(2) . . ?
C31 C30 H30 120.3 . . ?
C30 C31 H31 119.7 . . ?
C30 C31 C32 120.5(2) . . ?
C32 C31 H31 119.7 . . ?
C27 C32 H32 119.6 . . ?
C31 C32 C27 120.7(2) . . ?
C31 C32 H32 119.6 . . ?
C34 C33 P2 117.08(17) . . ?
C38 C33 P2 124.37(18) . . ?
C38 C33 C34 118.5(2) . . ?
C33 C34 H34 119.5 . . ?
C33 C34 C35 121.0(2) . . ?
C35 C34 H34 119.5 . . ?
C34 C35 H35 120.4 . . ?
C36 C35 C34 119.1(3) . . ?
C36 C35 H35 120.4 . . ?
C35 C36 H36 119.7 . . ?
C37 C36 C35 120.6(2) . . ?
C37 C36 H36 119.7 . . ?
C36 C37 H37 120.0 . . ?
C36 C37 C38 120.1(2) . . ?
C38 C37 H37 120.0 . . ?
C33 C38 C37 120.7(2) . . ?
C33 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
Zr1 C39 H39A 56.9(12) . . ?
Zr1 C39 H39B 126.8(14) . . ?
H39A C39 H39B 98.6(18) . . ?
C40 C39 Zr1 120.60(15) . . ?
C40 C39 H39A 105.9(12) . . ?
C40 C39 H39B 111.0(13) . . ?
C40 C39 B1 116.17(17) . . ?
B1 C39 Zr1 66.28(10) . . ?
B1 C39 H39A 120.8(12) . . ?
B1 C39 H39B 102.7(14) . . ?
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 . . ?
Zr1 C41 H41A 55.3(15) . . ?
Zr1 C41 H41B 121.0(13) . . ?
H41A C41 H41B 104.3(19) . . ?
C42 C41 Zr1 129.51(14) . . ?
C42 C41 H41A 102.8(16) . . ?
C42 C41 H41B 107.8(13) . . ?
C42 C41 B1 113.15(17) . . ?
B1 C41 Zr1 64.63(11) . . ?
B1 C41 H41A 119.9(15) . . ?
B1 C41 H41B 108.1(12) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
H43A C43 H43B 103.3(18) . . ?
C44 C43 H43A 108.3(14) . . ?
C44 C43 H43B 109.9(13) . . ?
C44 C43 B1 116.01(18) . . ?
B1 C43 H43A 110.6(14) . . ?
B1 C43 H43B 107.8(12) . . ?
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 . . ?
Zr1 B1 H1 57.6(10) . . ?
C39 B1 Zr1 75.67(11) . . ?
C39 B1 H1 106.6(11) . . ?
C41 B1 Zr1 78.20(12) . . ?
C41 B1 H1 110.4(11) . . ?
C41 B1 C39 111.02(17) . . ?
C43 B1 Zr1 160.91(16) . . ?
C43 B1 H1 103.5(11) . . ?
C43 B1 C39 110.72(17) . . ?
C43 B1 C41 114.09(18) . . ?
HA Zr51 H51 140.7(10) . . ?
HA Zr51 H89A 102.8(9) . . ?
HA Zr51 H91A 65.2(9) . . ?
H51 Zr51 H89A 80.5(8) . . ?
H51 Zr51 H91A 75.8(9) . . ?
P51 Zr51 HA 74.7(7) . . ?
P51 Zr51 H51 90.8(6) . . ?
P51 Zr51 H89A 162.8(6) . . ?
P51 Zr51 H91A 74.7(6) . . ?
P52 Zr51 HA 65.7(7) . . ?
P52 Zr51 H51 144.5(6) . . ?
P52 Zr51 P51 123.656(17) . . ?
P52 Zr51 H89A 68.2(6) . . ?
P52 Zr51 C91 126.04(5) . . ?
P52 Zr51 H91A 118.1(6) . . ?
N51 Zr51 HA 108.7(7) . . ?
N51 Zr51 H51 101.2(6) . . ?
N51 Zr51 P51 72.93(5) . . ?
N51 Zr51 P52 83.42(5) . . ?
N51 Zr51 C76 38.58(6) . . ?
N51 Zr51 C89 127.57(7) . . ?
N51 Zr51 H89A 123.2(6) . . ?
N51 Zr51 C91 150.36(6) . . ?
N51 Zr51 H91A 147.4(6) . . ?
N51 Zr51 B51 129.38(8) . . ?
C76 Zr51 HA 130.1(7) . . ?
C76 Zr51 H51 89.1(6) . . ?
C76 Zr51 P51 109.64(5) . . ?
C76 Zr51 P52 72.57(5) . . ?
C76 Zr51 C89 90.17(7) . . ?
C76 Zr51 H89A 85.2(6) . . ?
C76 Zr51 C91 144.36(7) . . ?
C76 Zr51 H91A 164.6(6) . . ?
C76 Zr51 B51 107.29(8) . . ?
C89 Zr51 HA 116.3(7) . . ?
C89 Zr51 H51 57.7(6) . . ?
C89 Zr51 P51 143.07(5) . . ?
C89 Zr51 P52 91.48(5) . . ?
C89 Zr51 H89A 23.4(6) . . ?
C89 Zr51 C91 62.05(7) . . ?
C89 Zr51 H91A 78.9(6) . . ?
H89A Zr51 H91A 88.7(8) . . ?
C91 Zr51 HA 84.4(7) . . ?
C91 Zr51 H51 57.8(6) . . ?
C91 Zr51 P51 85.79(5) . . ?
C91 Zr51 H89A 77.0(6) . . ?
C91 Zr51 H91A 20.4(6) . . ?
B51 Zr51 HA 119.7(7) . . ?
B51 Zr51 H51 29.2(6) . . ?
B51 Zr51 P51 105.22(5) . . ?
B51 Zr51 P52 128.57(5) . . ?
B51 Zr51 C89 37.95(7) . . ?
B51 Zr51 H89A 60.7(6) . . ?
B51 Zr51 C91 37.12(8) . . ?
B51 Zr51 H91A 57.5(6) . . ?
C51 P51 Zr51 107.56(6) . . ?
C51 P51 C58 103.04(9) . . ?
C58 P51 Zr51 116.24(6) . . ?
C64 P51 Zr51 121.01(7) . . ?
C64 P51 C51 104.46(9) . . ?
C64 P51 C58 102.60(9) . . ?
C70 P52 Zr51 105.38(6) . . ?
C70 P52 C77 105.98(9) . . ?
C70 P52 C83 105.67(9) . . ?
C77 P52 Zr51 115.35(7) . . ?
C83 P52 Zr51 119.06(6) . . ?
C83 P52 C77 104.35(9) . . ?
C57 N51 Zr51 153.90(13) . . ?
C76 N51 Zr51 82.35(11) . . ?
C76 N51 C57 122.90(17) . . ?
C52 C51 P51 120.52(15) . . ?
C56 C51 P51 120.44(16) . . ?
C56 C51 C52 119.04(19) . . ?
C51 C52 C57 122.83(18) . . ?
C53 C52 C51 118.75(19) . . ?
C53 C52 C57 118.41(19) . . ?
C52 C53 H53 119.3 . . ?
C54 C53 C52 121.4(2) . . ?
C54 C53 H53 119.3 . . ?
C53 C54 H54 120.2 . . ?
C55 C54 C53 119.6(2) . . ?
C55 C54 H54 120.2 . . ?
C54 C55 H55 120.1 . . ?
C56 C55 C54 119.8(2) . . ?
C56 C55 H55 120.1 . . ?
C51 C56 H56 119.3 . . ?
C55 C56 C51 121.3(2) . . ?
C55 C56 H56 119.3 . . ?
N51 C57 C52 111.58(17) . . ?
N51 C57 H57A 109.3 . . ?
N51 C57 H57B 109.3 . . ?
C52 C57 H57A 109.3 . . ?
C52 C57 H57B 109.3 . . ?
H57A C57 H57B 108.0 . . ?
C59 C58 P51 122.60(16) . . ?
C59 C58 C63 119.27(18) . . ?
C63 C58 P51 118.07(15) . . ?
C58 C59 H59 119.9 . . ?
C58 C59 C60 120.2(2) . . ?
C60 C59 H59 119.9 . . ?
C59 C60 H60 120.0 . . ?
C61 C60 C59 120.0(2) . . ?
C61 C60 H60 120.0 . . ?
C60 C61 H61 119.8 . . ?
C60 C61 C62 120.39(19) . . ?
C62 C61 H61 119.8 . . ?
C61 C62 H62 120.1 . . ?
C61 C62 C63 119.8(2) . . ?
C63 C62 H62 120.1 . . ?
C58 C63 H63 119.8 . . ?
C62 C63 C58 120.3(2) . . ?
C62 C63 H63 119.8 . . ?
C65 C64 P51 123.19(16) . . ?
C65 C64 C69 118.64(19) . . ?
C69 C64 P51 118.17(15) . . ?
C64 C65 H65 119.5 . . ?
C64 C65 C66 120.9(2) . . ?
C66 C65 H65 119.5 . . ?
C65 C66 H66 119.9 . . ?
C67 C66 C65 120.2(2) . . ?
C67 C66 H66 119.9 . . ?
C66 C67 H67 120.1 . . ?
C66 C67 C68 119.7(2) . . ?
C68 C67 H67 120.1 . . ?
C67 C68 H68 119.9 . . ?
C69 C68 C67 120.1(2) . . ?
C69 C68 H68 119.9 . . ?
C64 C69 H69 119.8 . . ?
C68 C69 C64 120.4(2) . . ?
C68 C69 H69 119.8 . . ?
C71 C70 P52 115.06(14) . . ?
C75 C70 P52 124.05(16) . . ?
C75 C70 C71 120.84(19) . . ?
C70 C71 C76 120.71(18) . . ?
C72 C71 C70 117.70(18) . . ?
C72 C71 C76 121.59(18) . . ?
C71 C72 H72 119.5 . . ?
C73 C72 C71 121.03(19) . . ?
C73 C72 H72 119.5 . . ?
C72 C73 H73 119.6 . . ?
C74 C73 C72 120.8(2) . . ?
C74 C73 H73 119.6 . . ?
C73 C74 H74 120.3 . . ?
C73 C74 C75 119.32(19) . . ?
C75 C74 H74 120.3 . . ?
C70 C75 H75 119.9 . . ?
C74 C75 C70 120.12(19) . . ?
C74 C75 H75 119.9 . . ?
Zr51 C76 H76 114.5 . . ?
N51 C76 Zr51 59.07(10) . . ?
N51 C76 C71 116.55(16) . . ?
N51 C76 H76 114.5 . . ?
C71 C76 Zr51 125.77(13) . . ?
C71 C76 H76 114.5 . . ?
C78 C77 P52 117.31(16) . . ?
C78 C77 C82 118.6(2) . . ?
C82 C77 P52 124.03(17) . . ?
C77 C78 H78 119.6 . . ?
C77 C78 C79 120.8(2) . . ?
C79 C78 H78 119.6 . . ?
C78 C79 H79 120.1 . . ?
C80 C79 C78 119.7(2) . . ?
C80 C79 H79 120.1 . . ?
C79 C80 H80 120.0 . . ?
C81 C80 C79 120.1(2) . . ?
C81 C80 H80 120.0 . . ?
C80 C81 H81 119.8 . . ?
C80 C81 C82 120.4(2) . . ?
C82 C81 H81 119.8 . . ?
C77 C82 C81 120.4(2) . . ?
C77 C82 H82 119.8 . . ?
C81 C82 H82 119.8 . . ?
C84 C83 P52 123.68(16) . . ?
C84 C83 C88 118.40(19) . . ?
C88 C83 P52 117.88(15) . . ?
C83 C84 H84 119.7 . . ?
C83 C84 C85 120.6(2) . . ?
C85 C84 H84 119.7 . . ?
C84 C85 H85 119.7 . . ?
C86 C85 C84 120.6(2) . . ?
C86 C85 H85 119.7 . . ?
C85 C86 H86 120.3 . . ?
C85 C86 C87 119.3(2) . . ?
C87 C86 H86 120.3 . . ?
C86 C87 H87 119.7 . . ?
C86 C87 C88 120.5(2) . . ?
C88 C87 H87 119.7 . . ?
C83 C88 H88 119.7 . . ?
C87 C88 C83 120.5(2) . . ?
C87 C88 H88 119.7 . . ?
Zr51 C89 H89A 53.5(11) . . ?
Zr51 C89 H89B 124.4(14) . . ?
H89A C89 H89B 101.9(18) . . ?
C90 C89 Zr51 120.18(15) . . ?
C90 C89 H89A 106.5(11) . . ?
C90 C89 H89B 114.4(14) . . ?
C90 C89 B51 116.07(18) . . ?
B51 C89 Zr51 65.99(11) . . ?
B51 C89 H89A 117.6(11) . . ?
B51 C89 H89B 99.5(14) . . ?
C89 C90 H90A 109.5 . . ?
C89 C90 H90B 109.5 . . ?
C89 C90 H90C 109.5 . . ?
H90A C90 H90B 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
Zr51 C91 H91A 54.4(14) . . ?
Zr51 C91 H91B 120.8(15) . . ?
H91A C91 H91B 102(2) . . ?
C92 C91 Zr51 126.92(15) . . ?
C92 C91 H91A 104.3(14) . . ?
C92 C91 H91B 110.4(15) . . ?
C92 C91 B51 113.51(18) . . ?
B51 C91 Zr51 64.43(11) . . ?
B51 C91 H91A 118.8(14) . . ?
B51 C91 H91B 107.5(14) . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92B 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
H93A C93 H93B 109(2) . . ?
C94 C93 H93A 109.5(13) . . ?
C94 C93 H93B 109.6(15) . . ?
C94 C93 B51 115.71(19) . . ?
B51 C93 H93A 108.9(13) . . ?
B51 C93 H93B 103.8(15) . . ?
C93 C94 H94A 109.5 . . ?
C93 C94 H94B 109.5 . . ?
C93 C94 H94C 109.5 . . ?
H94A C94 H94B 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 109.5 . . ?
Zr51 B51 H51 55.4(10) . . ?
C89 B51 Zr51 76.05(11) . . ?
C89 B51 H51 105.7(10) . . ?
C91 B51 Zr51 78.46(12) . . ?
C91 B51 H51 109.5(11) . . ?
C91 B51 C89 111.22(17) . . ?
C93 B51 Zr51 161.07(17) . . ?
C93 B51 H51 105.8(11) . . ?
C93 B51 C89 110.64(18) . . ?
C93 B51 C91 113.49(19) . . ?
C102 C101 H101 120.0 . . ?
C102 C101 C106 120.0 . . ?
C106 C101 H101 120.0 . . ?
C101 C102 H102 120.0 . . ?
C101 C102 C103 120.0 . . ?
C103 C102 H102 120.0 . . ?
C102 C103 H103 120.0 . . ?
C102 C103 C104 120.0 . . ?
C104 C103 H103 120.0 . . ?
C103 C104 H104 120.0 . . ?
C105 C104 C103 120.0 . . ?
C105 C104 H104 120.0 . . ?
C104 C105 H105 120.0 . . ?
C104 C105 C106 120.0 . . ?
C106 C105 H105 120.0 . . ?
C101 C106 H106 120.0 . . ?
C105 C106 C101 120.0 . . ?
C105 C106 H106 120.0 . . ?
C202 C201 H201 120.0 . . ?
C202 C201 C206 120.0 . . ?
C206 C201 H201 120.0 . . ?
C201 C202 H202 120.0 . . ?
C201 C202 C203 120.0 . . ?
C203 C202 H202 120.0 . . ?
C202 C203 H203 120.0 . . ?
C204 C203 C202 120.0 . . ?
C204 C203 H203 120.0 . . ?
C203 C204 H204 120.0 . . ?
C203 C204 C205 120.0 . . ?
C205 C204 H204 120.0 . . ?
C204 C205 H205 120.0 . . ?
C204 C205 C206 120.0 . . ?
C206 C205 H205 120.0 . . ?
C201 C206 H206 120.0 . . ?
C205 C206 C201 120.0 . . ?
C205 C206 H206 120.0 . . ?

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
Zr1 P1 C1 C2 46.61(16) . . . . ?
Zr1 P1 C1 C6 -133.25(14) . . . . ?
Zr1 P1 C8 C9 -123.66(15) . . . . ?
Zr1 P1 C8 C13 58.02(17) . . . . ?
Zr1 P1 C14 C15 -139.68(15) . . . . ?
Zr1 P1 C14 C19 40.0(2) . . . . ?
Zr1 P2 C20 C21 -7.26(16) . . . . ?
Zr1 P2 C20 C25 174.93(16) . . . . ?
Zr1 P2 C27 C28 139.68(16) . . . . ?
Zr1 P2 C27 C32 -38.9(2) . . . . ?
Zr1 P2 C33 C34 -60.3(2) . . . . ?
Zr1 P2 C33 C38 116.12(18) . . . . ?
Zr1 N1 C7 C2 37.5(4) . . . . ?
Zr1 N1 C26 C21 -117.74(16) . . . . ?
Zr1 C39 B1 C41 -71.08(14) . . . . ?
Zr1 C39 B1 C43 161.12(18) . . . . ?
Zr1 C41 B1 C39 69.44(14) . . . . ?
Zr1 C41 B1 C43 -164.61(18) . . . . ?
P1 C1 C2 C3 179.77(15) . . . . ?
P1 C1 C2 C7 -1.4(2) . . . . ?
P1 C1 C6 C5 -179.64(15) . . . . ?
P1 C8 C9 C10 -177.42(15) . . . . ?
P1 C8 C13 C12 176.86(16) . . . . ?
P1 C14 C15 C16 179.68(17) . . . . ?
P1 C14 C19 C18 -179.79(18) . . . . ?
P2 C20 C21 C22 -173.01(15) . . . . ?
P2 C20 C21 C26 8.3(2) . . . . ?
P2 C20 C25 C24 173.95(17) . . . . ?
P2 C27 C28 C29 -177.49(19) . . . . ?
P2 C27 C32 C31 178.26(19) . . . . ?
P2 C33 C34 C35 177.4(2) . . . . ?
P2 C33 C38 C37 -177.14(17) . . . . ?
C1 P1 C8 C9 -6.68(18) . . . . ?
C1 P1 C8 C13 175.00(16) . . . . ?
C1 P1 C14 C15 99.03(18) . . . . ?
C1 P1 C14 C19 -81.28(18) . . . . ?
C1 C2 C3 C4 0.1(3) . . . . ?
C1 C2 C7 N1 -42.4(2) . . . . ?
C2 C1 C6 C5 0.5(3) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C3 C2 C7 N1 136.46(19) . . . . ?
C3 C4 C5 C6 0.1(3) . . . . ?
C4 C5 C6 C1 -0.3(3) . . . . ?
C6 C1 C2 C3 -0.4(3) . . . . ?
C6 C1 C2 C7 178.45(18) . . . . ?
C7 N1 C26 Zr1 -173.41(19) . . . . ?
C7 N1 C26 C21 68.9(2) . . . . ?
C7 C2 C3 C4 -178.78(19) . . . . ?
C8 P1 C1 C2 -76.43(16) . . . . ?
C8 P1 C1 C6 103.70(16) . . . . ?
C8 P1 C14 C15 -8.2(2) . . . . ?
C8 P1 C14 C19 171.48(17) . . . . ?
C8 C9 C10 C11 0.4(3) . . . . ?
C9 C8 C13 C12 -1.5(3) . . . . ?
C9 C10 C11 C12 -1.1(3) . . . . ?
C10 C11 C12 C13 0.5(3) . . . . ?
C11 C12 C13 C8 0.8(3) . . . . ?
C13 C8 C9 C10 0.9(3) . . . . ?
C14 P1 C1 C2 176.45(15) . . . . ?
C14 P1 C1 C6 -3.41(18) . . . . ?
C14 P1 C8 C9 102.05(17) . . . . ?
C14 P1 C8 C13 -76.28(17) . . . . ?
C14 C15 C16 C17 0.2(3) . . . . ?
C15 C14 C19 C18 -0.1(3) . . . . ?
C15 C16 C17 C18 -0.3(3) . . . . ?
C16 C17 C18 C19 0.2(4) . . . . ?
C17 C18 C19 C14 0.0(4) . . . . ?
C19 C14 C15 C16 0.0(3) . . . . ?
C20 P2 C27 C28 -102.36(19) . . . . ?
C20 P2 C27 C32 79.06(19) . . . . ?
C20 P2 C33 C34 -176.50(18) . . . . ?
C20 P2 C33 C38 -0.1(2) . . . . ?
C20 C21 C22 C23 -2.6(3) . . . . ?
C20 C21 C26 Zr1 -5.1(3) . . . . ?
C20 C21 C26 N1 64.1(2) . . . . ?
C21 C20 C25 C24 -3.7(3) . . . . ?
C21 C22 C23 C24 -0.9(3) . . . . ?
C22 C21 C26 Zr1 176.29(15) . . . . ?
C22 C21 C26 N1 -114.5(2) . . . . ?
C22 C23 C24 C25 2.2(3) . . . . ?
C23 C24 C25 C20 0.2(3) . . . . ?
C25 C20 C21 C22 4.9(3) . . . . ?
C25 C20 C21 C26 -173.78(18) . . . . ?
C26 N1 C7 C2 -157.48(17) . . . . ?
C26 C21 C22 C23 176.1(2) . . . . ?
C27 P2 C20 C21 -134.22(15) . . . . ?
C27 P2 C20 C25 47.97(19) . . . . ?
C27 P2 C33 C34 72.7(2) . . . . ?
C27 P2 C33 C38 -110.92(19) . . . . ?
C27 C28 C29 C30 -0.9(4) . . . . ?
C28 C27 C32 C31 -0.4(3) . . . . ?
C28 C29 C30 C31 0.0(4) . . . . ?
C29 C30 C31 C32 0.7(4) . . . . ?
C30 C31 C32 C27 -0.5(4) . . . . ?
C32 C27 C28 C29 1.1(3) . . . . ?
C33 P2 C20 C21 115.47(15) . . . . ?
C33 P2 C20 C25 -62.33(19) . . . . ?
C33 P2 C27 C28 9.0(2) . . . . ?
C33 P2 C27 C32 -169.55(18) . . . . ?
C33 C34 C35 C36 -0.4(4) . . . . ?
C34 C33 C38 C37 -0.8(3) . . . . ?
C34 C35 C36 C37 0.0(5) . . . . ?
C35 C36 C37 C38 0.0(4) . . . . ?
C36 C37 C38 C33 0.4(4) . . . . ?
C38 C33 C34 C35 0.8(4) . . . . ?
C40 C39 B1 Zr1 -113.80(18) . . . . ?
C40 C39 B1 C41 175.12(18) . . . . ?
C40 C39 B1 C43 47.3(3) . . . . ?
C42 C41 B1 Zr1 -124.26(17) . . . . ?
C42 C41 B1 C39 -54.8(2) . . . . ?
C42 C41 B1 C43 71.1(2) . . . . ?
C44 C43 B1 Zr1 -68.1(5) . . . . ?
C44 C43 B1 C39 -174.56(19) . . . . ?
C44 C43 B1 C41 59.3(3) . . . . ?
Zr51 P51 C51 C52 46.35(16) . . . . ?
Zr51 P51 C51 C56 -133.55(14) . . . . ?
Zr51 P51 C58 C59 -125.22(15) . . . . ?
Zr51 P51 C58 C63 57.49(17) . . . . ?
Zr51 P51 C64 C65 -137.83(15) . . . . ?
Zr51 P51 C64 C69 42.20(19) . . . . ?
Zr51 P52 C70 C71 -6.96(15) . . . . ?
Zr51 P52 C70 C75 175.79(15) . . . . ?
Zr51 P52 C77 C78 -62.17(18) . . . . ?
Zr51 P52 C77 C82 114.91(17) . . . . ?
Zr51 P52 C83 C84 137.61(16) . . . . ?
Zr51 P52 C83 C88 -39.79(19) . . . . ?
Zr51 N51 C57 C52 38.1(4) . . . . ?
Zr51 N51 C76 C71 -117.53(16) . . . . ?
Zr51 C89 B51 C91 -71.48(15) . . . . ?
Zr51 C89 B51 C93 161.4(2) . . . . ?
Zr51 C91 B51 C89 69.93(14) . . . . ?
Zr51 C91 B51 C93 -164.55(19) . . . . ?
P51 C51 C52 C53 179.98(14) . . . . ?
P51 C51 C52 C57 -1.3(2) . . . . ?
P51 C51 C56 C55 179.98(15) . . . . ?
P51 C58 C59 C60 -177.09(15) . . . . ?
P51 C58 C63 C62 176.59(16) . . . . ?
P51 C64 C65 C66 179.87(16) . . . . ?
P51 C64 C69 C68 -179.97(17) . . . . ?
P52 C70 C71 C72 -172.07(14) . . . . ?
P52 C70 C71 C76 8.4(2) . . . . ?
P52 C70 C75 C74 173.33(16) . . . . ?
P52 C77 C78 C79 178.21(18) . . . . ?
P52 C77 C82 C81 -177.70(16) . . . . ?
P52 C83 C84 C85 -176.38(19) . . . . ?
P52 C83 C88 C87 176.89(18) . . . . ?
C51 P51 C58 C59 -7.86(19) . . . . ?
C51 P51 C58 C63 174.84(16) . . . . ?
C51 P51 C64 C65 100.93(18) . . . . ?
C51 P51 C64 C69 -79.03(18) . . . . ?
C51 C52 C53 C54 0.4(3) . . . . ?
C51 C52 C57 N51 -42.3(2) . . . . ?
C52 C51 C56 C55 0.1(3) . . . . ?
C52 C53 C54 C55 -0.6(3) . . . . ?
C53 C52 C57 N51 136.35(18) . . . . ?
C53 C54 C55 C56 0.5(3) . . . . ?
C54 C55 C56 C51 -0.3(3) . . . . ?
C56 C51 C52 C53 -0.1(3) . . . . ?
C56 C51 C52 C57 178.57(17) . . . . ?
C57 N51 C76 Zr51 -172.92(19) . . . . ?
C57 N51 C76 C71 69.5(2) . . . . ?
C57 C52 C53 C54 -178.37(18) . . . . ?
C58 P51 C51 C52 -76.97(16) . . . . ?
C58 P51 C51 C56 103.13(16) . . . . ?
C58 P51 C64 C65 -6.3(2) . . . . ?
C58 P51 C64 C69 173.72(16) . . . . ?
C58 C59 C60 C61 0.7(3) . . . . ?
C59 C58 C63 C62 -0.8(3) . . . . ?
C59 C60 C61 C62 -1.0(3) . . . . ?
C60 C61 C62 C63 0.4(3) . . . . ?
C61 C62 C63 C58 0.5(3) . . . . ?
C63 C58 C59 C60 0.2(3) . . . . ?
C64 P51 C51 C52 176.11(15) . . . . ?
C64 P51 C51 C56 -3.78(18) . . . . ?
C64 P51 C58 C59 100.46(18) . . . . ?
C64 P51 C58 C63 -76.84(17) . . . . ?
C64 C65 C66 C67 0.4(3) . . . . ?
C65 C64 C69 C68 0.1(3) . . . . ?
C65 C66 C67 C68 -0.5(3) . . . . ?
C66 C67 C68 C69 0.4(3) . . . . ?
C67 C68 C69 C64 -0.2(3) . . . . ?
C69 C64 C65 C66 -0.2(3) . . . . ?
C70 P52 C77 C78 -178.34(16) . . . . ?
C70 P52 C77 C82 -1.3(2) . . . . ?
C70 P52 C83 C84 -104.28(19) . . . . ?
C70 P52 C83 C88 78.31(18) . . . . ?
C70 C71 C72 C73 -3.2(3) . . . . ?
C70 C71 C76 Zr51 -5.6(3) . . . . ?
C70 C71 C76 N51 64.0(2) . . . . ?
C71 C70 C75 C74 -3.8(3) . . . . ?
C71 C72 C73 C74 -0.4(3) . . . . ?
C72 C71 C76 Zr51 174.87(14) . . . . ?
C72 C71 C76 N51 -115.5(2) . . . . ?
C72 C73 C74 C75 2.1(3) . . . . ?
C73 C74 C75 C70 0.0(3) . . . . ?
C75 C70 C71 C72 5.3(3) . . . . ?
C75 C70 C71 C76 -174.27(18) . . . . ?
C76 N51 C57 C52 -158.07(17) . . . . ?
C76 C71 C72 C73 176.35(19) . . . . ?
C77 P52 C70 C71 115.77(15) . . . . ?
C77 P52 C70 C75 -61.47(19) . . . . ?
C77 P52 C83 C84 7.2(2) . . . . ?
C77 P52 C83 C88 -170.16(17) . . . . ?
C77 C78 C79 C80 -0.5(4) . . . . ?
C78 C77 C82 C81 -0.7(3) . . . . ?
C78 C79 C80 C81 -0.3(4) . . . . ?
C79 C80 C81 C82 0.6(4) . . . . ?
C80 C81 C82 C77 -0.1(3) . . . . ?
C82 C77 C78 C79 1.0(3) . . . . ?
C83 P52 C70 C71 -133.86(14) . . . . ?
C83 P52 C70 C75 48.90(19) . . . . ?
C83 P52 C77 C78 70.36(18) . . . . ?
C83 P52 C77 C82 -112.56(18) . . . . ?
C83 C84 C85 C86 -0.5(4) . . . . ?
C84 C83 C88 C87 -0.6(3) . . . . ?
C84 C85 C86 C87 -0.5(4) . . . . ?
C85 C86 C87 C88 0.8(4) . . . . ?
C86 C87 C88 C83 -0.3(4) . . . . ?
C88 C83 C84 C85 1.0(3) . . . . ?
C90 C89 B51 Zr51 -113.25(17) . . . . ?
C90 C89 B51 C91 175.27(18) . . . . ?
C90 C89 B51 C93 48.2(3) . . . . ?
C92 C91 B51 Zr51 -121.20(17) . . . . ?
C92 C91 B51 C89 -51.3(2) . . . . ?
C92 C91 B51 C93 74.3(2) . . . . ?
C94 C93 B51 Zr51 -65.1(6) . . . . ?
C94 C93 B51 C89 -172.8(2) . . . . ?
C94 C93 B51 C91 61.3(3) . . . . ?
C101 C102 C103 C104 0.0 . . . . ?
C102 C101 C106 C105 0.0 . . . . ?
C102 C103 C104 C105 0.0 . . . . ?
C103 C104 C105 C106 0.0 . . . . ?
C104 C105 C106 C101 0.0 . . . . ?
C106 C101 C102 C103 0.0 . . . . ?
C201 C202 C203 C204 0.0 . . . . ?
C202 C201 C206 C205 0.0 . . . . ?
C202 C203 C204 C205 0.0 . . . . ?
C203 C204 C205 C206 0.0 . . . . ?
C204 C205 C206 C201 0.0 . . . . ?
C206 C201 C202 C203 0.0 . . . . ?
_audit_block_usercomment         'MS606 irregular yellow'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.229
_oxdiff_exptl_absorpt_empirical_full_min 0.754
_cell_oxdiff_length_a            17.3823(5)
_cell_oxdiff_length_b            17.7265(5)
_cell_oxdiff_length_c            21.7567(5)
_cell_oxdiff_angle_alpha         67.552(2)
_cell_oxdiff_angle_beta          66.932(2)
_cell_oxdiff_angle_gamma         66.047(3)
_cell_oxdiff_volume              5435.2(2)
_cell_oxdiff_measurement_reflns_used 36614
_symmetry_cell_setting           triclinic
#_space_group_name_H-M_alt       'P -1'
#_space_group_IT_number          2
_chemical_absolute_configuration .
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'



####################################################################### 
# 
# 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_ba_ms21
_database_code_depnum_ccdc_archive 'CCDC 1530468'
_audit_update_record             
;
2017-03-17 deposited with the CCDC.
2017-04-05 downloaded from the CCDC.
;
_audit_creation_date             2017-03-16

_audit_block_code                ba_ms21
_audit_block_refno               2196

_audit_creation_method           
;
Olex2 1.2
(compiled Mar  2 2017 14:00:58 for OlexSys, GUI svn.r5324)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C38 H32 I3 N P2 Zr, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C39.50 H35 Cl3 I3 N P2 Zr'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         1163.89
_chemical_melting_point          ?
_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_diffrn_ambient_temperature      120(1)
_chemical_oxdiff_formula         'C39.5 H35 Cl3 I3 N P2 Zr'
_chemical_oxdiff_usercomment     'MS461, needle, yellow'
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.32855(16)
_cell_length_b                   12.57691(19)
_cell_length_c                   15.78601(14)
_cell_angle_alpha                104.1686(10)
_cell_angle_beta                 96.0145(9)
_cell_angle_gamma                116.0700(14)
_cell_volume                     2067.44(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    69205
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.9060
_cell_measurement_theta_min      2.7560
_shelx_estimated_absorpt_T_max   0.767
_shelx_estimated_absorpt_T_min   0.767
_exptl_absorpt_coefficient_mu    2.806
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.522
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1118
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 17 0 0.0334
12 -17 0 0.0334
7 0 17 0.0892
-7 0 -17 0.1115
12 3 -16 0.0213
-12 -3 16 0.0213
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.043
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-11.9772 16.9767 -0.0108 0.0146 0.1095 -1.0119
11.9772 -16.9767 0.0108 -0.0146 -0.1095 1.0119
6.9793 0.0050 16.9803 -0.0632 1.0211 0.0828
-6.9793 -0.0050 -16.9803 0.0632 -1.0211 -0.0828
11.9891 2.9840 -15.9700 0.9848 -0.0394 0.1884
-11.9891 -2.9840 15.9700 -0.9848 0.0394 -0.1884

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            146604
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.070
_diffrn_reflns_theta_min         2.598
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     10.00  49.00   0.50   15.00    --   18.69 -77.00  30.00   78
  2  ω     -3.00  53.00   0.50   15.00    --   18.69  57.00 150.00  112
  3  ω     -2.00  25.00   0.50   15.00    --   18.69  57.00  30.00   54
  4  ω    -50.00  49.00   0.50   15.00    --   18.69 -77.00   0.00  198
  5  ω    -10.00  89.00   0.50   15.00    --   18.69  77.00-120.00  198
  6  ω    -47.00  49.00   0.50   15.00    --   18.69 -77.00 120.00  192
  7  ω    -47.00  49.00   0.50   15.00    --   18.69 -77.00 -60.00  192
  8  ω     19.00  77.00   0.50   15.00    --   18.69  57.00  60.00  116
  9  ω      3.00  69.00   0.50   15.00    --   18.69  77.00 -30.00  132
 10  ω    -29.00  49.00   0.50   15.00    --   18.69 -77.00-120.00  156
 11  ω     -3.00  40.00   0.50   15.00    --   18.69  57.00-150.00   86
 12  ω    -46.00  49.00   0.50   15.00    --   18.69 -77.00-180.00  190
 13  ω     21.00  47.00   0.50   15.00    --   18.69 -77.00  60.00   52
 14  ω    -43.00   6.00   0.50   15.00    --   18.69 -77.00  30.00   98
 15  ω    -11.00  89.00   0.50   15.00    --   18.69  77.00-150.00  200
 16  ω    -50.00  40.00   0.50   15.00    --   18.69 -57.00  90.00  180
 17  ω    -51.00  49.00   0.50   15.00    --   18.69 -77.00 -30.00  200
 18  ω    -11.00  89.00   0.50   15.00    --   18.69  77.00   0.00  200
 19  ω    -51.00  49.00   0.50   15.00    --   18.69 -77.00-150.00  200
 20  ω    -50.00  40.00   0.50   15.00    --   18.69 -57.00   0.00  180
 21  ω    -51.00  49.00   0.50   15.00    --   18.69 -77.00 -90.00  200
 22  ω     -3.00  87.00   0.50   15.00    --   18.69  57.00 -30.00  180
 23  ω     -3.00  87.00   0.50   15.00    --   18.69  57.00  90.00  180
 24  ω    -51.00  49.00   0.50   15.00    --   18.69 -77.00-180.00  200
 25  ω    -54.00  63.00   0.50   15.00    --   18.69 -19.00 150.00  234
 26  ω    -54.00  92.00   0.50   15.00    --   18.69   0.00   0.00  292
 27  ω    -54.00  92.00   0.50   15.00    --   18.69   0.00 120.00  292
 28  ω    -54.00  92.00   0.50   15.00    --   18.69   0.00 240.00  292
 29  φ      0.00 120.00   0.50   15.00  40.00  18.69   0.00    --   240
 30  φ      0.00 120.00   0.50   15.00  18.69  18.69 -20.00    --   240
 31  φ      0.00 120.00   0.50   15.00  18.69  18.69  20.00    --   240
 32  φ      0.00 120.00   0.50   15.00  18.69  18.69 -40.00    --   240
 33  φ      0.00 120.00   0.50   15.00  18.69  18.69  40.00    --   240
 34  φ      0.00 120.00   0.50   15.00  18.69  18.69 -60.00    --   240
 35  φ      0.00 120.00   0.50   15.00  18.69  18.69  60.00    --   240
 36  ω    -51.00  49.00   0.50   15.00    --   18.69 -77.00  90.00  200
 37  φ    120.00 217.00   0.50   15.00  40.00  18.69   0.00    --   194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0446627000
_diffrn_orient_matrix_UB_12      0.0323545000
_diffrn_orient_matrix_UB_13      -0.0220877000
_diffrn_orient_matrix_UB_21      0.0436373000
_diffrn_orient_matrix_UB_22      0.0372617000
_diffrn_orient_matrix_UB_23      0.0421879000
_diffrn_orient_matrix_UB_31      0.0215101000
_diffrn_orient_matrix_UB_32      -0.0444298000
_diffrn_orient_matrix_UB_33      -0.0039527000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9648
_reflns_number_total             10645
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2016/6
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         10645
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0221
_refine_ls_restrained_S_all      1.043
_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)+(0.0185P)²+1.9629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0471
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C39A-Cl1A \\sim C39A-Cl2 \\sim C39B-Cl1B \\sim C39B-Cl2
 with sigma of 0.02
 Cl2-Cl1A \\sim Cl2-Cl1B
 with sigma of 0.02
3. Others
 Sof(C39B)=Sof(H39C)=Sof(H39D)=Sof(Cl1B)=1-FVAR(1)
 Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(Cl1A)=FVAR(1)
 Fixed Sof: Cl3(0.5) Cl4(0.5) C40(0.5) H40A(0.5) H40B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C20(H20A,H20B), C39A(H39A,H39B), C39B(H39C,H39D), C40(H40A,H40B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
I1 I 0.80736(2) 0.20778(2) 0.43910(2) 0.01953(3) Uani 1 1 d . . . . .
I2 I 0.93463(2) 0.10581(2) 0.23772(2) 0.02250(4) Uani 1 1 d . . . . .
I3 I 0.57592(2) 0.00440(2) 0.13372(2) 0.02680(4) Uani 1 1 d . . . . .
Zr Zr 0.77750(2) 0.22029(2) 0.26093(2) 0.01370(4) Uani 1 1 d . . . . .
P1 P 0.86921(5) 0.30350(5) 0.12449(3) 0.01428(9) Uani 1 1 d . . . . .
P2 P 0.57943(5) 0.26106(5) 0.30859(3) 0.01520(10) Uani 1 1 d . . . . .
N N 0.84744(15) 0.40574(15) 0.30142(10) 0.0157(3) Uani 1 1 d . . . . .
C1 C 0.97956(18) 0.44612(19) 0.33309(13) 0.0168(4) Uani 1 1 d . . . . .
H1A H 0.987264 0.374260 0.341964 0.020 Uiso 1 1 calc R . . . .
H1B H 1.011782 0.512132 0.392617 0.020 Uiso 1 1 calc R . . . .
C2 C 1.06168(18) 0.49610(18) 0.27165(13) 0.0164(4) Uani 1 1 d . . . . .
C3 C 1.02591(18) 0.43426(18) 0.17812(13) 0.0159(4) Uani 1 1 d . . . . .
C4 C 1.10791(19) 0.48029(19) 0.12512(13) 0.0197(4) Uani 1 1 d . . . . .
H4 H 1.083958 0.438799 0.061928 0.024 Uiso 1 1 calc R . . . .
C5 C 1.2233(2) 0.5853(2) 0.16341(15) 0.0235(4) Uani 1 1 d . . . . .
H5 H 1.278596 0.615260 0.126832 0.028 Uiso 1 1 calc R . . . .
C6 C 1.2579(2) 0.6466(2) 0.25528(15) 0.0260(5) Uani 1 1 d . . . . .
H6 H 1.336620 0.719493 0.281762 0.031 Uiso 1 1 calc R . . . .
C7 C 1.1776(2) 0.6017(2) 0.30903(14) 0.0228(4) Uani 1 1 d . . . . .
H7 H 1.202509 0.643994 0.372138 0.027 Uiso 1 1 calc R . . . .
C8 C 0.88479(18) 0.21879(18) 0.01893(12) 0.0162(4) Uani 1 1 d . . . . .
C9 C 0.97097(19) 0.17448(19) 0.02108(13) 0.0193(4) Uani 1 1 d . . . . .
H9 H 1.019896 0.187990 0.077232 0.023 Uiso 1 1 calc R . . . .
C10 C 0.9851(2) 0.1110(2) -0.05842(14) 0.0213(4) Uani 1 1 d . . . . .
H10 H 1.043801 0.081390 -0.056471 0.026 Uiso 1 1 calc R . . . .
C11 C 0.9141(2) 0.0904(2) -0.14078(14) 0.0249(5) Uani 1 1 d . . . . .
H11 H 0.924648 0.047524 -0.195118 0.030 Uiso 1 1 calc R . . . .
C12 C 0.8278(2) 0.1327(2) -0.14352(14) 0.0286(5) Uani 1 1 d . . . . .
H12 H 0.778529 0.117949 -0.199884 0.034 Uiso 1 1 calc R . . . .
C13 C 0.8129(2) 0.1966(2) -0.06409(13) 0.0237(4) Uani 1 1 d . . . . .
H13 H 0.753449 0.225319 -0.066504 0.028 Uiso 1 1 calc R . . . .
C14 C 0.78559(18) 0.38202(19) 0.09103(12) 0.0163(4) Uani 1 1 d . . . . .
C15 C 0.65748(19) 0.3121(2) 0.05412(13) 0.0191(4) Uani 1 1 d . . . . .
H15 H 0.615123 0.225401 0.047282 0.023 Uiso 1 1 calc R . . . .
C16 C 0.5914(2) 0.3687(2) 0.02728(14) 0.0236(4) Uani 1 1 d . . . . .
H16 H 0.504517 0.320215 0.000690 0.028 Uiso 1 1 calc R . . . .
C17 C 0.6521(2) 0.4952(2) 0.03925(15) 0.0264(5) Uani 1 1 d . . . . .
H17 H 0.606739 0.533637 0.020844 0.032 Uiso 1 1 calc R . . . .
C18 C 0.7787(2) 0.5664(2) 0.07795(15) 0.0241(4) Uani 1 1 d . . . . .
H18 H 0.819659 0.653786 0.087287 0.029 Uiso 1 1 calc R . . . .
C19 C 0.84591(19) 0.51018(19) 0.10315(13) 0.0192(4) Uani 1 1 d . . . . .
H19 H 0.933090 0.558944 0.128674 0.023 Uiso 1 1 calc R . . . .
C20 C 0.81078(19) 0.50386(19) 0.31975(14) 0.0192(4) Uani 1 1 d . . . . .
H20A H 0.746445 0.486530 0.267489 0.023 Uiso 1 1 calc R . . . .
H20B H 0.883818 0.585883 0.328750 0.023 Uiso 1 1 calc R . . . .
C21 C 0.76003(19) 0.50878(19) 0.40304(13) 0.0179(4) Uani 1 1 d . . . . .
C22 C 0.65294(19) 0.40425(19) 0.40578(13) 0.0173(4) Uani 1 1 d . . . . .
C23 C 0.6095(2) 0.4100(2) 0.48413(14) 0.0222(4) Uani 1 1 d . . . . .
H23 H 0.537517 0.339611 0.486275 0.027 Uiso 1 1 calc R . . . .
C24 C 0.6708(2) 0.5178(2) 0.55906(14) 0.0278(5) Uani 1 1 d . . . . .
H24 H 0.640727 0.520940 0.612123 0.033 Uiso 1 1 calc R . . . .
C25 C 0.7755(2) 0.6203(2) 0.55609(15) 0.0273(5) Uani 1 1 d . . . . .
H25 H 0.817613 0.693907 0.607234 0.033 Uiso 1 1 calc R . . . .
C26 C 0.8194(2) 0.6158(2) 0.47845(15) 0.0243(4) Uani 1 1 d . . . . .
H26 H 0.891070 0.686968 0.476867 0.029 Uiso 1 1 calc R . . . .
C27 C 0.45333(19) 0.14707(19) 0.34278(13) 0.0186(4) Uani 1 1 d . . . . .
C28 C 0.4627(2) 0.05164(19) 0.36682(13) 0.0206(4) Uani 1 1 d . . . . .
H28 H 0.534682 0.042299 0.363470 0.025 Uiso 1 1 calc R . . . .
C29 C 0.3672(2) -0.0300(2) 0.39569(14) 0.0241(4) Uani 1 1 d . . . . .
H29 H 0.374815 -0.094185 0.412911 0.029 Uiso 1 1 calc R . . . .
C30 C 0.2612(2) -0.0186(2) 0.39955(14) 0.0256(5) Uani 1 1 d . . . . .
H30 H 0.195910 -0.075162 0.418913 0.031 Uiso 1 1 calc R . . . .
C31 C 0.2504(2) 0.0756(2) 0.37512(15) 0.0262(5) Uani 1 1 d . . . . .
H31 H 0.177441 0.083349 0.377550 0.031 Uiso 1 1 calc R . . . .
C32 C 0.3457(2) 0.1584(2) 0.34716(14) 0.0223(4) Uani 1 1 d . . . . .
H32 H 0.338147 0.223152 0.330874 0.027 Uiso 1 1 calc R . . . .
C33 C 0.48663(18) 0.2909(2) 0.22787(13) 0.0185(4) Uani 1 1 d . . . . .
C34 C 0.4009(2) 0.1898(2) 0.15327(14) 0.0241(4) Uani 1 1 d . . . . .
H34 H 0.399724 0.111477 0.141228 0.029 Uiso 1 1 calc R . . . .
C35 C 0.3174(2) 0.2032(2) 0.09661(16) 0.0302(5) Uani 1 1 d . . . . .
H35 H 0.258912 0.133882 0.046101 0.036 Uiso 1 1 calc R . . . .
C36 C 0.3190(2) 0.3170(3) 0.11335(17) 0.0326(5) Uani 1 1 d . . . . .
H36 H 0.260818 0.325565 0.074883 0.039 Uiso 1 1 calc R . . . .
C37 C 0.4048(2) 0.4180(2) 0.18576(17) 0.0318(5) Uani 1 1 d . . . . .
H37 H 0.406366 0.496407 0.196509 0.038 Uiso 1 1 calc R . . . .
C38 C 0.4892(2) 0.4062(2) 0.24336(15) 0.0239(4) Uani 1 1 d . . . . .
H38 H 0.548384 0.476374 0.293084 0.029 Uiso 1 1 calc R . . . .
Cl2 Cl 0.58498(8) 0.77545(9) 0.37512(5) 0.0643(2) Uani 1 1 d D . . . .
C39A C 0.6132(7) 0.8253(6) 0.2797(4) 0.0399(14) Uani 0.502(4) 1 d D . P A 1
H39A H 0.543374 0.836710 0.254989 0.048 Uiso 0.502(4) 1 calc R . P A 1
H39B H 0.690223 0.906991 0.298381 0.048 Uiso 0.502(4) 1 calc R . P A 1
Cl1A Cl 0.6287(2) 0.71752(15) 0.19671(11) 0.0565(6) Uani 0.502(4) 1 d D . P A 1
C39B C 0.6821(8) 0.8414(6) 0.3096(5) 0.0556(18) Uani 0.498(4) 1 d D . P A 2
H39C H 0.636491 0.859521 0.264638 0.067 Uiso 0.498(4) 1 calc R . P A 2
H39D H 0.754320 0.921709 0.348440 0.067 Uiso 0.498(4) 1 calc R . P A 2
Cl1B Cl 0.7347(4) 0.7434(2) 0.2546(3) 0.1193(19) Uani 0.498(4) 1 d D . P A 2
Cl3 Cl 0.93636(15) 0.84366(14) 0.34928(12) 0.0536(4) Uani 0.5 1 d . . P B -3
Cl4 Cl 1.03133(17) 1.0316(2) 0.52720(13) 0.0620(5) Uani 0.5 1 d . . P B -3
C40 C 0.9106(8) 0.9442(9) 0.4314(7) 0.070(2) Uani 0.5 1 d . . P B -3
H40A H 0.896048 1.002097 0.405141 0.084 Uiso 0.5 1 calc R . P B -3
H40B H 0.833976 0.894305 0.448760 0.084 Uiso 0.5 1 calc R . P B -3


_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
I1 Zr 2.8498(2) . ?
I2 Zr 2.8812(2) . ?
I3 Zr 2.8169(2) . ?
Zr P1 2.7543(5) . ?
Zr P2 2.8442(5) . ?
Zr N 1.9949(16) . ?
Zr C1 2.678(2) . ?
P1 C3 1.827(2) . ?
P1 C8 1.8239(19) . ?
P1 C14 1.831(2) . ?
P2 C22 1.828(2) . ?
P2 C27 1.833(2) . ?
P2 C33 1.838(2) . ?
N C1 1.463(2) . ?
N C20 1.467(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.518(3) . ?
C2 C3 1.407(3) . ?
C2 C7 1.388(3) . ?
C3 C4 1.399(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.383(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.383(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.392(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.401(3) . ?
C8 C13 1.393(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.386(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.386(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.383(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.392(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.394(3) . ?
C14 C19 1.398(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.391(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.380(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.384(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.389(3) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.514(3) . ?
C21 C22 1.410(3) . ?
C21 C26 1.390(3) . ?
C22 C23 1.397(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.391(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.382(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.389(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.390(3) . ?
C27 C32 1.402(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.388(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.382(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.386(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.385(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.395(3) . ?
C33 C38 1.396(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.386(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.382(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.376(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.391(3) . ?
C38 H38 0.9500 . ?
Cl2 C39A 1.779(5) . ?
Cl2 C39B 1.731(7) . ?
C39A H39A 0.9900 . ?
C39A H39B 0.9900 . ?
C39A Cl1A 1.732(6) . ?
C39B H39C 0.9900 . ?
C39B H39D 0.9900 . ?
C39B Cl1B 1.730(6) . ?
Cl3 C40 1.737(9) . ?
Cl4 C40 1.729(10) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Zr I2 85.137(6) . . ?
I3 Zr I1 114.009(7) . . ?
I3 Zr I2 90.489(7) . . ?
I3 Zr P2 81.052(12) . . ?
P1 Zr I1 152.319(13) . . ?
P1 Zr I2 81.943(11) . . ?
P1 Zr I3 90.549(12) . . ?
P1 Zr P2 116.856(15) . . ?
P2 Zr I1 81.119(11) . . ?
P2 Zr I2 159.218(13) . . ?
N Zr I1 94.33(5) . . ?
N Zr I2 121.75(5) . . ?
N Zr I3 139.36(5) . . ?
N Zr P1 72.32(5) . . ?
N Zr P2 75.02(5) . . ?
N Zr C1 32.49(6) . . ?
C1 Zr I1 84.76(4) . . ?
C1 Zr I2 90.02(4) . . ?
C1 Zr I3 161.20(4) . . ?
C1 Zr P1 70.92(4) . . ?
C1 Zr P2 104.09(4) . . ?
C3 P1 Zr 105.71(6) . . ?
C3 P1 C14 102.11(9) . . ?
C8 P1 Zr 130.14(6) . . ?
C8 P1 C3 104.14(9) . . ?
C8 P1 C14 104.57(9) . . ?
C14 P1 Zr 107.00(6) . . ?
C22 P2 Zr 105.51(6) . . ?
C22 P2 C27 104.92(9) . . ?
C22 P2 C33 104.39(9) . . ?
C27 P2 Zr 121.66(7) . . ?
C27 P2 C33 99.41(9) . . ?
C33 P2 Zr 119.10(6) . . ?
C1 N Zr 100.41(11) . . ?
C1 N C20 116.57(16) . . ?
C20 N Zr 142.27(13) . . ?
Zr C1 H1A 63.3 . . ?
Zr C1 H1B 133.8 . . ?
N C1 Zr 47.10(9) . . ?
N C1 H1A 108.4 . . ?
N C1 H1B 108.4 . . ?
N C1 C2 115.72(16) . . ?
H1A C1 H1B 107.4 . . ?
C2 C1 Zr 117.57(12) . . ?
C2 C1 H1A 108.4 . . ?
C2 C1 H1B 108.4 . . ?
C3 C2 C1 121.59(17) . . ?
C7 C2 C1 119.29(17) . . ?
C7 C2 C3 119.04(18) . . ?
C2 C3 P1 120.60(14) . . ?
C4 C3 P1 119.83(15) . . ?
C4 C3 C2 119.35(18) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 C3 120.93(19) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.62(19) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 H6 119.9 . . ?
C5 C6 C7 120.2(2) . . ?
C7 C6 H6 119.9 . . ?
C2 C7 C6 120.88(19) . . ?
C2 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C9 C8 P1 119.34(14) . . ?
C13 C8 P1 121.71(15) . . ?
C13 C8 C9 118.96(17) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.20(18) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 119.8 . . ?
C9 C10 C11 120.49(19) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 H11 120.1 . . ?
C12 C11 C10 119.71(19) . . ?
C12 C11 H11 120.1 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.3(2) . . ?
C13 C12 H12 119.8 . . ?
C8 C13 H13 119.8 . . ?
C12 C13 C8 120.32(19) . . ?
C12 C13 H13 119.8 . . ?
C15 C14 P1 118.82(15) . . ?
C15 C14 C19 119.18(18) . . ?
C19 C14 P1 121.98(15) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 C14 120.2(2) . . ?
C16 C15 H15 119.9 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 C15 120.1(2) . . ?
C17 C16 H16 120.0 . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.3(2) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.1(2) . . ?
C19 C18 H18 120.0 . . ?
C14 C19 H19 119.9 . . ?
C18 C19 C14 120.13(19) . . ?
C18 C19 H19 119.9 . . ?
N C20 H20A 109.6 . . ?
N C20 H20B 109.6 . . ?
N C20 C21 110.30(16) . . ?
H20A C20 H20B 108.1 . . ?
C21 C20 H20A 109.6 . . ?
C21 C20 H20B 109.6 . . ?
C22 C21 C20 120.50(17) . . ?
C26 C21 C20 120.46(19) . . ?
C26 C21 C22 119.03(18) . . ?
C21 C22 P2 118.94(14) . . ?
C23 C22 P2 121.49(16) . . ?
C23 C22 C21 119.48(19) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 C22 120.6(2) . . ?
C24 C23 H23 119.7 . . ?
C23 C24 H24 120.1 . . ?
C25 C24 C23 119.8(2) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 H25 119.9 . . ?
C24 C25 C26 120.1(2) . . ?
C26 C25 H25 119.9 . . ?
C21 C26 H26 119.5 . . ?
C25 C26 C21 121.0(2) . . ?
C25 C26 H26 119.5 . . ?
C28 C27 P2 121.87(16) . . ?
C28 C27 C32 119.03(19) . . ?
C32 C27 P2 119.08(15) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 C27 120.2(2) . . ?
C29 C28 H28 119.9 . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.5(2) . . ?
C30 C29 H29 119.8 . . ?
C29 C30 H30 120.1 . . ?
C29 C30 C31 119.9(2) . . ?
C31 C30 H30 120.1 . . ?
C30 C31 H31 119.9 . . ?
C32 C31 C30 120.1(2) . . ?
C32 C31 H31 119.9 . . ?
C27 C32 H32 119.8 . . ?
C31 C32 C27 120.3(2) . . ?
C31 C32 H32 119.8 . . ?
C34 C33 P2 117.87(16) . . ?
C34 C33 C38 119.14(19) . . ?
C38 C33 P2 122.62(16) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 C33 120.3(2) . . ?
C35 C34 H34 119.9 . . ?
C34 C35 H35 119.9 . . ?
C36 C35 C34 120.2(2) . . ?
C36 C35 H35 119.9 . . ?
C35 C36 H36 120.0 . . ?
C37 C36 C35 120.0(2) . . ?
C37 C36 H36 120.0 . . ?
C36 C37 H37 119.7 . . ?
C36 C37 C38 120.6(2) . . ?
C38 C37 H37 119.7 . . ?
C33 C38 H38 120.1 . . ?
C37 C38 C33 119.8(2) . . ?
C37 C38 H38 120.1 . . ?
Cl2 C39A H39A 109.3 . . ?
Cl2 C39A H39B 109.3 . . ?
H39A C39A H39B 108.0 . . ?
Cl1A C39A Cl2 111.4(3) . . ?
Cl1A C39A H39A 109.3 . . ?
Cl1A C39A H39B 109.3 . . ?
Cl2 C39B H39C 109.3 . . ?
Cl2 C39B H39D 109.3 . . ?
H39C C39B H39D 107.9 . . ?
Cl1B C39B Cl2 111.7(4) . . ?
Cl1B C39B H39C 109.3 . . ?
Cl1B C39B H39D 109.3 . . ?
Cl3 C40 H40A 108.7 . . ?
Cl3 C40 H40B 108.7 . . ?
Cl4 C40 Cl3 114.3(4) . . ?
Cl4 C40 H40A 108.7 . . ?
Cl4 C40 H40B 108.7 . . ?
H40A C40 H40B 107.6 . . ?

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 P1 C3 C2 -19.07(17) . . . . ?
Zr P1 C3 C4 166.29(14) . . . . ?
Zr P1 C8 C9 -68.26(18) . . . . ?
Zr P1 C8 C13 111.61(17) . . . . ?
Zr P1 C14 C15 -63.57(15) . . . . ?
Zr P1 C14 C19 115.06(15) . . . . ?
Zr P2 C22 C21 46.21(16) . . . . ?
Zr P2 C22 C23 -130.22(16) . . . . ?
Zr P2 C27 C28 15.0(2) . . . . ?
Zr P2 C27 C32 -166.71(13) . . . . ?
Zr P2 C33 C34 74.47(17) . . . . ?
Zr P2 C33 C38 -112.57(16) . . . . ?
Zr N C1 C2 104.69(15) . . . . ?
Zr N C20 C21 69.6(3) . . . . ?
Zr C1 C2 C3 7.7(2) . . . . ?
Zr C1 C2 C7 -168.94(14) . . . . ?
P1 C3 C4 C5 174.80(16) . . . . ?
P1 C8 C9 C10 -179.35(16) . . . . ?
P1 C8 C13 C12 179.41(18) . . . . ?
P1 C14 C15 C16 -179.42(15) . . . . ?
P1 C14 C19 C18 -179.12(15) . . . . ?
P2 C22 C23 C24 176.60(16) . . . . ?
P2 C27 C28 C29 177.50(16) . . . . ?
P2 C27 C32 C31 -178.26(17) . . . . ?
P2 C33 C34 C35 171.64(16) . . . . ?
P2 C33 C38 C37 -171.37(16) . . . . ?
N C1 C2 C3 -45.3(3) . . . . ?
N C1 C2 C7 137.99(19) . . . . ?
N C20 C21 C22 -61.4(2) . . . . ?
N C20 C21 C26 117.7(2) . . . . ?
C1 N C20 C21 -97.87(19) . . . . ?
C1 C2 C3 P1 8.9(3) . . . . ?
C1 C2 C3 C4 -176.49(18) . . . . ?
C1 C2 C7 C6 176.82(19) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C3 P1 C8 C9 57.03(18) . . . . ?
C3 P1 C8 C13 -123.10(18) . . . . ?
C3 P1 C14 C15 -174.38(15) . . . . ?
C3 P1 C14 C19 4.25(17) . . . . ?
C3 C2 C7 C6 0.1(3) . . . . ?
C3 C4 C5 C6 -0.6(3) . . . . ?
C4 C5 C6 C7 0.9(3) . . . . ?
C5 C6 C7 C2 -0.6(3) . . . . ?
C7 C2 C3 P1 -174.48(15) . . . . ?
C7 C2 C3 C4 0.2(3) . . . . ?
C8 P1 C3 C2 -158.66(16) . . . . ?
C8 P1 C3 C4 26.70(18) . . . . ?
C8 P1 C14 C15 77.32(16) . . . . ?
C8 P1 C14 C19 -104.05(16) . . . . ?
C8 C9 C10 C11 -0.1(3) . . . . ?
C9 C8 C13 C12 -0.7(3) . . . . ?
C9 C10 C11 C12 -0.6(3) . . . . ?
C10 C11 C12 C13 0.6(4) . . . . ?
C11 C12 C13 C8 0.0(4) . . . . ?
C13 C8 C9 C10 0.8(3) . . . . ?
C14 P1 C3 C2 92.71(17) . . . . ?
C14 P1 C3 C4 -81.93(17) . . . . ?
C14 P1 C8 C9 163.83(16) . . . . ?
C14 P1 C8 C13 -16.3(2) . . . . ?
C14 C15 C16 C17 -1.7(3) . . . . ?
C15 C14 C19 C18 -0.5(3) . . . . ?
C15 C16 C17 C18 0.0(3) . . . . ?
C16 C17 C18 C19 1.4(3) . . . . ?
C17 C18 C19 C14 -1.2(3) . . . . ?
C19 C14 C15 C16 1.9(3) . . . . ?
C20 N C1 Zr 172.27(18) . . . . ?
C20 N C1 C2 -83.0(2) . . . . ?
C20 C21 C22 P2 2.0(3) . . . . ?
C20 C21 C22 C23 178.51(18) . . . . ?
C20 C21 C26 C25 -178.33(19) . . . . ?
C21 C22 C23 C24 0.2(3) . . . . ?
C22 P2 C27 C28 -104.26(17) . . . . ?
C22 P2 C27 C32 73.99(18) . . . . ?
C22 P2 C33 C34 -168.22(16) . . . . ?
C22 P2 C33 C38 4.74(19) . . . . ?
C22 C21 C26 C25 0.7(3) . . . . ?
C22 C23 C24 C25 0.0(3) . . . . ?
C23 C24 C25 C26 0.1(3) . . . . ?
C24 C25 C26 C21 -0.5(3) . . . . ?
C26 C21 C22 P2 -177.06(15) . . . . ?
C26 C21 C22 C23 -0.6(3) . . . . ?
C27 P2 C22 C21 175.82(15) . . . . ?
C27 P2 C22 C23 -0.61(19) . . . . ?
C27 P2 C33 C34 -60.04(17) . . . . ?
C27 P2 C33 C38 112.92(17) . . . . ?
C27 C28 C29 C30 1.0(3) . . . . ?
C28 C27 C32 C31 0.0(3) . . . . ?
C28 C29 C30 C31 -0.5(3) . . . . ?
C29 C30 C31 C32 -0.2(3) . . . . ?
C30 C31 C32 C27 0.4(3) . . . . ?
C32 C27 C28 C29 -0.8(3) . . . . ?
C33 P2 C22 C21 -80.11(17) . . . . ?
C33 P2 C22 C23 103.46(17) . . . . ?
C33 P2 C27 C28 147.99(17) . . . . ?
C33 P2 C27 C32 -33.76(18) . . . . ?
C33 C34 C35 C36 0.4(3) . . . . ?
C34 C33 C38 C37 1.5(3) . . . . ?
C34 C35 C36 C37 0.9(3) . . . . ?
C35 C36 C37 C38 -1.0(3) . . . . ?
C36 C37 C38 C33 -0.3(3) . . . . ?
C38 C33 C34 C35 -1.6(3) . . . . ?
_audit_block_usercomment         'MS461, needle, yellow'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.164
_oxdiff_exptl_absorpt_empirical_full_min 0.813
_cell_oxdiff_length_a            12.32855(16)
_cell_oxdiff_length_b            12.57691(19)
_cell_oxdiff_length_c            15.78601(14)
_cell_oxdiff_angle_alpha         104.1686(10)
_cell_oxdiff_angle_beta          96.0145(9)
_cell_oxdiff_angle_gamma         116.0700(14)
_cell_oxdiff_volume              2067.45(4)
_cell_oxdiff_measurement_reflns_used 69205
_symmetry_cell_setting           triclinic
#_space_group_name_H-M_alt       'P -1'
#_space_group_IT_number          2
_chemical_absolute_configuration .
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ba_sb68_4
_database_code_depnum_ccdc_archive 'CCDC 1530470'
_audit_update_record             
;
2017-03-17 deposited with the CCDC.
2017-04-05 downloaded from the CCDC.
;
_audit_creation_date             2016-07-06

_audit_block_code                ba_sb68
_audit_block_refno               2738
_audit_block_usercomment         'sb-dh45,block, yellow'


# start Validation Reply Form
_vrf_PLAT910_ba_sb68_4           
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          11 Note
RESPONSE: limited by diffractometer.
;
# end Validation Reply Form

_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C38 H32 Hf I3 N P2, C7 H8'
_chemical_formula_sum            'C45 H40 Hf I3 N P2'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         1215.91
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_diffrn_ambient_temperature      120(1)
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'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/n'
_symmetry_int_tables_number      14
_chemical_absolute_configuration .

_space_group_name_Hall           '-P 2yn'
loop_
_symmetry_equiv_pos_as_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                   12.3761(2)
_cell_length_b                   17.07238(16)
_cell_length_c                   20.1630(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.9429(13)
_cell_angle_gamma                90
_cell_volume                     4168.04(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    38775
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      31.8460
_cell_measurement_theta_min      3.4140
_shelx_estimated_absorpt_T_max   0.644
_shelx_estimated_absorpt_T_min   0.644
_exptl_absorpt_coefficient_mu    4.834
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.056
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            111112
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.372
_diffrn_reflns_theta_min         2.920
_diffrn_detector_area_resol_mean 7.9621
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10980
_reflns_number_total             14368
_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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         2.483
_refine_diff_density_min         -1.400
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         14368
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0404
_refine_ls_restrained_S_all      1.161
_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)+(0.0298P)²+14.9794P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0946
_refine_special_details          
;
refinement against all singles involving the major twin domain.
see _twin_ and _oxdiff_twin_
;
_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), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C52(H52), C53(H53), C54(H54),
  C55(H55), C56(H56)
2.c Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Hf Hf 0.72082(2) 0.54818(2) 0.29478(2) 0.01254(5) Uani 1 1 d . . . . .
I1 I 0.68261(3) 0.64326(2) 0.17999(2) 0.01753(7) Uani 1 1 d . . . . .
I2 I 0.94301(3) 0.59273(2) 0.34237(2) 0.02042(7) Uani 1 1 d . . . . .
I3 I 0.67678(3) 0.65032(2) 0.39768(2) 0.02131(8) Uani 1 1 d . . . . .
P1 P 0.81008(11) 0.44262(7) 0.21090(6) 0.0156(2) Uani 1 1 d . . . . .
P2 P 0.49460(10) 0.55009(8) 0.26436(6) 0.0149(2) Uani 1 1 d . . . . .
N N 0.6693(3) 0.4383(2) 0.3146(2) 0.0153(8) Uani 1 1 d . . . . .
C1 C 0.8382(4) 0.3545(3) 0.2649(3) 0.0200(10) Uani 1 1 d . . . . .
H1A H 0.7752 0.3177 0.2538 0.024 Uiso 1 1 calc R . . . .
H1B H 0.9050 0.3277 0.2566 0.024 Uiso 1 1 calc R . . . .
C2 C 0.8552(4) 0.3784(3) 0.3381(3) 0.0182(10) Uani 1 1 d . . . . .
C3 C 0.7705(4) 0.4175(3) 0.3615(2) 0.0173(10) Uani 1 1 d . . . . .
C4 C 0.7844(4) 0.4399(3) 0.4295(3) 0.0208(10) Uani 1 1 d . . . . .
H4 H 0.7261 0.4651 0.4453 0.025 Uiso 1 1 calc R . . . .
C5 C 0.8846(5) 0.4249(4) 0.4739(3) 0.0268(12) Uani 1 1 d . . . . .
H5 H 0.8946 0.4403 0.5201 0.032 Uiso 1 1 calc R . . . .
C6 C 0.9694(4) 0.3878(4) 0.4511(3) 0.0296(13) Uani 1 1 d . . . . .
H6 H 1.0380 0.3790 0.4814 0.036 Uiso 1 1 calc R . . . .
C7 C 0.9548(4) 0.3634(3) 0.3839(3) 0.0240(11) Uani 1 1 d . . . . .
H7 H 1.0125 0.3364 0.3690 0.029 Uiso 1 1 calc R . . . .
C8 C 0.9353(4) 0.4569(3) 0.1774(2) 0.0194(10) Uani 1 1 d . . . . .
C9 C 0.9802(5) 0.5312(3) 0.1750(3) 0.0241(11) Uani 1 1 d . . . . .
H9 H 0.9475 0.5749 0.1924 0.029 Uiso 1 1 calc R . . . .
C10 C 1.0738(5) 0.5419(4) 0.1467(3) 0.0299(13) Uani 1 1 d . . . . .
H10 H 1.1045 0.5926 0.1449 0.036 Uiso 1 1 calc R . . . .
C11 C 1.1208(5) 0.4783(4) 0.1218(3) 0.0305(13) Uani 1 1 d . . . . .
H11 H 1.1837 0.4857 0.1022 0.037 Uiso 1 1 calc R . . . .
C12 C 1.0782(5) 0.4040(4) 0.1246(3) 0.0335(14) Uani 1 1 d . . . . .
H12 H 1.1124 0.3606 0.1078 0.040 Uiso 1 1 calc R . . . .
C13 C 0.9856(5) 0.3928(4) 0.1520(3) 0.0283(12) Uani 1 1 d . . . . .
H13 H 0.9560 0.3417 0.1537 0.034 Uiso 1 1 calc R . . . .
C14 C 0.7148(4) 0.4108(3) 0.1336(3) 0.0192(10) Uani 1 1 d . . . . .
C15 C 0.6981(5) 0.4632(3) 0.0787(3) 0.0265(12) Uani 1 1 d . . . . .
H15 H 0.7377 0.5112 0.0823 0.032 Uiso 1 1 calc R . . . .
C16 C 0.6234(6) 0.4446(4) 0.0190(3) 0.0369(15) Uani 1 1 d . . . . .
H16 H 0.6106 0.4807 -0.0177 0.044 Uiso 1 1 calc R . . . .
C17 C 0.5676(5) 0.3737(4) 0.0130(3) 0.0350(15) Uani 1 1 d . . . . .
H17 H 0.5173 0.3612 -0.0280 0.042 Uiso 1 1 calc R . . . .
C18 C 0.5850(5) 0.3213(4) 0.0662(3) 0.0337(14) Uani 1 1 d . . . . .
H18 H 0.5475 0.2725 0.0618 0.040 Uiso 1 1 calc R . . . .
C19 C 0.6587(4) 0.3407(3) 0.1270(3) 0.0240(11) Uani 1 1 d . . . . .
H19 H 0.6699 0.3049 0.1639 0.029 Uiso 1 1 calc R . . . .
C20 C 0.4752(4) 0.4679(3) 0.2043(3) 0.0188(10) Uani 1 1 d . . . . .
H20A H 0.3987 0.4685 0.1772 0.023 Uiso 1 1 calc R . . . .
H20B H 0.5262 0.4737 0.1727 0.023 Uiso 1 1 calc R . . . .
C21 C 0.4967(4) 0.3912(3) 0.2411(3) 0.0175(10) Uani 1 1 d . . . . .
C22 C 0.5907(4) 0.3784(3) 0.2943(3) 0.0168(9) Uani 1 1 d . . . . .
C23 C 0.6021(4) 0.3064(3) 0.3271(3) 0.0240(11) Uani 1 1 d . . . . .
H23 H 0.6630 0.2979 0.3637 0.029 Uiso 1 1 calc R . . . .
C24 C 0.5267(5) 0.2471(3) 0.3075(4) 0.0339(14) Uani 1 1 d . . . . .
H24 H 0.5372 0.1983 0.3306 0.041 Uiso 1 1 calc R . . . .
C25 C 0.4369(5) 0.2570(3) 0.2556(4) 0.0327(14) Uani 1 1 d . . . . .
H25 H 0.3856 0.2156 0.2421 0.039 Uiso 1 1 calc R . . . .
C26 C 0.4230(4) 0.3293(3) 0.2232(3) 0.0260(12) Uani 1 1 d . . . . .
H26 H 0.3607 0.3368 0.1873 0.031 Uiso 1 1 calc R . . . .
C27 C 0.4142(4) 0.6313(3) 0.2213(3) 0.0174(10) Uani 1 1 d . . . . .
C28 C 0.3724(4) 0.6314(3) 0.1516(3) 0.0229(11) Uani 1 1 d . . . . .
H28 H 0.3849 0.5876 0.1251 0.027 Uiso 1 1 calc R . . . .
C29 C 0.3126(4) 0.6948(4) 0.1208(3) 0.0270(12) Uani 1 1 d . . . . .
H29 H 0.2838 0.6944 0.0734 0.032 Uiso 1 1 calc R . . . .
C30 C 0.2948(5) 0.7591(4) 0.1594(3) 0.0301(13) Uani 1 1 d . . . . .
H30 H 0.2535 0.8025 0.1382 0.036 Uiso 1 1 calc R . . . .
C31 C 0.3369(5) 0.7604(3) 0.2284(3) 0.0287(13) Uani 1 1 d . . . . .
H31 H 0.3252 0.8046 0.2546 0.034 Uiso 1 1 calc R . . . .
C32 C 0.3968(4) 0.6962(3) 0.2593(3) 0.0233(11) Uani 1 1 d . . . . .
H32 H 0.4259 0.6969 0.3068 0.028 Uiso 1 1 calc R . . . .
C33 C 0.4092(4) 0.5179(3) 0.3239(2) 0.0161(9) Uani 1 1 d . . . . .
C34 C 0.2948(4) 0.5148(3) 0.3024(3) 0.0246(11) Uani 1 1 d . . . . .
H34 H 0.2618 0.5332 0.2584 0.029 Uiso 1 1 calc R . . . .
C35 C 0.2284(5) 0.4854(3) 0.3440(3) 0.0276(12) Uani 1 1 d . . . . .
H35 H 0.1505 0.4832 0.3285 0.033 Uiso 1 1 calc R . . . .
C36 C 0.2764(5) 0.4592(3) 0.4080(3) 0.0268(12) Uani 1 1 d . . . . .
H36 H 0.2311 0.4400 0.4371 0.032 Uiso 1 1 calc R . . . .
C37 C 0.3902(5) 0.4606(3) 0.4302(3) 0.0230(11) Uani 1 1 d . . . . .
H37 H 0.4230 0.4416 0.4740 0.028 Uiso 1 1 calc R . . . .
C38 C 0.4558(4) 0.4900(3) 0.3880(3) 0.0204(10) Uani 1 1 d . . . . .
H38 H 0.5338 0.4909 0.4032 0.025 Uiso 1 1 calc R . . . .
C51 C 0.5802(5) 0.2398(4) 0.5000(3) 0.0330(14) Uani 1 1 d . . . . .
C52 C 0.6157(5) 0.3006(4) 0.5452(3) 0.0292(13) Uani 1 1 d . . . . .
H52 H 0.5635 0.3369 0.5558 0.035 Uiso 1 1 calc R . . . .
C53 C 0.7269(6) 0.3088(4) 0.5747(3) 0.0370(15) Uani 1 1 d . . . . .
H53 H 0.7507 0.3504 0.6056 0.044 Uiso 1 1 calc R . . . .
C54 C 0.8019(5) 0.2569(5) 0.5593(4) 0.0403(16) Uani 1 1 d . . . . .
H54 H 0.8778 0.2622 0.5800 0.048 Uiso 1 1 calc R . . . .
C55 C 0.7690(5) 0.1973(4) 0.5141(3) 0.0334(14) Uani 1 1 d . . . . .
H55 H 0.8220 0.1619 0.5034 0.040 Uiso 1 1 calc R . . . .
C56 C 0.6597(5) 0.1890(4) 0.4846(3) 0.0365(15) Uani 1 1 d . . . . .
H56 H 0.6376 0.1478 0.4530 0.044 Uiso 1 1 calc R . . . .
C57 C 0.4593(6) 0.2294(6) 0.4701(4) 0.061(3) Uani 1 1 d . . . . .
H57A H 0.4195 0.2189 0.5064 0.091 Uiso 1 1 calc GR . . . .
H57B H 0.4493 0.1852 0.4383 0.091 Uiso 1 1 calc GR . . . .
H57C H 0.4302 0.2772 0.4459 0.091 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
Hf I1 2.7861(4) . ?
Hf I2 2.8229(4) . ?
Hf I3 2.8478(4) . ?
Hf P1 2.8465(13) . ?
Hf P2 2.7396(12) . ?
Hf N 2.048(4) . ?
Hf C3 2.612(5) . ?
P1 C1 1.848(5) . ?
P1 C8 1.830(5) . ?
P1 C14 1.832(5) . ?
P2 C20 1.838(5) . ?
P2 C27 1.819(5) . ?
P2 C33 1.839(5) . ?
N C3 1.448(6) . ?
N C22 1.412(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.504(7) . ?
C2 C3 1.403(7) . ?
C2 C7 1.402(7) . ?
C3 C4 1.400(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.394(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.384(8) . ?
C6 H6 0.9500 . ?
C6 C7 1.394(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.391(8) . ?
C8 C13 1.407(8) . ?
C9 H9 0.9500 . ?
C9 C10 1.404(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.375(9) . ?
C11 H11 0.9500 . ?
C11 C12 1.379(9) . ?
C12 H12 0.9500 . ?
C12 C13 1.385(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.404(8) . ?
C14 C19 1.376(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.395(8) . ?
C16 H16 0.9500 . ?
C16 C17 1.386(10) . ?
C17 H17 0.9500 . ?
C17 C18 1.379(10) . ?
C18 H18 0.9500 . ?
C18 C19 1.408(8) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.501(7) . ?
C21 C22 1.427(7) . ?
C21 C26 1.395(7) . ?
C22 C23 1.389(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.378(8) . ?
C24 H24 0.9500 . ?
C24 C25 1.371(9) . ?
C25 H25 0.9500 . ?
C25 C26 1.391(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.393(7) . ?
C27 C32 1.390(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.384(7) . ?
C29 H29 0.9500 . ?
C29 C30 1.388(9) . ?
C30 H30 0.9500 . ?
C30 C31 1.382(9) . ?
C31 H31 0.9500 . ?
C31 C32 1.395(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.393(7) . ?
C33 C38 1.387(7) . ?
C34 H34 0.9500 . ?
C34 C35 1.385(8) . ?
C35 H35 0.9500 . ?
C35 C36 1.379(8) . ?
C36 H36 0.9500 . ?
C36 C37 1.387(8) . ?
C37 H37 0.9500 . ?
C37 C38 1.386(7) . ?
C38 H38 0.9500 . ?
C51 C52 1.392(9) . ?
C51 C56 1.394(8) . ?
C51 C57 1.504(9) . ?
C52 H52 0.9500 . ?
C52 C53 1.390(9) . ?
C53 H53 0.9500 . ?
C53 C54 1.365(10) . ?
C54 H54 0.9500 . ?
C54 C55 1.369(10) . ?
C55 H55 0.9500 . ?
C55 C56 1.368(9) . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 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
I1 Hf I2 96.394(12) . . ?
I1 Hf I3 102.903(12) . . ?
I1 Hf P1 83.99(3) . . ?
I2 Hf I3 84.679(11) . . ?
I2 Hf P1 84.38(3) . . ?
P1 Hf I3 167.66(3) . . ?
P2 Hf I1 79.46(3) . . ?
P2 Hf I2 162.07(3) . . ?
P2 Hf I3 79.34(3) . . ?
P2 Hf P1 112.26(4) . . ?
N Hf I1 133.63(11) . . ?
N Hf I2 120.09(11) . . ?
N Hf I3 107.72(12) . . ?
N Hf P1 73.20(12) . . ?
N Hf P2 73.10(12) . . ?
N Hf C3 33.52(15) . . ?
C3 Hf I1 155.05(11) . . ?
C3 Hf I2 86.92(11) . . ?
C3 Hf I3 102.02(11) . . ?
C3 Hf P1 71.70(12) . . ?
C3 Hf P2 104.25(11) . . ?
C1 P1 Hf 102.35(17) . . ?
C8 P1 Hf 126.68(18) . . ?
C8 P1 C1 104.8(2) . . ?
C8 P1 C14 99.8(2) . . ?
C14 P1 Hf 115.63(16) . . ?
C14 P1 C1 105.7(2) . . ?
C20 P2 Hf 97.27(17) . . ?
C20 P2 C33 100.8(2) . . ?
C27 P2 Hf 123.25(17) . . ?
C27 P2 C20 106.5(2) . . ?
C27 P2 C33 102.0(2) . . ?
C33 P2 Hf 123.30(16) . . ?
C3 N Hf 95.1(3) . . ?
C22 N Hf 146.1(3) . . ?
C22 N C3 117.6(4) . . ?
P1 C1 H1A 109.8 . . ?
P1 C1 H1B 109.8 . . ?
H1A C1 H1B 108.3 . . ?
C2 C1 P1 109.2(4) . . ?
C2 C1 H1A 109.8 . . ?
C2 C1 H1B 109.8 . . ?
C3 C2 C1 119.7(4) . . ?
C7 C2 C1 121.5(5) . . ?
C7 C2 C3 118.8(5) . . ?
N C3 Hf 51.3(2) . . ?
C2 C3 Hf 110.3(3) . . ?
C2 C3 N 120.2(4) . . ?
C4 C3 Hf 103.8(3) . . ?
C4 C3 N 119.1(5) . . ?
C4 C3 C2 120.6(5) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.5(5) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 119.8 . . ?
C6 C5 C4 120.3(5) . . ?
C6 C5 H5 119.8 . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.4(5) . . ?
C7 C6 H6 119.8 . . ?
C2 C7 H7 119.8 . . ?
C6 C7 C2 120.3(5) . . ?
C6 C7 H7 119.8 . . ?
C9 C8 P1 120.6(4) . . ?
C9 C8 C13 119.1(5) . . ?
C13 C8 P1 120.2(4) . . ?
C8 C9 H9 119.9 . . ?
C8 C9 C10 120.1(5) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 120.2 . . ?
C11 C10 C9 119.6(6) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 119.5 . . ?
C10 C11 C12 121.1(5) . . ?
C12 C11 H11 119.5 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 119.9(6) . . ?
C13 C12 H12 120.0 . . ?
C8 C13 H13 119.9 . . ?
C12 C13 C8 120.2(6) . . ?
C12 C13 H13 119.9 . . ?
C15 C14 P1 116.4(4) . . ?
C19 C14 P1 124.2(4) . . ?
C19 C14 C15 119.3(5) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 C14 119.9(6) . . ?
C16 C15 H15 120.1 . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.2(6) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 119.9 . . ?
C18 C17 C16 120.2(6) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 H18 120.2 . . ?
C17 C18 C19 119.6(6) . . ?
C19 C18 H18 120.2 . . ?
C14 C19 C18 120.7(6) . . ?
C14 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
P2 C20 H20A 109.5 . . ?
P2 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
C21 C20 P2 110.7(3) . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
C22 C21 C20 122.7(4) . . ?
C26 C21 C20 119.5(5) . . ?
C26 C21 C22 117.8(5) . . ?
N C22 C21 120.8(4) . . ?
C23 C22 N 120.4(5) . . ?
C23 C22 C21 118.7(5) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 C22 121.2(5) . . ?
C24 C23 H23 119.4 . . ?
C23 C24 H24 119.2 . . ?
C25 C24 C23 121.5(6) . . ?
C25 C24 H24 119.2 . . ?
C24 C25 H25 121.0 . . ?
C24 C25 C26 118.0(5) . . ?
C26 C25 H25 121.0 . . ?
C21 C26 H26 118.6 . . ?
C25 C26 C21 122.7(5) . . ?
C25 C26 H26 118.6 . . ?
C28 C27 P2 122.3(4) . . ?
C32 C27 P2 118.5(4) . . ?
C32 C27 C28 119.2(5) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 C27 120.4(5) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 H29 120.0 . . ?
C28 C29 C30 120.0(5) . . ?
C30 C29 H29 120.0 . . ?
C29 C30 H30 119.8 . . ?
C31 C30 C29 120.4(5) . . ?
C31 C30 H30 119.8 . . ?
C30 C31 H31 120.3 . . ?
C30 C31 C32 119.5(6) . . ?
C32 C31 H31 120.3 . . ?
C27 C32 C31 120.5(5) . . ?
C27 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C34 C33 P2 119.5(4) . . ?
C38 C33 P2 121.8(4) . . ?
C38 C33 C34 118.5(5) . . ?
C33 C34 H34 119.4 . . ?
C35 C34 C33 121.3(5) . . ?
C35 C34 H34 119.4 . . ?
C34 C35 H35 120.4 . . ?
C36 C35 C34 119.3(5) . . ?
C36 C35 H35 120.4 . . ?
C35 C36 H36 119.7 . . ?
C35 C36 C37 120.6(5) . . ?
C37 C36 H36 119.7 . . ?
C36 C37 H37 120.2 . . ?
C38 C37 C36 119.6(5) . . ?
C38 C37 H37 120.2 . . ?
C33 C38 H38 119.6 . . ?
C37 C38 C33 120.9(5) . . ?
C37 C38 H38 119.6 . . ?
C52 C51 C56 118.0(6) . . ?
C52 C51 C57 120.3(6) . . ?
C56 C51 C57 121.8(6) . . ?
C51 C52 H52 119.8 . . ?
C53 C52 C51 120.4(6) . . ?
C53 C52 H52 119.8 . . ?
C52 C53 H53 120.1 . . ?
C54 C53 C52 119.8(6) . . ?
C54 C53 H53 120.1 . . ?
C53 C54 H54 119.6 . . ?
C53 C54 C55 120.7(6) . . ?
C55 C54 H54 119.6 . . ?
C54 C55 H55 120.1 . . ?
C56 C55 C54 119.9(6) . . ?
C56 C55 H55 120.1 . . ?
C51 C56 H56 119.4 . . ?
C55 C56 C51 121.2(6) . . ?
C55 C56 H56 119.4 . . ?
C51 C57 H57A 109.5 . . ?
C51 C57 H57B 109.5 . . ?
C51 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 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
Hf P1 C1 C2 -25.5(4) . . . . ?
Hf P1 C8 C9 -18.6(5) . . . . ?
Hf P1 C8 C13 163.2(4) . . . . ?
Hf P1 C14 C15 80.1(4) . . . . ?
Hf P1 C14 C19 -98.9(4) . . . . ?
Hf P2 C20 C21 75.4(4) . . . . ?
Hf P2 C27 C28 96.7(4) . . . . ?
Hf P2 C27 C32 -81.6(4) . . . . ?
Hf P2 C33 C34 -174.8(4) . . . . ?
Hf P2 C33 C38 -0.6(5) . . . . ?
Hf N C3 C2 -92.7(5) . . . . ?
Hf N C3 C4 84.6(5) . . . . ?
Hf N C22 C21 -7.4(9) . . . . ?
Hf N C22 C23 174.4(5) . . . . ?
Hf C3 C4 C5 -122.4(5) . . . . ?
P1 C1 C2 C3 59.6(6) . . . . ?
P1 C1 C2 C7 -119.6(5) . . . . ?
P1 C8 C9 C10 -177.5(4) . . . . ?
P1 C8 C13 C12 177.8(5) . . . . ?
P1 C14 C15 C16 -177.4(5) . . . . ?
P1 C14 C19 C18 178.7(4) . . . . ?
P2 C20 C21 C22 -46.3(6) . . . . ?
P2 C20 C21 C26 134.0(4) . . . . ?
P2 C27 C28 C29 -179.3(4) . . . . ?
P2 C27 C32 C31 179.2(4) . . . . ?
P2 C33 C34 C35 175.1(4) . . . . ?
P2 C33 C38 C37 -175.2(4) . . . . ?
N C3 C4 C5 -175.6(5) . . . . ?
N C22 C23 C24 -179.5(5) . . . . ?
C1 P1 C8 C9 -136.8(4) . . . . ?
C1 P1 C8 C13 45.0(5) . . . . ?
C1 P1 C14 C15 -167.6(4) . . . . ?
C1 P1 C14 C19 13.5(5) . . . . ?
C1 C2 C3 Hf -59.4(5) . . . . ?
C1 C2 C3 N -3.1(7) . . . . ?
C1 C2 C3 C4 179.7(5) . . . . ?
C1 C2 C7 C6 178.4(5) . . . . ?
C2 C3 C4 C5 1.7(8) . . . . ?
C3 N C22 C21 -170.8(4) . . . . ?
C3 N C22 C23 11.0(7) . . . . ?
C3 C2 C7 C6 -0.8(8) . . . . ?
C3 C4 C5 C6 -0.4(9) . . . . ?
C4 C5 C6 C7 -1.5(9) . . . . ?
C5 C6 C7 C2 2.1(9) . . . . ?
C7 C2 C3 Hf 119.9(4) . . . . ?
C7 C2 C3 N 176.1(5) . . . . ?
C7 C2 C3 C4 -1.1(8) . . . . ?
C8 P1 C1 C2 108.2(4) . . . . ?
C8 P1 C14 C15 -59.0(5) . . . . ?
C8 P1 C14 C19 122.1(5) . . . . ?
C8 C9 C10 C11 -0.1(9) . . . . ?
C9 C8 C13 C12 -0.4(9) . . . . ?
C9 C10 C11 C12 -0.7(9) . . . . ?
C10 C11 C12 C13 1.0(10) . . . . ?
C11 C12 C13 C8 -0.4(9) . . . . ?
C13 C8 C9 C10 0.7(8) . . . . ?
C14 P1 C1 C2 -146.9(4) . . . . ?
C14 P1 C8 C9 114.0(5) . . . . ?
C14 P1 C8 C13 -64.2(5) . . . . ?
C14 C15 C16 C17 -1.7(9) . . . . ?
C15 C14 C19 C18 -0.2(8) . . . . ?
C15 C16 C17 C18 0.5(10) . . . . ?
C16 C17 C18 C19 0.8(9) . . . . ?
C17 C18 C19 C14 -1.0(9) . . . . ?
C19 C14 C15 C16 1.5(8) . . . . ?
C20 P2 C27 C28 -13.9(5) . . . . ?
C20 P2 C27 C32 167.8(4) . . . . ?
C20 P2 C33 C34 -68.5(5) . . . . ?
C20 P2 C33 C38 105.6(4) . . . . ?
C20 C21 C22 N -0.3(7) . . . . ?
C20 C21 C22 C23 177.9(5) . . . . ?
C20 C21 C26 C25 -179.2(5) . . . . ?
C21 C22 C23 C24 2.2(8) . . . . ?
C22 N C3 Hf 170.8(5) . . . . ?
C22 N C3 C2 78.1(6) . . . . ?
C22 N C3 C4 -104.6(6) . . . . ?
C22 C21 C26 C25 1.0(8) . . . . ?
C22 C23 C24 C25 -0.7(9) . . . . ?
C23 C24 C25 C26 -0.6(9) . . . . ?
C24 C25 C26 C21 0.5(9) . . . . ?
C26 C21 C22 N 179.4(5) . . . . ?
C26 C21 C22 C23 -2.3(7) . . . . ?
C27 P2 C20 C21 -156.7(4) . . . . ?
C27 P2 C33 C34 41.1(5) . . . . ?
C27 P2 C33 C38 -144.7(4) . . . . ?
C27 C28 C29 C30 0.5(8) . . . . ?
C28 C27 C32 C31 0.8(8) . . . . ?
C28 C29 C30 C31 0.3(9) . . . . ?
C29 C30 C31 C32 -0.5(9) . . . . ?
C30 C31 C32 C27 0.0(8) . . . . ?
C32 C27 C28 C29 -1.0(8) . . . . ?
C33 P2 C20 C21 -50.7(4) . . . . ?
C33 P2 C27 C28 -119.2(4) . . . . ?
C33 P2 C27 C32 62.5(5) . . . . ?
C33 C34 C35 C36 0.4(9) . . . . ?
C34 C33 C38 C37 -1.0(8) . . . . ?
C34 C35 C36 C37 -1.4(9) . . . . ?
C35 C36 C37 C38 1.2(8) . . . . ?
C36 C37 C38 C33 0.0(8) . . . . ?
C38 C33 C34 C35 0.7(8) . . . . ?
C51 C52 C53 C54 0.2(10) . . . . ?
C52 C51 C56 C55 1.6(10) . . . . ?
C52 C53 C54 C55 0.9(11) . . . . ?
C53 C54 C55 C56 -0.7(11) . . . . ?
C54 C55 C56 C51 -0.6(11) . . . . ?
C56 C51 C52 C53 -1.4(10) . . . . ?
C57 C51 C52 C53 177.8(7) . . . . ?
C57 C51 C56 C55 -177.5(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            12.3761(2)
_cell_oxdiff_length_b            17.07238(16)
_cell_oxdiff_length_c            20.1630(3)
_cell_oxdiff_angle_alpha         90.0061(10)
_cell_oxdiff_angle_beta          101.9429(13)
_cell_oxdiff_angle_gamma         90.0098(11)
_cell_oxdiff_volume              4168.04(10)
_cell_oxdiff_measurement_reflns_used 38775
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
17 -3 -10 0.0292
14 -4 -21 0.0303
-3 -23 6 0.0431
-2 8 26 0.0366
-17 4 10 0.0259
2 -8 -27 0.0404
-15 -11 11 0.0382
1 4 -28 0.0296
-9 21 1 0.0337
3 22 -11 0.0299
4 -19 -17 0.0456
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
17.0146 -3.0043 -10.0102 0.0036 -0.1312 0.9863
14.0142 -4.0030 -21.0168 0.4600 -0.1093 0.8902
-3.0013 -23.0128 5.9986 -0.0148 -0.9661 -0.2056
-2.0063 8.0021 26.0188 -0.9160 0.2103 -0.2664
-17.0147 4.0048 10.0104 -0.0093 0.1723 -0.9861
2.0064 -8.0020 -27.0194 0.9511 -0.2054 0.2725
-15.0121 -11.0040 11.0069 -0.0015 -0.4567 -0.8868
1.0049 4.0051 -28.0168 0.9390 0.2968 0.2270
-9.0087 21.0135 1.0075 0.0379 0.8895 -0.4913
3.4745 22.0315 -11.4336 0.2010 0.9504 0.2643
4.1856 -19.0662 -17.0800 0.6186 -0.7159 0.3276
_oxdiff_exptl_absorpt_empirical_full_min 0.880
_oxdiff_exptl_absorpt_empirical_full_max 1.121
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_environment      perfluoro
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0214492000
_diffrn_orient_matrix_UB_12      -0.0057092000
_diffrn_orient_matrix_UB_13      -0.0351017000
_diffrn_orient_matrix_UB_21      -0.0032839000
_diffrn_orient_matrix_UB_22      0.0411518000
_diffrn_orient_matrix_UB_23      -0.0048286000
_diffrn_orient_matrix_UB_31      0.0544128000
_diffrn_orient_matrix_UB_32      0.0002419000
_diffrn_orient_matrix_UB_33      -0.0061178000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00  48.00   0.50   15.00    --   27.02 -57.00 -30.00  180
  2  ω     -3.00  97.00   0.50   15.00    --   27.02  77.00   0.00  200
  3  ω    -20.00  69.00   0.50   15.00    --   27.02 -99.00 -90.00  178
  4  ω    -20.00  69.00   0.50   15.00    --   27.02 -99.00  90.00  178
  5  ω    -45.00  53.00   0.50   15.00    --   27.02 -38.00-150.00  196
  6  ω      2.00  99.00   0.50   15.00    --   27.02  38.00-120.00  194
  7  ω    -42.00  48.00   0.50   15.00    --   27.02 -57.00 150.00  180
  8  ω     -3.00  97.00   0.50   15.00    --   27.02  77.00-180.00  200
  9  ω     -3.00  97.00   0.50   15.00    --   27.02  77.00 -90.00  200
 10  ω      7.00  96.00   0.50   15.00    --   27.02  57.00 120.00  178
 11  ω     -3.00  97.00   0.50   15.00    --   27.02  77.00  90.00  200
 12  ω    -20.00  31.00   0.50   15.00    --   27.02 -99.00 -30.00  102
 13  ω    -42.00  48.00   0.50   15.00    --   27.02 -57.00 120.00  180
;
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.8341 82672 36728 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.1659 0 36728 nmt 1.0139 -0.0003 0.0523 -0.0008 1.0020 0.0012 -0.1325
-0.0081 0.9748
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by 4.5797°
 around [-0.06 1.00 -0.00] (reciprocal) or [-0.12 0.99 -0.02] (direct)
Computed twin ratios:
Twin 1: 83.41% (11395 common observations, 1174 merged)
Twin 2: 16.59% (1872 common observations, 1174 merged)
;
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ba_sb64_sq
_database_code_depnum_ccdc_archive 'CCDC 1530467'
_audit_update_record             
;
2017-03-17 deposited with the CCDC.
2017-04-05 downloaded from the CCDC.
;
_audit_creation_date             2016-05-24

_audit_block_code                ba_sb64
_audit_block_refno               2723

_audit_creation_method           
;
Olex2 1.2
(compiled Mar  2 2017 14:00:58 for OlexSys, GUI svn.r5324)
;

# start Validation Reply Form
_vrf_CHEMW03_ba_sb64_sq          
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.95 <> 1.05
RESPONSE: see _platon_squeeze
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C41.75 H41 Cl3 N P2 Zr'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         816.26
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_diffrn_ambient_temperature      120(1)
_chemical_oxdiff_formula         'C41.75 H41 Cl3 N1 P2 Zr1'
_chemical_oxdiff_usercomment     'sb_dh36_2, irregular, yellow'
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'
Cl Cl 0.3639 0.7018 '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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 '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_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.44486(13)
_cell_length_b                   17.6843(2)
_cell_length_c                   19.9828(3)
_cell_angle_alpha                80.0131(11)
_cell_angle_beta                 88.4840(10)
_cell_angle_gamma                72.8933(10)
_cell_volume                     3805.61(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    111747
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.5070
_cell_measurement_theta_min      3.7360
_shelx_estimated_absorpt_T_max   0.618
_shelx_estimated_absorpt_T_min   0.618
_exptl_absorpt_coefficient_mu    5.332
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1678
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -6 9 0.0318
-1 9 9 0.0244
-2 5 -9 0.0649
7 3 4 0.0401
-7 -1 -5 0.0603
1 -9 -9 0.0244
-6 3 -1 0.0553
2 -5 -11 0.0492
0 -7 -11 0.0274
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.049
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0015 -5.9909 9.0131 -0.0327 -0.5044 0.8282
-0.9987 9.0050 8.9932 -1.0325 0.0568 -0.0363
-2.0007 4.9898 -9.0169 -0.0080 0.2718 -0.9578
6.9978 3.0073 4.0166 -0.0088 0.6846 0.7100
-6.9980 -1.0086 -5.0196 -0.0718 -0.5703 -0.8708
0.9987 -9.0050 -8.9932 1.0325 -0.0568 0.0363
-6.0000 2.9999 -1.0004 -0.4570 -0.4091 -0.7554
2.0000 -5.0000 -11.0000 0.9231 0.2669 -0.1950
0.0000 -7.0001 -11.0000 0.9453 -0.0095 -0.2730

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            219388
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.780
_diffrn_reflns_theta_min         3.764
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -72.00  26.00   1.00    1.00    --    0.00 -38.00 -60.00   98
  2  ω    -72.00  26.00   1.00    1.00    --    0.00 -38.00-150.00   98
  3  ω    -21.00  69.00   1.00    1.00    --    0.00  57.00 -90.00   90
  4  ω    -69.00  21.00   1.00    1.00    --    0.00 -57.00 120.00   90
  5  ω    -37.00  11.00   1.00    1.00    --   10.00 109.00 -14.08   48
  6  ω    -43.00  -1.00   1.00    1.00    --   14.00 124.00  30.85   42
  7  ω    -21.00  11.00   1.00    1.00    --   26.00 109.00 150.31   32
  8  ω    -21.00   6.00   1.00    4.00    --   30.00 115.00 -89.57   27
  9  ω     -9.00  18.00   1.00    4.00    --   34.00 101.00 103.10   27
 10  ω    -10.00  17.00   1.00    4.00    --   34.00 103.00  -1.18   27
 11  ω      5.00  32.00   1.00    4.00    --   42.00  90.00 -92.04   27
 12  ω      6.00  33.00   1.00    4.00    --   42.00  88.00  65.56   27
 13  ω     15.00  47.00   1.00    4.00    --   46.00  79.00-155.91   32
 14  ω     13.00  45.00   1.00    4.00    --   46.00  82.00  42.99   32
 15  ω     13.00  40.00   1.00    4.00    --   46.00  83.00 -44.93   27
 16  ω     13.00  45.00   1.00    4.00    --   46.00  82.00 115.72   32
 17  ω     13.00  40.00   1.00    4.00    --   46.00  83.00  86.22   27
 18  ω     13.00  45.00   1.00    4.00    --   46.00  82.00-110.75   32
 19  ω     13.00  45.00   1.00    4.00    --   46.00  82.00 -88.29   32
 20  ω     13.00  45.00   1.00    4.00    --   46.00  82.00 164.97   32
 21  ω     18.00  46.00   1.00    4.00    --   50.00  81.00  -5.69   28
 22  ω     19.00  49.00   1.00    4.00    --   50.00  78.00-146.91   30
 23  ω     18.00  46.00   1.00    4.00    --   50.00  80.00 173.78   28
 24  ω     19.00  49.00   1.00    4.00    --   50.00  78.00 -51.45   30
 25  ω     18.00  46.00   1.00    4.00    --   50.00  81.00 -94.71   28
 26  ω     18.00  46.00   1.00    4.00    --   50.00  80.00-149.72   28
 27  ω     24.00 124.00   1.00    4.00    --   54.00  77.00  23.31  100
 28  ω      1.00  96.00   1.00    4.00    --   54.00 -99.00 150.00   95
 29  ω    -15.00  75.00   1.00    4.00    --   54.00 -57.00 -90.00   90
 30  ω     23.00  49.00   1.00    4.00    --   54.00  78.00-120.28   26
 31  ω    -15.00  75.00   1.00    4.00    --   54.00 -57.00-180.00   90
 32  ω     25.00 124.00   1.00    4.00    --   54.00  75.00 143.51   99
 33  ω     27.00 123.00   1.00    4.00    --   54.00  72.00  87.46   96
 34  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 120.00  100
 35  ω     23.00 111.00   1.00    4.00    --   54.00-125.00  90.00   88
 36  ω     24.00 124.00   1.00    4.00    --   54.00  77.00  90.00  100
 37  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 150.00  100
 38  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 -90.00  100
 39  ω     23.00  49.00   1.00    4.00    --   54.00  78.00-178.76   26
 40  ω     24.00 124.00   1.00    4.00    --   54.00  77.00   0.00  100
 41  ω     29.00 128.00   1.00    4.00    --   58.00  76.00  37.06   99
 42  ω     29.00 128.00   1.00    4.00    --   58.00  76.00-122.19   99
 43  ω     30.00 128.00   1.00    4.00    --   58.00  74.00 -16.03   98
 44  ω     29.00 128.00   1.00    4.00    --   58.00  76.00 157.58   99
 45  ω     28.00 128.00   1.00    4.00    --   58.00  77.00  56.34  100
 46  ω     29.00 128.00   1.00    4.00    --   58.00  75.00-178.21   99
 47  ω     30.00 128.00   1.00    4.00    --   58.00  74.00-102.32   98
 48  ω     28.00 128.00   1.00    4.00    --   58.00  77.00 -77.28  100
 49  ω     29.00 128.00   1.00    4.00    --   58.00  75.00 -44.64   99
 50  ω     28.00 128.00   1.00    4.00    --   58.00  77.00  10.69  100
 51  ω     29.00 128.00   1.00    4.00    --   58.00  76.00-152.76   99
 52  ω     28.00 128.00   1.00    4.00    --   58.00  77.00 -60.32  100
 53  ω     34.00 131.00   1.00    4.00    --   62.00  73.00  85.64   97
 54  ω     33.00 132.00   1.00    4.00    --   62.00  75.00  93.39   99
 55  ω     34.00 132.00   1.00    4.00    --   62.00  74.00 -79.18   98
 56  ω     32.00 132.00   1.00    4.00    --   62.00  77.00 179.50  100
 57  ω     33.00 132.00   1.00    4.00    --   62.00  76.00   3.34   99
 58  ω     34.00 132.00   1.00    4.00    --   62.00  74.00 -49.00   98
 59  ω     33.00 132.00   1.00    4.00    --   62.00  76.00 123.54   99
 60  ω     39.00 135.00   1.00    4.00    --   66.00  72.00 -70.13   96
 61  ω     36.00 136.00   1.00    4.00    --   66.00  77.00 126.57  100
 62  ω     40.00 135.00   1.00    4.00    --   66.00  70.00  61.92   95
 63  ω     39.00 135.00   1.00    4.00    --   66.00  71.00 160.87   96
 64  ω     36.00 136.00   1.00    4.00    --   66.00  77.00-126.61  100
 65  ω     47.00 138.00   1.00    4.00    --   70.00  65.00 -29.88   91
 66  ω     46.00 138.00   1.00    4.00    --   70.00  67.00  89.68   92
 67  ω     43.00 139.00   1.00    4.00    --   70.00  71.00-141.14   96
 68  ω     40.00 140.00   1.00    4.00    --   70.00  77.00  28.11  100
 69  ω     44.00 144.00   1.00    4.00    --   74.00  77.00 -21.01  100
 70  ω     45.00 144.00   1.00    4.00    --   74.00  75.00 -96.59   99
 71  ω     47.00 143.00   1.00    4.00    --   74.00  72.00 -78.60   96
 72  ω     50.00 142.00   1.00    4.00    --   74.00  68.00-159.62   92
 73  ω     52.00 144.00   1.00    4.00    --   74.00  50.00  49.59   92
 74  ω     50.00 142.00   1.00    4.00    --   74.00  68.00 141.44   92
 75  ω     49.00 148.00   1.00    4.00    --   78.00  76.00  48.65   99
 76  ω     53.00 146.00   1.00    4.00    --   78.00  69.00-172.71   93
 77  ω     56.00 148.00   1.00    4.00    --   78.00  49.00 -78.07   92
 78  ω     55.00 146.00   1.00    4.00    --   78.00  66.00  -3.28   91
 79  ω     52.00 152.00   1.00    8.00    --   82.00  77.00  99.37  100
 80  ω     55.00 151.00   1.00    8.00    --   82.00  72.00 153.47   96
 81  ω     53.00 152.00   1.00    8.00    --   82.00  76.00  74.51   99
 82  ω     53.00 152.00   1.00    8.00    --   82.00  75.00 -67.00   99
 83  ω     58.00 156.00   1.00    8.00    --   86.00  74.00  68.50   98
 84  ω     65.00 154.00   1.00    8.00    --   86.00  60.00 108.12   89
 85  ω     64.00 154.00   1.00    8.00    --   86.00  61.00  45.84   90
 86  ω     56.00 156.00   1.00    8.00    --   86.00  77.00 140.45  100
 87  ω     62.00 154.00   1.00    8.00    --   86.00  67.00-124.16   92
 88  ω     63.00 159.00   1.00    8.00    --   90.00  71.00 -22.41   96
 89  ω     69.00 159.00   1.00    8.00    --   90.00  55.00 -22.27   90
 90  ω     62.00 160.00   1.00    8.00    --   90.00  74.00 -17.10   98
 91  ω     69.00 162.00   1.00    8.00    --   94.00  69.00 132.69   93
 92  ω     64.00 164.00   1.00    8.00    --   94.00  77.00  27.36  100
 93  ω     65.00 164.00   1.00    8.00    --   94.00  75.00-178.65   99
 94  ω     71.00 167.00   1.00    8.00    --   98.00  72.00 135.68   96
 95  ω     75.00 169.00   1.00    8.00    --   98.00  46.00 126.78   94
 96  ω     75.00 166.00   1.00    8.00    --   98.00  65.00 -52.84   91
 97  ω     81.00 172.00   1.00    8.00    --  102.00  53.00 101.91   91
 98  ω     75.00 171.00   1.00    8.00    --  102.00  72.00   3.67   96
 99  ω     85.00 176.00   1.00    8.00    --  106.00  53.00-109.96   91
100  ω     78.00 178.00   1.00    8.00    --  108.00  77.00 -30.00  100
101  ω     78.00 178.00   1.00    8.00    --  108.00  77.00  30.00  100
102  ω     78.00 178.00   1.00    8.00    --  108.00  77.00  90.00  100
103  ω     78.00 178.00   1.00    8.00    --  108.00  77.00 -60.00  100
104  ω     78.00 178.00   1.00    8.00    --  108.00  77.00-180.00  100
105  ω     78.00 178.00   1.00    8.00    --  108.00  77.00 -90.00  100
106  ω     78.00 178.00   1.00    8.00    --  108.00  77.00-150.00  100
107  ω     78.00 178.00   1.00    8.00    --  108.00  77.00 120.00  100
108  ω     78.00 178.00   1.00    8.00    --  108.00  77.00-120.00  100
109  ω     36.00 116.00   1.00    8.00    --  108.00-111.00-180.00   80
110  ω     78.00 178.00   1.00    8.00    --  108.00  77.00 150.00  100
111  ω     36.00 116.00   1.00    8.00    --  108.00-111.00   0.00   80
112  ω     85.00 175.00   1.00    8.00    --  108.00  64.00 -30.00   90
113  ω     78.00 178.00   1.00    8.00    --  108.00  77.00  60.00  100
114  ω    100.00 178.00   1.00    8.00    --  108.00 111.00 150.00   78
115  ω     41.00 131.00   1.00    8.00    --  108.00 -64.00  60.00   90
116  ω     36.00 146.00   1.00    8.00    --  108.00 -92.00-150.00  110
117  ω     36.00 116.00   1.00    8.00    --  108.00-111.00  90.00   80
118  ω     83.00 178.00   1.00    8.00    --  108.00  41.00 -61.88   95
119  ω     78.00 178.00   1.00    8.00    --  108.00  77.00  19.15  100
120  ω     82.00 178.00   1.00    8.00    --  108.00  38.00  90.00   96
121  ω     82.00 178.00   1.00    8.00    --  108.00  38.00 -90.00   96
122  ω     85.00 175.00   1.00    8.00    --  108.00  64.00 120.00   90
123  ω     85.00 175.00   1.00    8.00    --  108.00  64.00 -60.00   90
124  ω     85.00 175.00   1.00    8.00    --  108.00  64.00-150.00   90
125  ω     85.00 175.00   1.00    8.00    --  108.00  64.00-180.00   90
126  ω     85.00 175.00   1.00    8.00    --  108.00  64.00  90.00   90
127  ω     85.00 175.00   1.00    8.00    --  108.00  64.00 -90.00   90
128  ω     82.00 178.00   1.00    8.00    --  108.00  38.00-120.00   96
129  ω     85.00 175.00   1.00    8.00    --  108.00  64.00 150.00   90
130  ω     78.00 178.00   1.00    8.00    --  108.00  77.00   0.00  100
131  ω     85.00 175.00   1.00    8.00    --  108.00  64.00-120.00   90
132  ω     38.00 138.00   1.00    8.00    --  108.00 -77.00-120.00  100
133  φ    120.00 240.00   1.00    1.00   0.00   0.00 -60.00    --   120
134  φ      0.00 120.00   1.00    1.00   0.00   0.00  60.00    --   120
135  φ    240.00 360.00   1.00    1.00   0.00   0.00 -40.00    --   120
136  φ    120.00 240.00   1.00    1.00   0.00   0.00  60.00    --   120
137  φ      0.00 120.00   1.00    1.00   0.00   0.00 -60.00    --   120
138  φ    120.00 240.00   1.00    1.00   0.00   0.00  40.00    --   120
139  φ      0.00 120.00   1.00    1.00   0.00   0.00  40.00    --   120
140  φ      0.00 120.00   1.00    1.00   0.00   0.00 -40.00    --   120
141  φ    120.00 240.00   1.00    1.00   0.00   0.00 -40.00    --   120
142  φ    120.00 240.00   1.00    4.00  54.00  54.00 -40.00    --   120
143  φ      0.00 120.00   1.00    4.00  54.00  54.00  60.00    --   120
144  φ      0.00 120.00   1.00    4.00  54.00  54.00 -60.00    --   120
145  φ      0.00 120.00   1.00    4.00  54.00  54.00  40.00    --   120
146  φ    120.00 240.00   1.00    4.00  54.00  54.00  40.00    --   120
147  φ      0.00 120.00   1.00    4.00  54.00  54.00 -40.00    --   120
148  φ    240.00 355.00   1.00    4.00  54.00  54.00 -40.00    --   115
149  φ    120.00 240.00   1.00    4.00  54.00  54.00  60.00    --   120
150  φ    120.00 240.00   1.00    4.00  54.00  54.00 -60.00    --   120
151  φ      0.00 270.00   1.00    0.50   0.00   0.00   0.00    --   270
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0521505000
_diffrn_orient_matrix_UB_12      -0.0632522000
_diffrn_orient_matrix_UB_13      -0.0456826000
_diffrn_orient_matrix_UB_21      0.0945141000
_diffrn_orient_matrix_UB_22      0.0436883000
_diffrn_orient_matrix_UB_23      -0.0269369000
_diffrn_orient_matrix_UB_31      0.0905335000
_diffrn_orient_matrix_UB_32      -0.0515339000
_diffrn_orient_matrix_UB_33      0.0576152000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13711
_reflns_number_total             14522
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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,
 see _platon_squeeze_.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2016/6
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         14522
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0251
_refine_ls_restrained_S_all      1.053
_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)+(0.0253P)²+3.0191P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0611
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C20(H20A,H20B), C51(H51A,H51B), C70(H70A,H70B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C54(H54), C55(H55), C56(H56),
  C57(H57), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65),
 C66(H66), C67(H67), C68(H68), C69(H69), C73(H73), C74(H74), C75(H75), C76(H76),
  C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C84(H84), C85(H85),
 C86(H86), C87(H87), C88(H88)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Zr1 Zr 0.87043(2) 0.49915(2) 0.26771(2) 0.02193(4) Uani 1 1 d . . . . .
Cl1 Cl 1.02663(4) 0.52229(3) 0.33632(2) 0.02608(9) Uani 1 1 d . . . . .
Cl2 Cl 0.82333(4) 0.63321(3) 0.20026(2) 0.02980(10) Uani 1 1 d . . . . .
Cl3 Cl 1.02935(4) 0.42592(3) 0.19745(2) 0.03401(11) Uani 1 1 d . . . . .
P1 P 0.72773(4) 0.48001(3) 0.16224(2) 0.02425(10) Uani 1 1 d . . . . .
P2 P 0.92044(4) 0.34820(3) 0.35577(2) 0.02414(10) Uani 1 1 d . . . . .
N1 N 0.70131(14) 0.50542(9) 0.31263(8) 0.0247(3) Uani 1 1 d . . . . .
C1 C 0.57307(17) 0.53606(12) 0.18209(10) 0.0274(4) Uani 1 1 d . . . . .
H1A H 0.571608 0.591553 0.185345 0.033 Uiso 1 1 calc R . . . .
H1B H 0.516491 0.539217 0.144383 0.033 Uiso 1 1 calc R . . . .
C2 C 0.52809(17) 0.49879(11) 0.24752(10) 0.0264(4) Uani 1 1 d . . . . .
C3 C 0.58574(16) 0.49194(11) 0.31049(10) 0.0249(4) Uani 1 1 d . . . . .
C4 C 0.52480(18) 0.47330(12) 0.36999(11) 0.0302(4) Uani 1 1 d . . . . .
H4 H 0.559524 0.472091 0.412961 0.036 Uiso 1 1 calc R . . . .
C5 C 0.41382(18) 0.45655(12) 0.36667(12) 0.0349(5) Uani 1 1 d . . . . .
H5 H 0.373005 0.444657 0.407381 0.042 Uiso 1 1 calc R . . . .
C6 C 0.36261(18) 0.45705(13) 0.30490(12) 0.0361(5) Uani 1 1 d . . . . .
H6 H 0.289254 0.442642 0.302897 0.043 Uiso 1 1 calc R . . . .
C7 C 0.41947(18) 0.47882(12) 0.24585(11) 0.0317(4) Uani 1 1 d . . . . .
H7 H 0.383538 0.480173 0.203175 0.038 Uiso 1 1 calc R . . . .
C8 C 0.71742(18) 0.38444(11) 0.14409(10) 0.0269(4) Uani 1 1 d . . . . .
C9 C 0.82174(19) 0.31835(12) 0.15148(10) 0.0306(4) Uani 1 1 d . . . . .
H9 H 0.895042 0.321785 0.170236 0.037 Uiso 1 1 calc R . . . .
C10 C 0.8189(2) 0.24764(12) 0.13156(11) 0.0347(5) Uani 1 1 d . . . . .
H10 H 0.890799 0.203147 0.136072 0.042 Uiso 1 1 calc R . . . .
C11 C 0.7131(2) 0.24127(13) 0.10534(11) 0.0382(5) Uani 1 1 d . . . . .
H11 H 0.711329 0.192365 0.092464 0.046 Uiso 1 1 calc R . . . .
C12 C 0.6097(2) 0.30639(15) 0.09786(13) 0.0464(6) Uani 1 1 d . . . . .
H12 H 0.536524 0.302326 0.079417 0.056 Uiso 1 1 calc R . . . .
C13 C 0.6112(2) 0.37766(14) 0.11696(13) 0.0403(5) Uani 1 1 d . . . . .
H13 H 0.539316 0.422160 0.111482 0.048 Uiso 1 1 calc R . . . .
C14 C 0.74952(18) 0.53013(12) 0.07690(10) 0.0278(4) Uani 1 1 d . . . . .
C15 C 0.8362(2) 0.48910(13) 0.03588(11) 0.0343(5) Uani 1 1 d . . . . .
H15 H 0.884450 0.435678 0.052625 0.041 Uiso 1 1 calc R . . . .
C16 C 0.8530(2) 0.52546(13) -0.02932(11) 0.0392(5) Uani 1 1 d . . . . .
H16 H 0.912359 0.496792 -0.057147 0.047 Uiso 1 1 calc R . . . .
C17 C 0.7837(2) 0.60345(14) -0.05415(11) 0.0392(5) Uani 1 1 d . . . . .
H17 H 0.794169 0.627973 -0.099200 0.047 Uiso 1 1 calc R . . . .
C18 C 0.6997(2) 0.64512(14) -0.01324(11) 0.0385(5) Uani 1 1 d . . . . .
H18 H 0.653446 0.699100 -0.029700 0.046 Uiso 1 1 calc R . . . .
C19 C 0.6820(2) 0.60876(13) 0.05205(11) 0.0350(5) Uani 1 1 d . . . . .
H19 H 0.623297 0.637903 0.079889 0.042 Uiso 1 1 calc R . . . .
C20 C 0.81465(18) 0.37526(11) 0.42485(10) 0.0279(4) Uani 1 1 d . . . . .
H20A H 0.735357 0.366668 0.415628 0.033 Uiso 1 1 calc R . . . .
H20B H 0.849130 0.340762 0.468476 0.033 Uiso 1 1 calc R . . . .
C21 C 0.79564(16) 0.46195(11) 0.42951(10) 0.0249(4) Uani 1 1 d . . . . .
C22 C 0.73847(16) 0.52317(11) 0.37534(9) 0.0237(4) Uani 1 1 d . . . . .
C23 C 0.72331(17) 0.60338(12) 0.37944(10) 0.0288(4) Uani 1 1 d . . . . .
H23 H 0.683591 0.644536 0.343132 0.035 Uiso 1 1 calc R . . . .
C24 C 0.7659(2) 0.62332(13) 0.43620(11) 0.0344(5) Uani 1 1 d . . . . .
H24 H 0.755414 0.678047 0.438804 0.041 Uiso 1 1 calc R . . . .
C25 C 0.82371(19) 0.56344(13) 0.48909(11) 0.0344(5) Uani 1 1 d . . . . .
H25 H 0.853812 0.577047 0.527797 0.041 Uiso 1 1 calc R . . . .
C26 C 0.83788(18) 0.48340(13) 0.48574(10) 0.0303(4) Uani 1 1 d . . . . .
H26 H 0.877095 0.442763 0.522516 0.036 Uiso 1 1 calc R . . . .
C27 C 0.87978(18) 0.26534(11) 0.32931(10) 0.0266(4) Uani 1 1 d . . . . .
C28 C 0.9684(2) 0.19482(12) 0.32047(11) 0.0352(5) Uani 1 1 d . . . . .
H28 H 1.052290 0.188710 0.328956 0.042 Uiso 1 1 calc R . . . .
C29 C 0.9343(2) 0.13329(13) 0.29921(13) 0.0445(6) Uani 1 1 d . . . . .
H29 H 0.995020 0.085310 0.293049 0.053 Uiso 1 1 calc R . . . .
C30 C 0.8131(2) 0.14173(14) 0.28711(12) 0.0447(6) Uani 1 1 d . . . . .
H30 H 0.790096 0.099105 0.273538 0.054 Uiso 1 1 calc R . . . .
C31 C 0.7244(2) 0.21213(14) 0.29463(11) 0.0390(5) Uani 1 1 d . . . . .
H31 H 0.640808 0.217976 0.285737 0.047 Uiso 1 1 calc R . . . .
C32 C 0.75754(19) 0.27401(13) 0.31509(10) 0.0316(4) Uani 1 1 d . . . . .
H32 H 0.696646 0.322614 0.319452 0.038 Uiso 1 1 calc R . . . .
C33 C 1.06995(18) 0.29992(12) 0.39711(11) 0.0300(4) Uani 1 1 d . . . . .
C34 C 1.0845(2) 0.24631(14) 0.45811(12) 0.0414(5) Uani 1 1 d . . . . .
H34 H 1.014831 0.235742 0.480007 0.050 Uiso 1 1 calc R . . . .
C35 C 1.1996(2) 0.20825(16) 0.48715(13) 0.0491(6) Uani 1 1 d . . . . .
H35 H 1.208737 0.171598 0.528834 0.059 Uiso 1 1 calc R . . . .
C36 C 1.3013(2) 0.22317(16) 0.45597(14) 0.0505(6) Uani 1 1 d . . . . .
H36 H 1.380432 0.196675 0.475877 0.061 Uiso 1 1 calc R . . . .
C37 C 1.2877(2) 0.27645(15) 0.39609(14) 0.0467(6) Uani 1 1 d . . . . .
H37 H 1.357609 0.287387 0.374882 0.056 Uiso 1 1 calc R . . . .
C38 C 1.17269(19) 0.31459(13) 0.36613(12) 0.0365(5) Uani 1 1 d . . . . .
H38 H 1.164409 0.350845 0.324259 0.044 Uiso 1 1 calc R . . . .
Zr51 Zr 0.36337(2) 0.87653(2) 0.21636(2) 0.02036(4) Uani 1 1 d . . . . .
Cl51 Cl 0.45371(4) 0.97937(3) 0.16029(2) 0.02701(10) Uani 1 1 d . . . . .
Cl52 Cl 0.54267(4) 0.80098(3) 0.28622(3) 0.03158(10) Uani 1 1 d . . . . .
Cl53 Cl 0.25743(4) 0.96658(3) 0.29421(2) 0.03022(10) Uani 1 1 d . . . . .
P51 P 0.24895(4) 0.77942(3) 0.30446(2) 0.02264(10) Uani 1 1 d . . . . .
P52 P 0.16829(4) 0.96077(3) 0.12254(2) 0.02033(9) Uani 1 1 d . . . . .
N51 N 0.35744(13) 0.78844(9) 0.15985(8) 0.0218(3) Uani 1 1 d . . . . .
C51 C 0.30297(18) 0.68226(11) 0.27666(10) 0.0277(4) Uani 1 1 d . . . . .
H51A H 0.393460 0.663894 0.279461 0.033 Uiso 1 1 calc R . . . .
H51B H 0.273014 0.642629 0.308069 0.033 Uiso 1 1 calc R . . . .
C52 C 0.26186(17) 0.68429(11) 0.20542(10) 0.0259(4) Uani 1 1 d . . . . .
C53 C 0.30213(16) 0.72983(10) 0.14908(10) 0.0233(4) Uani 1 1 d . . . . .
C54 C 0.28468(18) 0.71508(11) 0.08420(10) 0.0279(4) Uani 1 1 d . . . . .
H54 H 0.319391 0.740547 0.046406 0.033 Uiso 1 1 calc R . . . .
C55 C 0.2179(2) 0.66413(12) 0.07374(11) 0.0341(5) Uani 1 1 d . . . . .
H55 H 0.207182 0.654939 0.029168 0.041 Uiso 1 1 calc R . . . .
C56 C 0.1667(2) 0.62661(13) 0.12839(12) 0.0378(5) Uani 1 1 d . . . . .
H56 H 0.115455 0.594955 0.121294 0.045 Uiso 1 1 calc R . . . .
C57 C 0.19117(19) 0.63584(12) 0.19338(11) 0.0330(5) Uani 1 1 d . . . . .
H57 H 0.158770 0.608296 0.230926 0.040 Uiso 1 1 calc R . . . .
C58 C 0.08412(17) 0.80067(11) 0.31232(9) 0.0245(4) Uani 1 1 d . . . . .
C59 C 0.01212(18) 0.87933(12) 0.31236(10) 0.0285(4) Uani 1 1 d . . . . .
H59 H 0.048967 0.921585 0.306702 0.034 Uiso 1 1 calc R . . . .
C60 C -0.11341(19) 0.89629(13) 0.32065(11) 0.0340(5) Uani 1 1 d . . . . .
H60 H -0.161786 0.949798 0.321993 0.041 Uiso 1 1 calc R . . . .
C61 C -0.16791(19) 0.83527(15) 0.32694(11) 0.0380(5) Uani 1 1 d . . . . .
H61 H -0.253911 0.847070 0.331708 0.046 Uiso 1 1 calc R . . . .
C62 C -0.0976(2) 0.75739(14) 0.32630(11) 0.0385(5) Uani 1 1 d . . . . .
H62 H -0.135272 0.715666 0.330160 0.046 Uiso 1 1 calc R . . . .
C63 C 0.02782(19) 0.73978(13) 0.32005(10) 0.0323(4) Uani 1 1 d . . . . .
H63 H 0.076010 0.685720 0.321023 0.039 Uiso 1 1 calc R . . . .
C64 C 0.30363(18) 0.75929(12) 0.39273(10) 0.0286(4) Uani 1 1 d . . . . .
C65 C 0.2428(2) 0.80803(14) 0.43784(11) 0.0413(5) Uani 1 1 d . . . . .
H65 H 0.169419 0.849523 0.423578 0.050 Uiso 1 1 calc R . . . .
C66 C 0.2884(3) 0.79660(17) 0.50372(12) 0.0500(6) Uani 1 1 d . . . . .
H66 H 0.246173 0.830296 0.534263 0.060 Uiso 1 1 calc R . . . .
C67 C 0.3942(2) 0.73693(18) 0.52487(12) 0.0496(7) Uani 1 1 d . . . . .
H67 H 0.425427 0.729355 0.569902 0.059 Uiso 1 1 calc R . . . .
C68 C 0.4541(2) 0.68866(19) 0.48116(12) 0.0547(7) Uani 1 1 d . . . . .
H68 H 0.527408 0.647345 0.495873 0.066 Uiso 1 1 calc R . . . .
C69 C 0.4093(2) 0.69898(16) 0.41503(11) 0.0432(6) Uani 1 1 d . . . . .
H69 H 0.451695 0.664387 0.385167 0.052 Uiso 1 1 calc R . . . .
C70 C 0.22335(16) 0.91267(11) 0.04780(9) 0.0231(4) Uani 1 1 d . . . . .
H70A H 0.187358 0.868319 0.046980 0.028 Uiso 1 1 calc R . . . .
H70B H 0.196371 0.952502 0.005673 0.028 Uiso 1 1 calc R . . . .
C71 C 0.36107(16) 0.88013(11) 0.05014(9) 0.0224(4) Uani 1 1 d . . . . .
C72 C 0.42238(16) 0.81965(11) 0.10406(9) 0.0222(4) Uani 1 1 d . . . . .
C73 C 0.55026(17) 0.79285(11) 0.10750(10) 0.0268(4) Uani 1 1 d . . . . .
H73 H 0.591166 0.752527 0.144058 0.032 Uiso 1 1 calc R . . . .
C74 C 0.61763(18) 0.82494(12) 0.05771(11) 0.0317(4) Uani 1 1 d . . . . .
H74 H 0.704458 0.806706 0.060297 0.038 Uiso 1 1 calc R . . . .
C75 C 0.55824(18) 0.88345(12) 0.00438(10) 0.0317(4) Uani 1 1 d . . . . .
H75 H 0.604368 0.904947 -0.029962 0.038 Uiso 1 1 calc R . . . .
C76 C 0.43097(18) 0.91099(11) 0.00082(10) 0.0274(4) Uani 1 1 d . . . . .
H76 H 0.391197 0.951531 -0.035882 0.033 Uiso 1 1 calc R . . . .
C77 C 0.13876(16) 1.06851(11) 0.09363(10) 0.0228(4) Uani 1 1 d . . . . .
C78 C 0.08800(17) 1.10622(11) 0.02943(10) 0.0268(4) Uani 1 1 d . . . . .
H78 H 0.069531 1.075221 -0.000886 0.032 Uiso 1 1 calc R . . . .
C79 C 0.06418(18) 1.18849(12) 0.00935(11) 0.0308(4) Uani 1 1 d . . . . .
H79 H 0.028835 1.213642 -0.034363 0.037 Uiso 1 1 calc R . . . .
C80 C 0.09180(19) 1.23384(12) 0.05283(12) 0.0346(5) Uani 1 1 d . . . . .
H80 H 0.075986 1.290155 0.038934 0.042 Uiso 1 1 calc R . . . .
C81 C 0.1424(2) 1.19737(12) 0.11658(12) 0.0375(5) Uani 1 1 d . . . . .
H81 H 0.161561 1.228711 0.146386 0.045 Uiso 1 1 calc R . . . .
C82 C 0.16559(18) 1.11484(12) 0.13735(11) 0.0305(4) Uani 1 1 d . . . . .
H82 H 0.199718 1.090132 0.181397 0.037 Uiso 1 1 calc R . . . .
C83 C 0.01658(16) 0.94737(11) 0.13510(9) 0.0213(4) Uani 1 1 d . . . . .
C84 C -0.08817(17) 1.01133(11) 0.13888(9) 0.0248(4) Uani 1 1 d . . . . .
H84 H -0.082102 1.064472 0.133544 0.030 Uiso 1 1 calc R . . . .
C85 C -0.20114(17) 0.99786(12) 0.15038(10) 0.0290(4) Uani 1 1 d . . . . .
H85 H -0.271861 1.041857 0.152680 0.035 Uiso 1 1 calc R . . . .
C86 C -0.21141(17) 0.92065(12) 0.15852(10) 0.0296(4) Uani 1 1 d . . . . .
H86 H -0.288978 0.911701 0.165883 0.036 Uiso 1 1 calc R . . . .
C87 C -0.10771(18) 0.85655(12) 0.15585(10) 0.0275(4) Uani 1 1 d . . . . .
H87 H -0.114161 0.803473 0.161684 0.033 Uiso 1 1 calc R . . . .
C88 C 0.00522(17) 0.86968(11) 0.14470(9) 0.0239(4) Uani 1 1 d . . . . .
H88 H 0.075894 0.825297 0.143561 0.029 Uiso 1 1 calc R . . . .


_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
Zr1 Cl1 2.4490(5) . ?
Zr1 Cl2 2.4302(5) . ?
Zr1 Cl3 2.4630(5) . ?
Zr1 P1 2.8245(5) . ?
Zr1 P2 2.8417(5) . ?
Zr1 N1 2.0930(15) . ?
Zr1 C22 2.6182(17) . ?
P1 C1 1.8276(19) . ?
P1 C8 1.8260(19) . ?
P1 C14 1.827(2) . ?
P2 C20 1.8440(19) . ?
P2 C27 1.8237(19) . ?
P2 C33 1.819(2) . ?
N1 C3 1.414(2) . ?
N1 C22 1.447(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.508(3) . ?
C2 C3 1.406(3) . ?
C2 C7 1.391(3) . ?
C3 C4 1.401(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.392(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.378(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.383(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.393(3) . ?
C8 C13 1.389(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.386(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.374(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.378(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.384(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(3) . ?
C14 C19 1.388(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.384(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.385(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.373(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.389(3) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.503(3) . ?
C21 C22 1.409(3) . ?
C21 C26 1.387(3) . ?
C22 C23 1.394(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.385(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.383(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.390(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.392(3) . ?
C27 C32 1.393(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.391(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.375(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.384(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.384(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.389(3) . ?
C33 C38 1.385(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.382(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.377(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.370(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.387(3) . ?
C38 H38 0.9500 . ?
Zr51 Cl51 2.4434(4) . ?
Zr51 Cl52 2.4160(5) . ?
Zr51 Cl53 2.4597(5) . ?
Zr51 P51 2.8135(5) . ?
Zr51 P52 2.8311(5) . ?
Zr51 N51 2.0934(15) . ?
Zr51 C72 2.6089(18) . ?
P51 C51 1.8250(19) . ?
P51 C58 1.8200(19) . ?
P51 C64 1.827(2) . ?
P52 C70 1.8512(19) . ?
P52 C77 1.8243(18) . ?
P52 C83 1.8255(18) . ?
N51 C53 1.411(2) . ?
N51 C72 1.444(2) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 C52 1.502(3) . ?
C52 C53 1.416(3) . ?
C52 C57 1.391(3) . ?
C53 C54 1.396(3) . ?
C54 H54 0.9500 . ?
C54 C55 1.385(3) . ?
C55 H55 0.9500 . ?
C55 C56 1.385(3) . ?
C56 H56 0.9500 . ?
C56 C57 1.383(3) . ?
C57 H57 0.9500 . ?
C58 C59 1.393(3) . ?
C58 C63 1.394(3) . ?
C59 H59 0.9500 . ?
C59 C60 1.390(3) . ?
C60 H60 0.9500 . ?
C60 C61 1.384(3) . ?
C61 H61 0.9500 . ?
C61 C62 1.378(3) . ?
C62 H62 0.9500 . ?
C62 C63 1.383(3) . ?
C63 H63 0.9500 . ?
C64 C65 1.387(3) . ?
C64 C69 1.380(3) . ?
C65 H65 0.9500 . ?
C65 C66 1.389(3) . ?
C66 H66 0.9500 . ?
C66 C67 1.370(4) . ?
C67 H67 0.9500 . ?
C67 C68 1.358(4) . ?
C68 H68 0.9500 . ?
C68 C69 1.392(3) . ?
C69 H69 0.9500 . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C70 C71 1.509(2) . ?
C71 C72 1.413(3) . ?
C71 C76 1.392(2) . ?
C72 C73 1.399(3) . ?
C73 H73 0.9500 . ?
C73 C74 1.388(3) . ?
C74 H74 0.9500 . ?
C74 C75 1.382(3) . ?
C75 H75 0.9500 . ?
C75 C76 1.393(3) . ?
C76 H76 0.9500 . ?
C77 C78 1.394(3) . ?
C77 C82 1.393(3) . ?
C78 H78 0.9500 . ?
C78 C79 1.386(3) . ?
C79 H79 0.9500 . ?
C79 C80 1.380(3) . ?
C80 H80 0.9500 . ?
C80 C81 1.382(3) . ?
C81 H81 0.9500 . ?
C81 C82 1.393(3) . ?
C82 H82 0.9500 . ?
C83 C84 1.396(3) . ?
C83 C88 1.398(3) . ?
C84 H84 0.9500 . ?
C84 C85 1.388(3) . ?
C85 H85 0.9500 . ?
C85 C86 1.386(3) . ?
C86 H86 0.9500 . ?
C86 C87 1.386(3) . ?
C87 H87 0.9500 . ?
C87 C88 1.385(3) . ?
C88 H88 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Zr1 Cl3 90.696(16) . . ?
Cl1 Zr1 P1 165.968(15) . . ?
Cl1 Zr1 P2 85.031(15) . . ?
Cl1 Zr1 C22 83.15(4) . . ?
Cl2 Zr1 Cl1 92.650(16) . . ?
Cl2 Zr1 Cl3 99.654(17) . . ?
Cl2 Zr1 P1 80.486(15) . . ?
Cl2 Zr1 P2 175.489(16) . . ?
Cl2 Zr1 C22 102.62(4) . . ?
Cl3 Zr1 P1 78.533(16) . . ?
Cl3 Zr1 P2 84.263(16) . . ?
Cl3 Zr1 C22 157.12(4) . . ?
P1 Zr1 P2 102.595(14) . . ?
N1 Zr1 Cl1 116.62(5) . . ?
N1 Zr1 Cl2 99.87(4) . . ?
N1 Zr1 Cl3 145.36(4) . . ?
N1 Zr1 P1 76.83(4) . . ?
N1 Zr1 P2 77.81(4) . . ?
N1 Zr1 C22 33.47(6) . . ?
C22 Zr1 P1 110.21(4) . . ?
C22 Zr1 P2 73.28(4) . . ?
C1 P1 Zr1 102.48(7) . . ?
C8 P1 Zr1 125.76(7) . . ?
C8 P1 C1 106.13(9) . . ?
C8 P1 C14 100.65(9) . . ?
C14 P1 Zr1 116.12(6) . . ?
C14 P1 C1 103.47(9) . . ?
C20 P2 Zr1 100.57(6) . . ?
C27 P2 Zr1 120.13(6) . . ?
C27 P2 C20 103.86(9) . . ?
C33 P2 Zr1 121.15(7) . . ?
C33 P2 C20 105.47(9) . . ?
C33 P2 C27 103.39(9) . . ?
C3 N1 Zr1 148.39(13) . . ?
C3 N1 C22 117.39(14) . . ?
C22 N1 Zr1 93.61(10) . . ?
P1 C1 H1A 109.0 . . ?
P1 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 P1 113.13(13) . . ?
C2 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
C3 C2 C1 121.57(17) . . ?
C7 C2 C1 118.61(18) . . ?
C7 C2 C3 119.45(18) . . ?
C2 C3 N1 119.94(16) . . ?
C4 C3 N1 121.65(18) . . ?
C4 C3 C2 118.40(17) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.6(2) . . ?
C5 C4 H4 119.7 . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.62(19) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 H6 120.5 . . ?
C5 C6 C7 119.09(19) . . ?
C7 C6 H6 120.5 . . ?
C2 C7 H7 119.2 . . ?
C6 C7 C2 121.5(2) . . ?
C6 C7 H7 119.2 . . ?
C9 C8 P1 119.32(15) . . ?
C13 C8 P1 121.66(16) . . ?
C13 C8 C9 118.73(19) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.2(2) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 119.7 . . ?
C11 C10 C9 120.6(2) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 H11 120.3 . . ?
C10 C11 C12 119.5(2) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 H12 119.7 . . ?
C11 C12 C13 120.6(2) . . ?
C13 C12 H12 119.7 . . ?
C8 C13 H13 119.8 . . ?
C12 C13 C8 120.3(2) . . ?
C12 C13 H13 119.8 . . ?
C15 C14 P1 119.46(16) . . ?
C15 C14 C19 118.87(19) . . ?
C19 C14 P1 121.67(15) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 C14 120.5(2) . . ?
C16 C15 H15 119.8 . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.3(2) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 120.2 . . ?
C18 C17 C16 119.6(2) . . ?
C18 C17 H17 120.2 . . ?
C17 C18 H18 119.8 . . ?
C17 C18 C19 120.3(2) . . ?
C19 C18 H18 119.8 . . ?
C14 C19 C18 120.4(2) . . ?
C14 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
P2 C20 H20A 109.8 . . ?
P2 C20 H20B 109.8 . . ?
H20A C20 H20B 108.3 . . ?
C21 C20 P2 109.23(12) . . ?
C21 C20 H20A 109.8 . . ?
C21 C20 H20B 109.8 . . ?
C22 C21 C20 120.37(17) . . ?
C26 C21 C20 121.03(18) . . ?
C26 C21 C22 118.56(18) . . ?
N1 C22 Zr1 52.92(8) . . ?
C21 C22 Zr1 107.55(11) . . ?
C21 C22 N1 121.90(16) . . ?
C23 C22 Zr1 104.45(12) . . ?
C23 C22 N1 117.89(17) . . ?
C23 C22 C21 120.08(18) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 C22 120.3(2) . . ?
C24 C23 H23 119.9 . . ?
C23 C24 H24 120.1 . . ?
C25 C24 C23 119.88(19) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 H25 119.9 . . ?
C24 C25 C26 120.17(19) . . ?
C26 C25 H25 119.9 . . ?
C21 C26 C25 121.0(2) . . ?
C21 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C28 C27 P2 121.56(16) . . ?
C28 C27 C32 119.18(18) . . ?
C32 C27 P2 119.21(15) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 C27 120.0(2) . . ?
C29 C28 H28 120.0 . . ?
C28 C29 H29 119.9 . . ?
C30 C29 C28 120.2(2) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 119.9 . . ?
C29 C30 C31 120.2(2) . . ?
C31 C30 H30 119.9 . . ?
C30 C31 H31 120.0 . . ?
C32 C31 C30 120.0(2) . . ?
C32 C31 H31 120.0 . . ?
C27 C32 H32 119.8 . . ?
C31 C32 C27 120.3(2) . . ?
C31 C32 H32 119.8 . . ?
C34 C33 P2 121.61(16) . . ?
C38 C33 P2 119.50(17) . . ?
C38 C33 C34 118.9(2) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 C33 120.4(2) . . ?
C35 C34 H34 119.8 . . ?
C34 C35 H35 119.8 . . ?
C36 C35 C34 120.4(2) . . ?
C36 C35 H35 119.8 . . ?
C35 C36 H36 120.2 . . ?
C37 C36 C35 119.6(2) . . ?
C37 C36 H36 120.2 . . ?
C36 C37 H37 119.7 . . ?
C36 C37 C38 120.6(2) . . ?
C38 C37 H37 119.7 . . ?
C33 C38 C37 120.2(2) . . ?
C33 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
Cl51 Zr51 Cl53 90.048(16) . . ?
Cl51 Zr51 P51 166.938(16) . . ?
Cl51 Zr51 P52 82.569(14) . . ?
Cl51 Zr51 C72 82.38(4) . . ?
Cl52 Zr51 Cl51 94.894(16) . . ?
Cl52 Zr51 Cl53 99.115(18) . . ?
Cl52 Zr51 P51 83.526(15) . . ?
Cl52 Zr51 P52 173.966(16) . . ?
Cl52 Zr51 C72 100.02(4) . . ?
Cl53 Zr51 P51 77.451(14) . . ?
Cl53 Zr51 P52 86.391(15) . . ?
Cl53 Zr51 C72 159.94(4) . . ?
P51 Zr51 P52 100.176(14) . . ?
N51 Zr51 Cl51 115.85(4) . . ?
N51 Zr51 Cl52 98.27(4) . . ?
N51 Zr51 Cl53 147.23(4) . . ?
N51 Zr51 P51 77.18(4) . . ?
N51 Zr51 P52 78.06(4) . . ?
N51 Zr51 C72 33.54(5) . . ?
C72 Zr51 P51 110.67(4) . . ?
C72 Zr51 P52 74.26(4) . . ?
C51 P51 Zr51 103.53(6) . . ?
C51 P51 C64 104.48(9) . . ?
C58 P51 Zr51 124.28(6) . . ?
C58 P51 C51 106.27(9) . . ?
C58 P51 C64 103.05(9) . . ?
C64 P51 Zr51 113.52(6) . . ?
C70 P52 Zr51 99.98(6) . . ?
C77 P52 Zr51 119.70(6) . . ?
C77 P52 C70 106.12(8) . . ?
C77 P52 C83 104.41(8) . . ?
C83 P52 Zr51 120.99(6) . . ?
C83 P52 C70 103.34(8) . . ?
C53 N51 Zr51 147.50(12) . . ?
C53 N51 C72 117.40(15) . . ?
C72 N51 Zr51 93.22(10) . . ?
P51 C51 H51A 108.9 . . ?
P51 C51 H51B 108.9 . . ?
H51A C51 H51B 107.7 . . ?
C52 C51 P51 113.36(13) . . ?
C52 C51 H51A 108.9 . . ?
C52 C51 H51B 108.9 . . ?
C53 C52 C51 121.11(17) . . ?
C57 C52 C51 120.03(17) . . ?
C57 C52 C53 118.66(18) . . ?
N51 C53 C52 119.56(17) . . ?
C54 C53 N51 122.22(16) . . ?
C54 C53 C52 118.21(17) . . ?
C53 C54 H54 119.3 . . ?
C55 C54 C53 121.46(18) . . ?
C55 C54 H54 119.3 . . ?
C54 C55 H55 120.1 . . ?
C54 C55 C56 119.9(2) . . ?
C56 C55 H55 120.1 . . ?
C55 C56 H56 120.4 . . ?
C57 C56 C55 119.13(19) . . ?
C57 C56 H56 120.4 . . ?
C52 C57 H57 119.0 . . ?
C56 C57 C52 121.94(19) . . ?
C56 C57 H57 119.0 . . ?
C59 C58 P51 119.51(14) . . ?
C59 C58 C63 118.81(18) . . ?
C63 C58 P51 121.66(15) . . ?
C58 C59 H59 119.9 . . ?
C60 C59 C58 120.30(18) . . ?
C60 C59 H59 119.9 . . ?
C59 C60 H60 120.0 . . ?
C61 C60 C59 120.0(2) . . ?
C61 C60 H60 120.0 . . ?
C60 C61 H61 120.0 . . ?
C62 C61 C60 120.05(19) . . ?
C62 C61 H61 120.0 . . ?
C61 C62 H62 119.9 . . ?
C61 C62 C63 120.18(19) . . ?
C63 C62 H62 119.9 . . ?
C58 C63 H63 119.7 . . ?
C62 C63 C58 120.6(2) . . ?
C62 C63 H63 119.7 . . ?
C65 C64 P51 120.06(16) . . ?
C69 C64 P51 121.29(17) . . ?
C69 C64 C65 118.5(2) . . ?
C64 C65 H65 119.8 . . ?
C64 C65 C66 120.4(2) . . ?
C66 C65 H65 119.8 . . ?
C65 C66 H66 119.9 . . ?
C67 C66 C65 120.3(2) . . ?
C67 C66 H66 119.9 . . ?
C66 C67 H67 120.2 . . ?
C68 C67 C66 119.7(2) . . ?
C68 C67 H67 120.2 . . ?
C67 C68 H68 119.6 . . ?
C67 C68 C69 120.8(2) . . ?
C69 C68 H68 119.6 . . ?
C64 C69 C68 120.2(2) . . ?
C64 C69 H69 119.9 . . ?
C68 C69 H69 119.9 . . ?
P52 C70 H70A 109.5 . . ?
P52 C70 H70B 109.5 . . ?
H70A C70 H70B 108.1 . . ?
C71 C70 P52 110.80(13) . . ?
C71 C70 H70A 109.5 . . ?
C71 C70 H70B 109.5 . . ?
C72 C71 C70 120.64(15) . . ?
C76 C71 C70 120.96(17) . . ?
C76 C71 C72 118.35(17) . . ?
N51 C72 Zr51 53.24(8) . . ?
C71 C72 Zr51 107.08(11) . . ?
C71 C72 N51 121.95(15) . . ?
C73 C72 Zr51 103.80(13) . . ?
C73 C72 N51 117.74(16) . . ?
C73 C72 C71 120.10(16) . . ?
C72 C73 H73 119.9 . . ?
C74 C73 C72 120.29(18) . . ?
C74 C73 H73 119.9 . . ?
C73 C74 H74 120.0 . . ?
C75 C74 C73 119.92(18) . . ?
C75 C74 H74 120.0 . . ?
C74 C75 H75 119.9 . . ?
C74 C75 C76 120.21(18) . . ?
C76 C75 H75 119.9 . . ?
C71 C76 C75 121.13(18) . . ?
C71 C76 H76 119.4 . . ?
C75 C76 H76 119.4 . . ?
C78 C77 P52 121.96(14) . . ?
C82 C77 P52 119.14(15) . . ?
C82 C77 C78 118.89(17) . . ?
C77 C78 H78 119.6 . . ?
C79 C78 C77 120.71(19) . . ?
C79 C78 H78 119.6 . . ?
C78 C79 H79 120.0 . . ?
C80 C79 C78 120.0(2) . . ?
C80 C79 H79 120.0 . . ?
C79 C80 H80 120.0 . . ?
C79 C80 C81 120.02(19) . . ?
C81 C80 H80 120.0 . . ?
C80 C81 H81 119.9 . . ?
C80 C81 C82 120.3(2) . . ?
C82 C81 H81 119.9 . . ?
C77 C82 C81 120.1(2) . . ?
C77 C82 H82 120.0 . . ?
C81 C82 H82 120.0 . . ?
C84 C83 P52 122.59(14) . . ?
C84 C83 C88 118.43(16) . . ?
C88 C83 P52 118.90(13) . . ?
C83 C84 H84 119.8 . . ?
C85 C84 C83 120.50(17) . . ?
C85 C84 H84 119.8 . . ?
C84 C85 H85 119.8 . . ?
C86 C85 C84 120.43(18) . . ?
C86 C85 H85 119.8 . . ?
C85 C86 H86 120.2 . . ?
C85 C86 C87 119.56(17) . . ?
C87 C86 H86 120.2 . . ?
C86 C87 H87 119.9 . . ?
C88 C87 C86 120.20(18) . . ?
C88 C87 H87 119.9 . . ?
C83 C88 H88 119.6 . . ?
C87 C88 C83 120.86(17) . . ?
C87 C88 H88 119.6 . . ?

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
Zr1 P1 C1 C2 -66.10(14) . . . . ?
Zr1 P1 C8 C9 -37.68(18) . . . . ?
Zr1 P1 C8 C13 148.51(15) . . . . ?
Zr1 P1 C14 C15 90.89(17) . . . . ?
Zr1 P1 C14 C19 -88.60(18) . . . . ?
Zr1 P2 C20 C21 -29.03(14) . . . . ?
Zr1 P2 C27 C28 116.44(16) . . . . ?
Zr1 P2 C27 C32 -61.05(17) . . . . ?
Zr1 P2 C33 C34 153.88(15) . . . . ?
Zr1 P2 C33 C38 -28.37(19) . . . . ?
Zr1 N1 C3 C2 -31.7(3) . . . . ?
Zr1 N1 C3 C4 149.6(2) . . . . ?
Zr1 N1 C22 C21 -88.56(16) . . . . ?
Zr1 N1 C22 C23 87.36(15) . . . . ?
Zr1 C22 C23 C24 -119.63(16) . . . . ?
P1 C1 C2 C3 63.3(2) . . . . ?
P1 C1 C2 C7 -123.70(17) . . . . ?
P1 C8 C9 C10 -173.56(15) . . . . ?
P1 C8 C13 C12 173.97(19) . . . . ?
P1 C14 C15 C16 179.03(17) . . . . ?
P1 C14 C19 C18 -179.41(17) . . . . ?
P2 C20 C21 C22 64.4(2) . . . . ?
P2 C20 C21 C26 -113.08(17) . . . . ?
P2 C27 C28 C29 -178.99(17) . . . . ?
P2 C27 C32 C31 179.71(16) . . . . ?
P2 C33 C34 C35 177.62(18) . . . . ?
P2 C33 C38 C37 -178.17(17) . . . . ?
N1 C3 C4 C5 -176.94(18) . . . . ?
N1 C22 C23 C24 -175.01(16) . . . . ?
C1 P1 C8 C9 -156.73(16) . . . . ?
C1 P1 C8 C13 29.5(2) . . . . ?
C1 P1 C14 C15 -157.71(17) . . . . ?
C1 P1 C14 C19 22.81(19) . . . . ?
C1 C2 C3 N1 -12.4(3) . . . . ?
C1 C2 C3 C4 166.28(17) . . . . ?
C1 C2 C7 C6 -169.15(18) . . . . ?
C2 C3 C4 C5 4.4(3) . . . . ?
C3 N1 C22 Zr1 173.56(18) . . . . ?
C3 N1 C22 C21 85.0(2) . . . . ?
C3 N1 C22 C23 -99.08(19) . . . . ?
C3 C2 C7 C6 4.0(3) . . . . ?
C3 C4 C5 C6 0.8(3) . . . . ?
C4 C5 C6 C7 -3.6(3) . . . . ?
C5 C6 C7 C2 1.2(3) . . . . ?
C7 C2 C3 N1 174.59(17) . . . . ?
C7 C2 C3 C4 -6.7(3) . . . . ?
C8 P1 C1 C2 67.30(16) . . . . ?
C8 P1 C14 C15 -48.09(18) . . . . ?
C8 P1 C14 C19 132.42(18) . . . . ?
C8 C9 C10 C11 -1.0(3) . . . . ?
C9 C8 C13 C12 0.1(3) . . . . ?
C9 C10 C11 C12 1.1(3) . . . . ?
C10 C11 C12 C13 -0.5(4) . . . . ?
C11 C12 C13 C8 -0.1(4) . . . . ?
C13 C8 C9 C10 0.4(3) . . . . ?
C14 P1 C1 C2 172.79(14) . . . . ?
C14 P1 C8 C9 95.75(17) . . . . ?
C14 P1 C8 C13 -78.06(19) . . . . ?
C14 C15 C16 C17 0.3(3) . . . . ?
C15 C14 C19 C18 1.1(3) . . . . ?
C15 C16 C17 C18 1.2(3) . . . . ?
C16 C17 C18 C19 -1.6(3) . . . . ?
C17 C18 C19 C14 0.4(3) . . . . ?
C19 C14 C15 C16 -1.5(3) . . . . ?
C20 P2 C27 C28 -132.35(17) . . . . ?
C20 P2 C27 C32 50.16(18) . . . . ?
C20 P2 C33 C34 40.9(2) . . . . ?
C20 P2 C33 C38 -141.31(17) . . . . ?
C20 C21 C22 Zr1 -59.67(18) . . . . ?
C20 C21 C22 N1 -2.9(3) . . . . ?
C20 C21 C22 C23 -178.72(16) . . . . ?
C20 C21 C26 C25 177.95(17) . . . . ?
C21 C22 C23 C24 1.0(3) . . . . ?
C22 N1 C3 C2 160.59(17) . . . . ?
C22 N1 C3 C4 -18.1(3) . . . . ?
C22 C21 C26 C25 0.4(3) . . . . ?
C22 C23 C24 C25 0.0(3) . . . . ?
C23 C24 C25 C26 -0.8(3) . . . . ?
C24 C25 C26 C21 0.5(3) . . . . ?
C26 C21 C22 Zr1 117.89(15) . . . . ?
C26 C21 C22 N1 174.66(16) . . . . ?
C26 C21 C22 C23 -1.2(3) . . . . ?
C27 P2 C20 C21 -153.92(14) . . . . ?
C27 P2 C33 C34 -67.81(19) . . . . ?
C27 P2 C33 C38 109.95(17) . . . . ?
C27 C28 C29 C30 -0.2(4) . . . . ?
C28 C27 C32 C31 2.2(3) . . . . ?
C28 C29 C30 C31 1.3(4) . . . . ?
C29 C30 C31 C32 -0.7(4) . . . . ?
C30 C31 C32 C27 -1.1(3) . . . . ?
C32 C27 C28 C29 -1.5(3) . . . . ?
C33 P2 C20 C21 97.67(15) . . . . ?
C33 P2 C27 C28 -22.41(19) . . . . ?
C33 P2 C27 C32 160.11(16) . . . . ?
C33 C34 C35 C36 0.1(4) . . . . ?
C34 C33 C38 C37 -0.4(3) . . . . ?
C34 C35 C36 C37 0.4(4) . . . . ?
C35 C36 C37 C38 -0.9(4) . . . . ?
C36 C37 C38 C33 0.9(4) . . . . ?
C38 C33 C34 C35 -0.1(3) . . . . ?
Zr51 P51 C51 C52 -63.94(14) . . . . ?
Zr51 P51 C58 C59 -40.91(18) . . . . ?
Zr51 P51 C58 C63 140.71(14) . . . . ?
Zr51 P51 C64 C65 93.50(17) . . . . ?
Zr51 P51 C64 C69 -82.62(18) . . . . ?
Zr51 P52 C70 C71 -25.86(13) . . . . ?
Zr51 P52 C77 C78 150.24(13) . . . . ?
Zr51 P52 C77 C82 -30.95(17) . . . . ?
Zr51 P52 C83 C84 123.18(14) . . . . ?
Zr51 P52 C83 C88 -53.56(16) . . . . ?
Zr51 N51 C53 C52 -35.6(3) . . . . ?
Zr51 N51 C53 C54 144.02(19) . . . . ?
Zr51 N51 C72 C71 -88.06(17) . . . . ?
Zr51 N51 C72 C73 86.76(16) . . . . ?
Zr51 C72 C73 C74 -120.04(17) . . . . ?
P51 C51 C52 C53 65.1(2) . . . . ?
P51 C51 C52 C57 -120.25(17) . . . . ?
P51 C58 C59 C60 -177.80(16) . . . . ?
P51 C58 C63 C62 179.64(16) . . . . ?
P51 C64 C65 C66 -175.57(19) . . . . ?
P51 C64 C69 C68 175.20(19) . . . . ?
P52 C70 C71 C72 61.7(2) . . . . ?
P52 C70 C71 C76 -115.76(17) . . . . ?
P52 C77 C78 C79 178.63(14) . . . . ?
P52 C77 C82 C81 -179.26(16) . . . . ?
P52 C83 C84 C85 -178.20(15) . . . . ?
P52 C83 C88 C87 178.62(15) . . . . ?
N51 C53 C54 C55 -172.45(18) . . . . ?
N51 C72 C73 C74 -175.49(17) . . . . ?
C51 P51 C58 C59 -160.51(15) . . . . ?
C51 P51 C58 C63 21.12(19) . . . . ?
C51 P51 C64 C65 -154.42(17) . . . . ?
C51 P51 C64 C69 29.5(2) . . . . ?
C51 C52 C53 N51 -15.0(3) . . . . ?
C51 C52 C53 C54 165.39(17) . . . . ?
C51 C52 C57 C56 -170.14(19) . . . . ?
C52 C53 C54 C55 7.2(3) . . . . ?
C53 N51 C72 Zr51 168.71(17) . . . . ?
C53 N51 C72 C71 80.7(2) . . . . ?
C53 N51 C72 C73 -104.5(2) . . . . ?
C53 C52 C57 C56 4.7(3) . . . . ?
C53 C54 C55 C56 0.0(3) . . . . ?
C54 C55 C56 C57 -5.0(3) . . . . ?
C55 C56 C57 C52 2.6(3) . . . . ?
C57 C52 C53 N51 170.27(17) . . . . ?
C57 C52 C53 C54 -9.4(3) . . . . ?
C58 P51 C51 C52 68.42(15) . . . . ?
C58 P51 C64 C65 -43.52(19) . . . . ?
C58 P51 C64 C69 140.36(18) . . . . ?
C58 C59 C60 C61 -1.9(3) . . . . ?
C59 C58 C63 C62 1.3(3) . . . . ?
C59 C60 C61 C62 1.2(3) . . . . ?
C60 C61 C62 C63 0.6(3) . . . . ?
C61 C62 C63 C58 -1.9(3) . . . . ?
C63 C58 C59 C60 0.6(3) . . . . ?
C64 P51 C51 C52 176.97(13) . . . . ?
C64 P51 C58 C59 89.92(17) . . . . ?
C64 P51 C58 C63 -88.46(17) . . . . ?
C64 C65 C66 C67 0.0(4) . . . . ?
C65 C64 C69 C68 -1.0(3) . . . . ?
C65 C66 C67 C68 -0.3(4) . . . . ?
C66 C67 C68 C69 -0.1(4) . . . . ?
C67 C68 C69 C64 0.7(4) . . . . ?
C69 C64 C65 C66 0.7(3) . . . . ?
C70 P52 C77 C78 38.37(17) . . . . ?
C70 P52 C77 C82 -142.82(15) . . . . ?
C70 P52 C83 C84 -126.32(16) . . . . ?
C70 P52 C83 C88 56.94(16) . . . . ?
C70 C71 C72 Zr51 -58.95(18) . . . . ?
C70 C71 C72 N51 -2.1(3) . . . . ?
C70 C71 C72 C73 -176.76(17) . . . . ?
C70 C71 C76 C75 177.29(18) . . . . ?
C71 C72 C73 C74 -0.6(3) . . . . ?
C72 N51 C53 C52 165.72(16) . . . . ?
C72 N51 C53 C54 -14.7(2) . . . . ?
C72 C71 C76 C75 -0.3(3) . . . . ?
C72 C73 C74 C75 -0.2(3) . . . . ?
C73 C74 C75 C76 0.7(3) . . . . ?
C74 C75 C76 C71 -0.5(3) . . . . ?
C76 C71 C72 Zr51 118.60(15) . . . . ?
C76 C71 C72 N51 175.49(17) . . . . ?
C76 C71 C72 C73 0.8(3) . . . . ?
C77 P52 C70 C71 99.21(13) . . . . ?
C77 P52 C83 C84 -15.50(18) . . . . ?
C77 P52 C83 C88 167.76(15) . . . . ?
C77 C78 C79 C80 0.6(3) . . . . ?
C78 C77 C82 C81 -0.4(3) . . . . ?
C78 C79 C80 C81 -0.4(3) . . . . ?
C79 C80 C81 C82 -0.2(3) . . . . ?
C80 C81 C82 C77 0.6(3) . . . . ?
C82 C77 C78 C79 -0.2(3) . . . . ?
C83 P52 C70 C71 -151.24(13) . . . . ?
C83 P52 C77 C78 -70.43(16) . . . . ?
C83 P52 C77 C82 108.38(15) . . . . ?
C83 C84 C85 C86 0.2(3) . . . . ?
C84 C83 C88 C87 1.7(3) . . . . ?
C84 C85 C86 C87 0.7(3) . . . . ?
C85 C86 C87 C88 -0.4(3) . . . . ?
C86 C87 C88 C83 -0.8(3) . . . . ?
C88 C83 C84 C85 -1.4(3) . . . . ?
_audit_block_usercomment         'sb_dh36_2, irregular, yellow'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.194
_oxdiff_exptl_absorpt_empirical_full_min 0.829
_cell_oxdiff_length_a            11.44486(13)
_cell_oxdiff_length_b            17.6843(2)
_cell_oxdiff_length_c            19.9828(3)
_cell_oxdiff_angle_alpha         80.0131(11)
_cell_oxdiff_angle_beta          88.4840(10)
_cell_oxdiff_angle_gamma         72.8933(10)
_cell_oxdiff_volume              3805.61(8)
_cell_oxdiff_measurement_reflns_used 111747
_symmetry_cell_setting           triclinic
#_space_group_name_H-M_alt       'P -1'
#_space_group_IT_number          2
_chemical_absolute_configuration .
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ba_sb71_sq
_database_code_depnum_ccdc_archive 'CCDC 1530474'
_audit_update_record             
;
2017-03-17 deposited with the CCDC.
2017-04-05 downloaded from the CCDC.
;
_audit_creation_date             2016-08-08

_audit_block_code                ba_sb71
_audit_block_refno               2751


# start Validation Reply Form
_vrf_PLAT910_ba_sb71_sq          
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          13 Note
RESPONSE: limited by diffractometer.
;
# end Validation Reply Form

_audit_creation_method           
;
Olex2 1.2
(compiled Dec 12 2016 15:58:59 for OlexSys, GUI svn.r5292)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C47 H45 Cl N O0.50 P2 Zr'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         820.45
_chemical_melting_point          ?
_exptl_crystal_description       plate
_exptl_crystal_colour            green
_diffrn_ambient_temperature      120(1)
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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   18.9791(3)
_cell_length_b                   11.12020(16)
_cell_length_c                   38.2266(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.1276(14)
_cell_angle_gamma                90
_cell_volume                     7916.1(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    29506
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      31.8860
_cell_measurement_theta_min      3.2530
_shelx_estimated_absorpt_T_max   0.955
_shelx_estimated_absorpt_T_min   0.955
_exptl_absorpt_coefficient_mu    0.462
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3400
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-13 -13 18 0.0521
23 0 -36 0.0689
-4 15 8 0.0565
-13 13 22 0.0577
3 -15 -7 0.0746
7 0 48 0.0137
-7 0 -48 0.0137
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.027
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-13.0044 -13.0067 17.9991 -0.0640 0.9898 0.0026
23.0114 -0.0004 -35.9790 0.0422 -0.5431 -0.8391
-4.0043 15.0081 7.9837 0.0551 -0.6969 0.6820
-13.0085 13.0072 21.9772 0.0279 -0.3784 0.9401
3.0039 -15.0081 -6.9846 -0.0476 0.7185 -0.6502
7.0001 -0.0010 48.0005 -0.9642 0.0453 0.2383
-7.0001 0.0010 -48.0005 0.9642 -0.0453 -0.2383

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            125681
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.287
_diffrn_reflns_theta_min         2.982
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -3.00  99.00   0.50   25.00    --   28.16  77.00-150.00  204
  2  ω      7.00  97.00   0.50   25.00    --   28.16  57.00 -30.00  180
  3  ω    -20.00  72.00   0.50   25.00    --   28.16 -99.00 120.00  184
  4  ω    -44.00  56.00   0.50   25.00    --   28.16 -38.00 -30.00  200
  5  ω     -3.00  99.00   0.50   25.00    --   28.16  77.00 120.00  204
  6  ω    -44.00  56.00   0.50   25.00    --   28.16 -38.00  60.00  200
  7  ω     -3.00  99.00   0.50   25.00    --   28.16  77.00  30.00  204
  8  ω    -43.00  60.00   0.50   25.00    --   28.16 -77.00 -90.00  206
  9  ω    -41.00  50.00   0.50   25.00    --   28.16 -57.00-180.00  182
 10  ω     -3.00  99.00   0.50   25.00    --   28.16  77.00 -90.00  204
 11  ω      1.00 101.00   0.50   25.00    --   28.16  38.00-180.00  200
 12  ω    -20.00  72.00   0.50   25.00    --   28.16 -99.00-180.00  184
 13  ω      1.00  49.00   0.50   25.00    --   28.16  38.00 120.00   96
 14  ω    -20.00  72.00   0.50   25.00    --   28.16 -99.00   0.00  184
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0240834000
_diffrn_orient_matrix_UB_12      0.0060659000
_diffrn_orient_matrix_UB_13      -0.0165751000
_diffrn_orient_matrix_UB_21      -0.0180189000
_diffrn_orient_matrix_UB_22      -0.0531432000
_diffrn_orient_matrix_UB_23      0.0035709000
_diffrn_orient_matrix_UB_31      -0.0233713000
_diffrn_orient_matrix_UB_32      0.0347519000
_diffrn_orient_matrix_UB_33      0.0083727000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11129
_reflns_number_total             13622
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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,
 see _platon_squeeze_.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2016/6
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         1.483
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         13622
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0342
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0353P)²+7.7814P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0810
_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 distances
 C40-H40 \\sim C44-H44
 with sigma of 0.02
 C41-H41 \\sim C43-H43
 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C20(H20A,H20B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
3.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.31972(2) 0.86053(2) 0.61273(2) 0.01324(4) Uani 1 1 d . . . . .
Cl Cl 0.19533(2) 0.95290(3) 0.59828(2) 0.01999(7) Uani 1 1 d . . . . .
P1 P 0.36433(2) 1.08801(3) 0.59516(2) 0.01706(7) Uani 1 1 d . . . . .
P2 P 0.25952(2) 0.75686(3) 0.66426(2) 0.01444(7) Uani 1 1 d . . . . .
N N 0.37051(6) 0.93946(11) 0.66463(3) 0.0162(2) Uani 1 1 d . . . . .
C1 C 0.43883(8) 1.12989(13) 0.63178(4) 0.0193(3) Uani 1 1 d . . . . .
H1A H 0.471318 1.187003 0.622887 0.023 Uiso 1 1 calc R . . . .
H1B H 0.419482 1.169871 0.651058 0.023 Uiso 1 1 calc R . . . .
C2 C 0.47990(7) 1.01893(13) 0.64611(4) 0.0175(3) Uani 1 1 d . . . . .
C3 C 0.44486(7) 0.92914(13) 0.66258(4) 0.0161(2) Uani 1 1 d . . . . .
C4 C 0.48272(8) 0.82516(14) 0.67570(4) 0.0199(3) Uani 1 1 d . . . . .
H4 H 0.460025 0.765545 0.687473 0.024 Uiso 1 1 calc R . . . .
C5 C 0.55363(8) 0.80868(15) 0.67155(4) 0.0230(3) Uani 1 1 d . . . . .
H5 H 0.578795 0.737591 0.680261 0.028 Uiso 1 1 calc R . . . .
C6 C 0.58722(8) 0.89572(15) 0.65479(4) 0.0234(3) Uani 1 1 d . . . . .
H6 H 0.635244 0.883961 0.651738 0.028 Uiso 1 1 calc R . . . .
C7 C 0.55067(8) 1.00072(14) 0.64236(4) 0.0214(3) Uani 1 1 d . . . . .
H7 H 0.574346 1.060639 0.631180 0.026 Uiso 1 1 calc R . . . .
C8 C 0.39693(8) 1.11317(13) 0.55387(4) 0.0204(3) Uani 1 1 d . . . . .
C9 C 0.34832(9) 1.09710(15) 0.52155(4) 0.0254(3) Uani 1 1 d . . . . .
H9 H 0.299701 1.077795 0.521901 0.031 Uiso 1 1 calc R . . . .
C10 C 0.37020(10) 1.10899(17) 0.48894(5) 0.0318(4) Uani 1 1 d . . . . .
H10 H 0.336673 1.098162 0.467264 0.038 Uiso 1 1 calc R . . . .
C11 C 0.44084(11) 1.13656(18) 0.48834(5) 0.0360(4) Uani 1 1 d . . . . .
H11 H 0.455808 1.146439 0.466187 0.043 Uiso 1 1 calc R . . . .
C12 C 0.48996(10) 1.14987(18) 0.51998(5) 0.0346(4) Uani 1 1 d . . . . .
H12 H 0.538730 1.167183 0.519387 0.041 Uiso 1 1 calc R . . . .
C13 C 0.46853(9) 1.13811(15) 0.55261(5) 0.0260(3) Uani 1 1 d . . . . .
H13 H 0.502746 1.147070 0.574140 0.031 Uiso 1 1 calc R . . . .
C14 C 0.29934(8) 1.20891(14) 0.59696(5) 0.0241(3) Uani 1 1 d . . . . .
C15 C 0.27440(9) 1.22182(15) 0.62912(5) 0.0322(4) Uani 1 1 d . . . . .
H15 H 0.294125 1.173417 0.649096 0.039 Uiso 1 1 calc R . . . .
C16 C 0.22102(10) 1.30505(17) 0.63181(7) 0.0436(5) Uani 1 1 d . . . . .
H16 H 0.205889 1.315594 0.653894 0.052 Uiso 1 1 calc R . . . .
C17 C 0.19004(11) 1.37217(18) 0.60268(8) 0.0506(6) Uani 1 1 d . . . . .
H17 H 0.152075 1.426223 0.604362 0.061 Uiso 1 1 calc R . . . .
C18 C 0.21402(12) 1.36104(17) 0.57113(7) 0.0496(6) Uani 1 1 d . . . . .
H18 H 0.192860 1.408349 0.551155 0.059 Uiso 1 1 calc R . . . .
C19 C 0.26946(10) 1.28047(15) 0.56812(5) 0.0344(4) Uani 1 1 d . . . . .
H19 H 0.286532 1.274894 0.546394 0.041 Uiso 1 1 calc R . . . .
C20 C 0.23369(7) 0.88485(13) 0.68951(4) 0.0177(3) Uani 1 1 d . . . . .
H20A H 0.193638 0.926522 0.673717 0.021 Uiso 1 1 calc R . . . .
H20B H 0.213935 0.851168 0.709576 0.021 Uiso 1 1 calc R . . . .
C21 C 0.28794(7) 0.98037(13) 0.70497(4) 0.0160(2) Uani 1 1 d . . . . .
C22 C 0.35441(7) 0.99879(13) 0.69413(4) 0.0157(2) Uani 1 1 d . . . . .
C23 C 0.40323(8) 1.08062(13) 0.71424(4) 0.0191(3) Uani 1 1 d . . . . .
H23 H 0.449686 1.089439 0.708747 0.023 Uiso 1 1 calc R . . . .
C24 C 0.38539(8) 1.14820(14) 0.74167(4) 0.0220(3) Uani 1 1 d . . . . .
H24 H 0.419214 1.203199 0.754403 0.026 Uiso 1 1 calc R . . . .
C25 C 0.31818(9) 1.13592(15) 0.75065(4) 0.0244(3) Uani 1 1 d . . . . .
H25 H 0.304785 1.184373 0.768766 0.029 Uiso 1 1 calc R . . . .
C26 C 0.27097(8) 1.05094(14) 0.73247(4) 0.0212(3) Uani 1 1 d . . . . .
H26 H 0.225532 1.040502 0.738998 0.025 Uiso 1 1 calc R . . . .
C27 C 0.31750(7) 0.66118(13) 0.69626(4) 0.0175(3) Uani 1 1 d . . . . .
C28 C 0.35535(8) 0.70418(14) 0.72885(4) 0.0205(3) Uani 1 1 d . . . . .
H28 H 0.348682 0.784796 0.735761 0.025 Uiso 1 1 calc R . . . .
C29 C 0.40294(8) 0.62915(16) 0.75130(4) 0.0262(3) Uani 1 1 d . . . . .
H29 H 0.428417 0.658981 0.773445 0.031 Uiso 1 1 calc R . . . .
C30 C 0.41325(9) 0.51148(16) 0.74148(5) 0.0300(4) Uani 1 1 d . . . . .
H30 H 0.445868 0.460941 0.756817 0.036 Uiso 1 1 calc R . . . .
C31 C 0.37575(9) 0.46746(15) 0.70914(5) 0.0278(3) Uani 1 1 d . . . . .
H31 H 0.382604 0.386738 0.702371 0.033 Uiso 1 1 calc R . . . .
C32 C 0.32820(8) 0.54188(14) 0.68671(4) 0.0233(3) Uani 1 1 d . . . . .
H32 H 0.302676 0.511437 0.664658 0.028 Uiso 1 1 calc R . . . .
C33 C 0.17404(7) 0.67458(13) 0.65665(4) 0.0172(3) Uani 1 1 d . . . . .
C34 C 0.15109(9) 0.61159(15) 0.68406(4) 0.0259(3) Uani 1 1 d . . . . .
H34 H 0.181139 0.607583 0.706986 0.031 Uiso 1 1 calc R . . . .
C35 C 0.08451(9) 0.55468(16) 0.67799(5) 0.0328(4) Uani 1 1 d . . . . .
H35 H 0.069163 0.512708 0.696837 0.039 Uiso 1 1 calc R . . . .
C36 C 0.04065(9) 0.55901(16) 0.64465(5) 0.0321(4) Uani 1 1 d . . . . .
H36 H -0.004843 0.520366 0.640667 0.039 Uiso 1 1 calc R . . . .
C37 C 0.06291(8) 0.61966(14) 0.61702(5) 0.0255(3) Uani 1 1 d . . . . .
H37 H 0.033092 0.621360 0.594008 0.031 Uiso 1 1 calc R . . . .
C38 C 0.12927(8) 0.67828(14) 0.62307(4) 0.0200(3) Uani 1 1 d . . . . .
H38 H 0.144040 0.720963 0.604194 0.024 Uiso 1 1 calc R . . . .
C39 C 0.27072(8) 0.72323(14) 0.55975(4) 0.0207(3) Uani 1 1 d . . . . .
C40 C 0.29742(8) 0.65233(13) 0.58892(4) 0.0207(3) Uani 1 1 d D . . . .
H40 H 0.2688(10) 0.5931(16) 0.5953(5) 0.025 Uiso 1 1 d DR . . . .
C41 C 0.36967(8) 0.67107(14) 0.60957(4) 0.0208(3) Uani 1 1 d D . . . .
H41 H 0.3861(10) 0.6216(16) 0.6280(5) 0.025 Uiso 1 1 d DR . . . .
C42 C 0.41790(8) 0.74134(15) 0.59298(4) 0.0235(3) Uani 1 1 d . . . . .
H42 H 0.4695(11) 0.7431(18) 0.6029(5) 0.028 Uiso 1 1 d R . . . .
C43 C 0.39079(8) 0.81608(15) 0.56503(4) 0.0224(3) Uani 1 1 d D . . . .
H43 H 0.4205(10) 0.8666(16) 0.5554(5) 0.027 Uiso 1 1 d DR . . . .
C44 C 0.31443(8) 0.82086(15) 0.55094(4) 0.0208(3) Uani 1 1 d D . . . .
H44 H 0.2955(10) 0.8681(16) 0.5318(5) 0.025 Uiso 1 1 d DR . . . .
C45 C 0.19588(9) 0.70715(17) 0.53848(4) 0.0283(3) Uani 1 1 d . . . . .
H45A H 0.170551 0.646456 0.549956 0.042 Uiso 1 1 calc GR . . . .
H45B H 0.198358 0.680770 0.514286 0.042 Uiso 1 1 calc GR . . . .
H45C H 0.170000 0.783740 0.537347 0.042 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
Zr Cl 2.5358(4) . ?
Zr P1 2.7905(4) . ?
Zr P2 2.7170(4) . ?
Zr N 2.2130(12) . ?
Zr C3 2.8473(13) . ?
Zr C39 2.5633(14) . ?
Zr C40 2.4938(15) . ?
Zr C41 2.3230(15) . ?
Zr C42 2.5184(15) . ?
Zr C43 2.5175(14) . ?
Zr C44 2.3861(14) . ?
P1 C1 1.8472(15) . ?
P1 C8 1.8244(15) . ?
P1 C14 1.8349(16) . ?
P2 C20 1.8386(15) . ?
P2 C27 1.8221(14) . ?
P2 C33 1.8361(14) . ?
N C3 1.4330(17) . ?
N C22 1.3901(17) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.505(2) . ?
C2 C3 1.413(2) . ?
C2 C7 1.393(2) . ?
C3 C4 1.402(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.397(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.383(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.394(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.403(2) . ?
C8 C13 1.397(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.394(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.380(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.385(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.391(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.407(2) . ?
C14 C19 1.389(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.391(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.375(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.375(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.404(3) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.517(2) . ?
C21 C22 1.4167(19) . ?
C21 C26 1.3986(19) . ?
C22 C23 1.415(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.384(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.390(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.392(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.397(2) . ?
C27 C32 1.401(2) . ?
C28 H28 0.9500 . ?
C28 C29 1.396(2) . ?
C29 H29 0.9500 . ?
C29 C30 1.386(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.391(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.391(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.398(2) . ?
C33 C38 1.397(2) . ?
C34 H34 0.9500 . ?
C34 C35 1.392(2) . ?
C35 H35 0.9500 . ?
C35 C36 1.382(3) . ?
C36 H36 0.9500 . ?
C36 C37 1.386(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.397(2) . ?
C38 H38 0.9500 . ?
C39 C40 1.380(2) . ?
C39 C44 1.445(2) . ?
C39 C45 1.505(2) . ?
C40 H40 0.917(16) . ?
C40 C41 1.459(2) . ?
C41 H41 0.902(16) . ?
C41 C42 1.441(2) . ?
C42 H42 0.98(2) . ?
C42 C43 1.373(2) . ?
C43 H43 0.921(16) . ?
C43 C44 1.446(2) . ?
C44 H44 0.914(16) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 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
Cl Zr P1 83.876(12) . . ?
Cl Zr P2 79.965(11) . . ?
Cl Zr C3 131.19(3) . . ?
Cl Zr C39 83.60(4) . . ?
P1 Zr C3 70.46(3) . . ?
P2 Zr P1 138.484(12) . . ?
P2 Zr C3 92.39(3) . . ?
N Zr Cl 105.11(3) . . ?
N Zr P1 75.90(3) . . ?
N Zr P2 71.92(3) . . ?
N Zr C3 29.66(4) . . ?
N Zr C39 166.75(5) . . ?
N Zr C40 135.18(5) . . ?
N Zr C41 107.15(5) . . ?
N Zr C42 104.96(5) . . ?
N Zr C43 121.72(5) . . ?
N Zr C44 152.71(5) . . ?
C39 Zr P1 115.49(4) . . ?
C39 Zr P2 100.42(3) . . ?
C39 Zr C3 144.78(4) . . ?
C40 Zr Cl 102.20(4) . . ?
C40 Zr P1 142.34(4) . . ?
C40 Zr P2 78.77(4) . . ?
C40 Zr C3 123.64(5) . . ?
C40 Zr C39 31.63(5) . . ?
C40 Zr C42 59.02(5) . . ?
C40 Zr C43 68.30(5) . . ?
C41 Zr Cl 136.73(4) . . ?
C41 Zr P1 131.59(4) . . ?
C41 Zr P2 83.44(4) . . ?
C41 Zr C3 88.96(5) . . ?
C41 Zr C39 60.54(5) . . ?
C41 Zr C40 35.04(5) . . ?
C41 Zr C42 34.32(5) . . ?
C41 Zr C43 60.21(5) . . ?
C41 Zr C44 73.77(6) . . ?
C42 Zr Cl 149.25(4) . . ?
C42 Zr P1 97.38(4) . . ?
C42 Zr P2 115.66(4) . . ?
C42 Zr C3 76.81(5) . . ?
C42 Zr C39 68.05(5) . . ?
C43 Zr Cl 121.88(4) . . ?
C43 Zr P1 76.92(4) . . ?
C43 Zr P2 143.21(4) . . ?
C43 Zr C3 92.47(5) . . ?
C43 Zr C39 58.28(5) . . ?
C43 Zr C42 31.64(5) . . ?
C44 Zr Cl 89.98(4) . . ?
C44 Zr P1 83.45(4) . . ?
C44 Zr P2 134.10(4) . . ?
C44 Zr C3 125.62(5) . . ?
C44 Zr C39 33.71(5) . . ?
C44 Zr C40 59.69(5) . . ?
C44 Zr C42 59.87(5) . . ?
C44 Zr C43 34.18(5) . . ?
C1 P1 Zr 105.63(5) . . ?
C8 P1 Zr 121.11(5) . . ?
C8 P1 C1 106.22(7) . . ?
C8 P1 C14 105.24(7) . . ?
C14 P1 Zr 114.69(5) . . ?
C14 P1 C1 102.04(7) . . ?
C20 P2 Zr 104.14(5) . . ?
C27 P2 Zr 116.78(5) . . ?
C27 P2 C20 106.68(7) . . ?
C27 P2 C33 102.47(7) . . ?
C33 P2 Zr 125.38(5) . . ?
C33 P2 C20 98.74(6) . . ?
C3 N Zr 100.50(8) . . ?
C22 N Zr 142.13(9) . . ?
C22 N C3 117.08(11) . . ?
P1 C1 H1A 109.7 . . ?
P1 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
C2 C1 P1 109.64(10) . . ?
C2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
C3 C2 C1 119.09(12) . . ?
C7 C2 C1 121.59(13) . . ?
C7 C2 C3 119.28(13) . . ?
N C3 Zr 49.84(6) . . ?
C2 C3 Zr 107.13(9) . . ?
C2 C3 N 121.39(13) . . ?
C4 C3 Zr 108.79(9) . . ?
C4 C3 N 119.25(13) . . ?
C4 C3 C2 119.29(13) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.40(14) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.07(14) . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.05(14) . . ?
C7 C6 H6 120.0 . . ?
C2 C7 C6 120.86(14) . . ?
C2 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C9 C8 P1 117.84(11) . . ?
C13 C8 P1 123.70(12) . . ?
C13 C8 C9 118.27(14) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 C8 121.10(16) . . ?
C10 C9 H9 119.5 . . ?
C9 C10 H10 120.2 . . ?
C11 C10 C9 119.61(17) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.09(17) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 119.7 . . ?
C11 C12 C13 120.61(17) . . ?
C13 C12 H12 119.7 . . ?
C8 C13 H13 119.9 . . ?
C12 C13 C8 120.29(16) . . ?
C12 C13 H13 119.9 . . ?
C15 C14 P1 116.71(13) . . ?
C19 C14 P1 124.36(14) . . ?
C19 C14 C15 118.71(16) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 C14 120.34(19) . . ?
C16 C15 H15 119.8 . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.4(2) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 119.97(19) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 119.7 . . ?
C17 C18 C19 120.6(2) . . ?
C19 C18 H18 119.7 . . ?
C14 C19 C18 119.9(2) . . ?
C14 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
P2 C20 H20A 107.1 . . ?
P2 C20 H20B 107.1 . . ?
H20A C20 H20B 106.8 . . ?
C21 C20 P2 121.11(10) . . ?
C21 C20 H20A 107.1 . . ?
C21 C20 H20B 107.1 . . ?
C22 C21 C20 124.26(12) . . ?
C26 C21 C20 116.62(12) . . ?
C26 C21 C22 119.08(13) . . ?
N C22 C21 121.06(12) . . ?
N C22 C23 121.50(12) . . ?
C23 C22 C21 117.43(12) . . ?
C22 C23 H23 119.0 . . ?
C24 C23 C22 122.04(14) . . ?
C24 C23 H23 119.0 . . ?
C23 C24 H24 119.9 . . ?
C23 C24 C25 120.27(14) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 120.8 . . ?
C24 C25 C26 118.43(14) . . ?
C26 C25 H25 120.8 . . ?
C21 C26 H26 118.8 . . ?
C25 C26 C21 122.46(14) . . ?
C25 C26 H26 118.8 . . ?
C28 C27 P2 122.61(11) . . ?
C28 C27 C32 118.74(13) . . ?
C32 C27 P2 118.51(11) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 C27 120.27(15) . . ?
C29 C28 H28 119.9 . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.42(16) . . ?
C30 C29 H29 119.8 . . ?
C29 C30 H30 120.1 . . ?
C29 C30 C31 119.88(15) . . ?
C31 C30 H30 120.1 . . ?
C30 C31 H31 120.1 . . ?
C30 C31 C32 119.87(16) . . ?
C32 C31 H31 120.1 . . ?
C27 C32 H32 119.6 . . ?
C31 C32 C27 120.82(15) . . ?
C31 C32 H32 119.6 . . ?
C34 C33 P2 121.65(11) . . ?
C38 C33 P2 119.54(11) . . ?
C38 C33 C34 118.77(14) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 C33 120.47(16) . . ?
C35 C34 H34 119.8 . . ?
C34 C35 H35 119.9 . . ?
C36 C35 C34 120.24(16) . . ?
C36 C35 H35 119.9 . . ?
C35 C36 H36 119.9 . . ?
C35 C36 C37 120.12(15) . . ?
C37 C36 H36 119.9 . . ?
C36 C37 H37 120.0 . . ?
C36 C37 C38 119.91(15) . . ?
C38 C37 H37 120.0 . . ?
C33 C38 C37 120.49(14) . . ?
C33 C38 H38 119.8 . . ?
C37 C38 H38 119.8 . . ?
C40 C39 Zr 71.41(8) . . ?
C40 C39 C44 118.68(14) . . ?
C40 C39 C45 122.00(14) . . ?
C44 C39 Zr 66.40(8) . . ?
C44 C39 C45 119.19(14) . . ?
C45 C39 Zr 131.17(11) . . ?
Zr C40 H40 129.6(12) . . ?
C39 C40 Zr 76.97(9) . . ?
C39 C40 H40 118.9(12) . . ?
C39 C40 C41 121.06(14) . . ?
C41 C40 Zr 66.07(8) . . ?
C41 C40 H40 120.1(12) . . ?
Zr C41 H41 126.6(12) . . ?
C40 C41 Zr 78.89(9) . . ?
C40 C41 H41 118.9(13) . . ?
C42 C41 Zr 80.28(9) . . ?
C42 C41 C40 116.73(14) . . ?
C42 C41 H41 121.5(12) . . ?
Zr C42 H42 128.1(11) . . ?
C41 C42 Zr 65.39(8) . . ?
C41 C42 H42 120.9(11) . . ?
C43 C42 Zr 74.15(9) . . ?
C43 C42 C41 119.77(14) . . ?
C43 C42 H42 119.0(12) . . ?
Zr C43 H43 128.7(12) . . ?
C42 C43 Zr 74.22(9) . . ?
C42 C43 H43 120.9(13) . . ?
C42 C43 C44 120.68(14) . . ?
C44 C43 Zr 67.93(8) . . ?
C44 C43 H43 118.4(12) . . ?
Zr C44 H44 128.3(12) . . ?
C39 C44 Zr 79.89(8) . . ?
C39 C44 C43 117.68(14) . . ?
C39 C44 H44 117.6(12) . . ?
C43 C44 Zr 77.89(8) . . ?
C43 C44 H44 121.9(12) . . ?
C39 C45 H45A 109.5 . . ?
C39 C45 H45B 109.5 . . ?
C39 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 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 P1 C1 C2 32.91(11) . . . . ?
Zr P1 C8 C9 64.73(14) . . . . ?
Zr P1 C8 C13 -110.03(13) . . . . ?
Zr P1 C14 C15 54.22(14) . . . . ?
Zr P1 C14 C19 -120.30(13) . . . . ?
Zr P2 C20 C21 -53.86(12) . . . . ?
Zr P2 C27 C28 93.25(12) . . . . ?
Zr P2 C27 C32 -82.35(12) . . . . ?
Zr P2 C33 C34 172.13(11) . . . . ?
Zr P2 C33 C38 -10.32(14) . . . . ?
Zr N C3 C2 86.37(13) . . . . ?
Zr N C3 C4 -90.59(13) . . . . ?
Zr N C22 C21 28.8(2) . . . . ?
Zr N C22 C23 -150.57(13) . . . . ?
Zr C3 C4 C5 121.22(13) . . . . ?
Zr C39 C40 C41 -51.29(12) . . . . ?
Zr C39 C44 C43 70.48(12) . . . . ?
Zr C40 C41 C42 -73.06(12) . . . . ?
Zr C41 C42 C43 -52.54(14) . . . . ?
Zr C42 C43 C44 -51.56(13) . . . . ?
Zr C43 C44 C39 -71.62(12) . . . . ?
P1 C1 C2 C3 -63.99(15) . . . . ?
P1 C1 C2 C7 113.63(14) . . . . ?
P1 C8 C9 C10 -176.85(13) . . . . ?
P1 C8 C13 C12 176.55(14) . . . . ?
P1 C14 C15 C16 -175.05(14) . . . . ?
P1 C14 C19 C18 172.54(14) . . . . ?
P2 C20 C21 C22 17.41(19) . . . . ?
P2 C20 C21 C26 -160.40(11) . . . . ?
P2 C27 C28 C29 -175.48(12) . . . . ?
P2 C27 C32 C31 175.57(12) . . . . ?
P2 C33 C34 C35 176.96(13) . . . . ?
P2 C33 C38 C37 -177.85(12) . . . . ?
N C3 C4 C5 175.05(13) . . . . ?
N C22 C23 C24 174.14(14) . . . . ?
C1 P1 C8 C9 -175.05(12) . . . . ?
C1 P1 C8 C13 10.18(15) . . . . ?
C1 P1 C14 C15 -59.43(14) . . . . ?
C1 P1 C14 C19 126.04(14) . . . . ?
C1 C2 C3 Zr 55.45(14) . . . . ?
C1 C2 C3 N 2.5(2) . . . . ?
C1 C2 C3 C4 179.46(13) . . . . ?
C1 C2 C7 C6 -177.96(14) . . . . ?
C2 C3 C4 C5 -2.0(2) . . . . ?
C3 N C22 C21 -158.88(13) . . . . ?
C3 N C22 C23 21.77(19) . . . . ?
C3 C2 C7 C6 -0.4(2) . . . . ?
C3 C4 C5 C6 0.7(2) . . . . ?
C4 C5 C6 C7 0.7(2) . . . . ?
C5 C6 C7 C2 -0.9(2) . . . . ?
C7 C2 C3 Zr -122.22(12) . . . . ?
C7 C2 C3 N -175.17(13) . . . . ?
C7 C2 C3 C4 1.8(2) . . . . ?
C8 P1 C1 C2 -96.89(11) . . . . ?
C8 P1 C14 C15 -170.17(13) . . . . ?
C8 P1 C14 C19 15.30(16) . . . . ?
C8 C9 C10 C11 0.2(3) . . . . ?
C9 C8 C13 C12 1.8(2) . . . . ?
C9 C10 C11 C12 1.3(3) . . . . ?
C10 C11 C12 C13 -1.3(3) . . . . ?
C11 C12 C13 C8 -0.3(3) . . . . ?
C13 C8 C9 C10 -1.8(2) . . . . ?
C14 P1 C1 C2 153.12(10) . . . . ?
C14 P1 C8 C9 -67.34(14) . . . . ?
C14 P1 C8 C13 117.90(14) . . . . ?
C14 C15 C16 C17 2.6(3) . . . . ?
C15 C14 C19 C18 -1.9(3) . . . . ?
C15 C16 C17 C18 -2.9(3) . . . . ?
C16 C17 C18 C19 0.8(3) . . . . ?
C17 C18 C19 C14 1.6(3) . . . . ?
C19 C14 C15 C16 -0.2(3) . . . . ?
C20 P2 C27 C28 -22.66(14) . . . . ?
C20 P2 C27 C32 161.75(11) . . . . ?
C20 P2 C33 C34 -73.53(14) . . . . ?
C20 P2 C33 C38 104.03(12) . . . . ?
C20 C21 C22 N 8.8(2) . . . . ?
C20 C21 C22 C23 -171.87(13) . . . . ?
C20 C21 C26 C25 175.41(14) . . . . ?
C21 C22 C23 C24 -5.2(2) . . . . ?
C22 N C3 Zr -175.22(15) . . . . ?
C22 N C3 C2 -88.86(16) . . . . ?
C22 N C3 C4 94.18(16) . . . . ?
C22 C21 C26 C25 -2.5(2) . . . . ?
C22 C23 C24 C25 0.9(2) . . . . ?
C23 C24 C25 C26 2.7(2) . . . . ?
C24 C25 C26 C21 -1.9(2) . . . . ?
C26 C21 C22 N -173.49(13) . . . . ?
C26 C21 C22 C23 5.9(2) . . . . ?
C27 P2 C20 C21 70.23(12) . . . . ?
C27 P2 C33 C34 35.83(14) . . . . ?
C27 P2 C33 C38 -146.62(12) . . . . ?
C27 C28 C29 C30 0.1(2) . . . . ?
C28 C27 C32 C31 -0.2(2) . . . . ?
C28 C29 C30 C31 -0.3(2) . . . . ?
C29 C30 C31 C32 0.2(3) . . . . ?
C30 C31 C32 C27 0.1(2) . . . . ?
C32 C27 C28 C29 0.1(2) . . . . ?
C33 P2 C20 C21 176.14(11) . . . . ?
C33 P2 C27 C28 -125.88(12) . . . . ?
C33 P2 C27 C32 58.53(13) . . . . ?
C33 C34 C35 C36 0.6(3) . . . . ?
C34 C33 C38 C37 -0.2(2) . . . . ?
C34 C35 C36 C37 0.3(3) . . . . ?
C35 C36 C37 C38 -1.1(3) . . . . ?
C36 C37 C38 C33 1.1(2) . . . . ?
C38 C33 C34 C35 -0.6(2) . . . . ?
C39 C40 C41 Zr 56.27(13) . . . . ?
C39 C40 C41 C42 -16.8(2) . . . . ?
C40 C39 C44 Zr -50.54(13) . . . . ?
C40 C39 C44 C43 19.9(2) . . . . ?
C40 C41 C42 Zr 72.24(12) . . . . ?
C40 C41 C42 C43 19.7(2) . . . . ?
C41 C42 C43 Zr 48.61(13) . . . . ?
C41 C42 C43 C44 -2.9(2) . . . . ?
C42 C43 C44 Zr 54.42(14) . . . . ?
C42 C43 C44 C39 -17.2(2) . . . . ?
C44 C39 C40 Zr 48.29(12) . . . . ?
C44 C39 C40 C41 -3.0(2) . . . . ?
C45 C39 C40 Zr -127.51(14) . . . . ?
C45 C39 C40 C41 -178.80(14) . . . . ?
C45 C39 C44 Zr 125.37(13) . . . . ?
C45 C39 C44 C43 -164.15(14) . . . . ?
_audit_block_usercomment         'sb561, plate, green'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.109
_oxdiff_exptl_absorpt_empirical_full_min 0.894
_cell_oxdiff_length_a            18.9789(4)
_cell_oxdiff_length_b            11.11995(18)
_cell_oxdiff_length_c            38.2295(8)
_cell_oxdiff_angle_alpha         90.0350(15)
_cell_oxdiff_angle_beta          101.1396(17)
_cell_oxdiff_angle_gamma         89.9771(15)
_cell_oxdiff_volume              7916.1(3)
_cell_oxdiff_measurement_reflns_used 29506
_symmetry_cell_setting           monoclinic
#_space_group_name_H-M_alt       'I 2/a'
#_space_group_IT_number          15
_chemical_absolute_configuration .
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
####################################################################### 
# 
# 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_ba_dh1
_database_code_depnum_ccdc_archive 'CCDC 1530469'
_audit_update_record             
;
2017-03-17 deposited with the CCDC.
2017-04-05 downloaded from the CCDC.
;
_audit_creation_date             2016-04-14

_audit_block_code                ba_dh1
_audit_block_refno               2701
_audit_block_usercomment         sb_dh20


_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C38 H32 I3 N P2 Zr, C H2 Cl2'
_chemical_formula_sum            'C39 H34 Cl2 I3 N P2 Zr'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         1121.43
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            red
_diffrn_ambient_temperature      100(1)
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/n'
_symmetry_int_tables_number      14

_chemical_absolute_configuration .

_space_group_name_Hall           '-P 2yn'
loop_
_symmetry_equiv_pos_as_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                   12.220(5)
_cell_length_b                   16.920(7)
_cell_length_c                   19.864(9)
_cell_angle_alpha                90
_cell_angle_beta                 106.052(10)
_cell_angle_gamma                90
_cell_volume                     3947(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7809
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.06
_cell_measurement_theta_min      2.41
_shelx_estimated_absorpt_T_max   0.598
_shelx_estimated_absorpt_T_min   0.558
_exptl_absorpt_coefficient_mu    2.871
_exptl_absorpt_correction_T_max  0.4950
_exptl_absorpt_correction_T_min  0.4342

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            100238
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.454
_diffrn_reflns_theta_min         1.608
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11834
_reflns_number_total             13638
_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 (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        
'SAINT V8.35A (Bruker AXS, 1997-2013),SADABS-2014_5 (Sheldrick and Bruker AXS, 1997-2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.111
_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     461
_refine_ls_number_reflns         13638
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0223
_refine_ls_restrained_S_all      1.045
_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)+(0.0186P)²+4.0510P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0500
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C51A-Cl1A \\sim C51A-Cl2A \\sim C51B-Cl1B \\sim C51B-Cl2B
 with sigma of 0.02
 Cl1A-Cl2A \\sim Cl1B-Cl2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1A \\sim Cl2A \\sim Cl1B \\sim Cl2B: within 1A with sigma of 0.02 and sigma
for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C51A, C51B, Cl1A, Cl2A, Cl1B, Cl2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl1B)=Sof(Cl2B)=Sof(C51B)=Sof(H51C)=Sof(H51D)=1-FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C51A)=Sof(H51A)=Sof(H51B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C20(H20A,H20B), C51A(H51A,H51B), C51B(H51C,H51D)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
I1 I 0.33433(2) 0.35770(2) 0.10837(2) 0.01903(3) Uani 1 1 d . . . . .
I2 I 0.06861(2) 0.42106(2) 0.16967(2) 0.01525(3) Uani 1 1 d . . . . .
I3 I 0.34826(2) 0.37380(2) 0.33181(2) 0.01413(3) Uani 1 1 d . . . . .
Zr Zr 0.29988(2) 0.46727(2) 0.21108(2) 0.01030(3) Uani 1 1 d . . . . .
P1 P 0.21644(4) 0.57831(3) 0.29176(2) 0.01170(8) Uani 1 1 d . . . . .
P2 P 0.53535(4) 0.46810(3) 0.24754(2) 0.01335(8) Uani 1 1 d . . . . .
N N 0.34889(12) 0.57756(9) 0.18713(8) 0.0130(3) Uani 1 1 d . . . . .
C1 C 0.17085(16) 0.66059(11) 0.22925(9) 0.0165(3) Uani 1 1 d . . . . .
H1A H 0.0993 0.6836 0.2347 0.020 Uiso 1 1 calc R . . . .
H1B H 0.2298 0.7025 0.2395 0.020 Uiso 1 1 calc R . . . .
C2 C 0.15250(15) 0.63212(10) 0.15560(9) 0.0145(3) Uani 1 1 d . . . . .
C3 C 0.24115(14) 0.59340(10) 0.13604(9) 0.0140(3) Uani 1 1 d . . . . .
C4 C 0.22344(17) 0.56600(13) 0.06752(10) 0.0212(4) Uani 1 1 d . . . . .
H4 H 0.2837 0.5408 0.0542 0.025 Uiso 1 1 calc R . . . .
C5 C 0.11844(19) 0.57533(15) 0.01887(11) 0.0304(5) Uani 1 1 d . . . . .
H5 H 0.1065 0.5559 -0.0275 0.037 Uiso 1 1 calc R . . . .
C6 C 0.03093(18) 0.61308(14) 0.03789(11) 0.0280(5) Uani 1 1 d . . . . .
H6 H -0.0411 0.6194 0.0046 0.034 Uiso 1 1 calc R . . . .
C7 C 0.04820(16) 0.64183(12) 0.10566(10) 0.0189(3) Uani 1 1 d . . . . .
H7 H -0.0120 0.6684 0.1180 0.023 Uiso 1 1 calc R . . . .
C8 C 0.09951(15) 0.56521(11) 0.33150(9) 0.0160(3) Uani 1 1 d . . . . .
C9 C 0.07157(18) 0.49063(12) 0.35041(11) 0.0227(4) Uani 1 1 d . . . . .
H9 H 0.1097 0.4456 0.3394 0.027 Uiso 1 1 calc R . . . .
C10 C -0.01195(19) 0.48112(12) 0.38540(12) 0.0269(4) Uani 1 1 d . . . . .
H10 H -0.0298 0.4298 0.3986 0.032 Uiso 1 1 calc R . . . .
C11 C -0.06842(19) 0.54576(13) 0.40076(13) 0.0295(5) Uani 1 1 d . . . . .
H11 H -0.1247 0.5394 0.4251 0.035 Uiso 1 1 calc R . . . .
C12 C -0.0431(3) 0.62012(15) 0.38071(18) 0.0472(8) Uani 1 1 d . . . . .
H12 H -0.0838 0.6647 0.3901 0.057 Uiso 1 1 calc R . . . .
C13 C 0.0412(2) 0.63021(13) 0.34689(15) 0.0371(6) Uani 1 1 d . . . . .
H13 H 0.0591 0.6818 0.3342 0.045 Uiso 1 1 calc R . . . .
C14 C 0.32575(15) 0.61976(10) 0.36543(9) 0.0134(3) Uani 1 1 d . . . . .
C15 C 0.37899(18) 0.69199(11) 0.36379(10) 0.0233(4) Uani 1 1 d . . . . .
H15 H 0.3567 0.7242 0.3231 0.028 Uiso 1 1 calc R . . . .
C16 C 0.4646(3) 0.71728(14) 0.42134(12) 0.0434(7) Uani 1 1 d . . . . .
H16 H 0.5013 0.7664 0.4196 0.052 Uiso 1 1 calc R . . . .
C17 C 0.4969(2) 0.67150(14) 0.48111(12) 0.0387(6) Uani 1 1 d . . . . .
H17 H 0.5550 0.6895 0.5206 0.046 Uiso 1 1 calc R . . . .
C18 C 0.44457(18) 0.59926(12) 0.48352(10) 0.0237(4) Uani 1 1 d . . . . .
H18 H 0.4670 0.5676 0.5245 0.028 Uiso 1 1 calc R . . . .
C19 C 0.35988(16) 0.57349(11) 0.42628(9) 0.0182(3) Uani 1 1 d . . . . .
H19 H 0.3243 0.5239 0.4281 0.022 Uiso 1 1 calc R . . . .
C20 C 0.55911(15) 0.55666(11) 0.30303(9) 0.0161(3) Uani 1 1 d . . . . .
H20A H 0.5123 0.5532 0.3364 0.019 Uiso 1 1 calc R . . . .
H20B H 0.6401 0.5589 0.3305 0.019 Uiso 1 1 calc R . . . .
C21 C 0.52900(15) 0.63119(10) 0.26039(10) 0.0152(3) Uani 1 1 d . . . . .
C22 C 0.42765(15) 0.64016(10) 0.20593(10) 0.0146(3) Uani 1 1 d . . . . .
C23 C 0.40669(17) 0.71265(12) 0.17062(12) 0.0230(4) Uani 1 1 d . . . . .
H23 H 0.3387 0.7194 0.1338 0.028 Uiso 1 1 calc R . . . .
C24 C 0.48323(18) 0.77443(12) 0.18840(14) 0.0296(5) Uani 1 1 d . . . . .
H24 H 0.4674 0.8231 0.1638 0.036 Uiso 1 1 calc R . . . .
C25 C 0.58271(18) 0.76576(12) 0.24177(14) 0.0289(5) Uani 1 1 d . . . . .
H25 H 0.6351 0.8083 0.2543 0.035 Uiso 1 1 calc R . . . .
C26 C 0.60487(16) 0.69447(12) 0.27659(11) 0.0223(4) Uani 1 1 d . . . . .
H26 H 0.6739 0.6883 0.3127 0.027 Uiso 1 1 calc R . . . .
C27 C 0.61472(15) 0.49417(10) 0.18534(10) 0.0161(3) Uani 1 1 d . . . . .
C28 C 0.55889(16) 0.51771(11) 0.11742(10) 0.0185(3) Uani 1 1 d . . . . .
H28 H 0.4782 0.5147 0.1014 0.022 Uiso 1 1 calc R . . . .
C29 C 0.62014(18) 0.54562(12) 0.07258(11) 0.0222(4) Uani 1 1 d . . . . .
H29 H 0.5813 0.5614 0.0262 0.027 Uiso 1 1 calc R . . . .
C30 C 0.73766(18) 0.55018(12) 0.09587(12) 0.0245(4) Uani 1 1 d . . . . .
H30 H 0.7796 0.5690 0.0654 0.029 Uiso 1 1 calc R . . . .
C31 C 0.79416(17) 0.52735(13) 0.16346(13) 0.0267(4) Uani 1 1 d . . . . .
H31 H 0.8748 0.5310 0.1793 0.032 Uiso 1 1 calc R . . . .
C32 C 0.73348(16) 0.49906(12) 0.20822(11) 0.0218(4) Uani 1 1 d . . . . .
H32 H 0.7728 0.4830 0.2544 0.026 Uiso 1 1 calc R . . . .
C33 C 0.61902(15) 0.39019(11) 0.30081(11) 0.0194(4) Uani 1 1 d . . . . .
C34 C 0.67469(17) 0.39969(14) 0.37131(12) 0.0282(4) Uani 1 1 d . . . . .
H34 H 0.6740 0.4496 0.3931 0.034 Uiso 1 1 calc R . . . .
C35 C 0.7319(2) 0.33597(16) 0.41043(14) 0.0374(6) Uani 1 1 d . . . . .
H35 H 0.7698 0.3427 0.4587 0.045 Uiso 1 1 calc R . . . .
C36 C 0.7334(2) 0.26331(15) 0.37908(15) 0.0389(6) Uani 1 1 d . . . . .
H36 H 0.7727 0.2202 0.4057 0.047 Uiso 1 1 calc R . . . .
C37 C 0.6778(2) 0.25338(14) 0.30914(15) 0.0347(5) Uani 1 1 d . . . . .
H37 H 0.6787 0.2032 0.2878 0.042 Uiso 1 1 calc R . . . .
C38 C 0.62024(17) 0.31634(12) 0.26944(12) 0.0240(4) Uani 1 1 d . . . . .
H38 H 0.5820 0.3091 0.2212 0.029 Uiso 1 1 calc R . . . .
Cl1A Cl 0.1765(4) 0.1725(2) 0.58177(16) 0.0520(7) Uani 0.613(6) 1 d D U P A 1
Cl2A Cl 0.1816(2) 0.30776(10) 0.49341(9) 0.0383(4) Uani 0.613(6) 1 d D U P A 1
C51A C 0.1009(4) 0.2255(3) 0.5071(2) 0.0436(12) Uani 0.613(6) 1 d D U P A 1
H51A H 0.0274 0.2438 0.5135 0.052 Uiso 0.613(6) 1 calc R . P A 1
H51B H 0.0844 0.1905 0.4656 0.052 Uiso 0.613(6) 1 calc R . P A 1
Cl1B Cl 0.1543(6) 0.1758(4) 0.5602(3) 0.0574(12) Uani 0.387(6) 1 d D U P A 2
Cl2B Cl 0.2219(4) 0.3257(2) 0.50677(19) 0.0456(7) Uani 0.387(6) 1 d D U P A 2
C51B C 0.2672(6) 0.2312(4) 0.5413(4) 0.0418(17) Uani 0.387(6) 1 d D U P A 2
H51C H 0.3300 0.2374 0.5849 0.050 Uiso 0.387(6) 1 calc R . P A 2
H51D H 0.2971 0.2015 0.5073 0.050 Uiso 0.387(6) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Zr 2.8727(8) . ?
I2 Zr 2.8265(11) . ?
I3 Zr 2.7959(9) . ?
Zr P1 2.8357(8) . ?
Zr P2 2.7661(12) . ?
Zr N 2.0555(16) . ?
Zr C3 2.5884(18) . ?
P1 C1 1.8459(19) . ?
P1 C8 1.8270(19) . ?
P1 C14 1.8266(18) . ?
P2 C20 1.8349(19) . ?
P2 C27 1.8234(19) . ?
P2 C33 1.8179(19) . ?
N C3 1.448(2) . ?
N C22 1.410(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.497(3) . ?
C2 C3 1.409(2) . ?
C2 C7 1.391(2) . ?
C3 C4 1.397(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.385(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.385(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.392(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.386(3) . ?
C8 C13 1.390(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.394(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.372(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.380(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.387(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(3) . ?
C14 C19 1.403(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.387(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.381(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.386(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.379(3) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.507(3) . ?
C21 C22 1.409(3) . ?
C21 C26 1.394(3) . ?
C22 C23 1.401(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.382(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.382(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.379(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.391(3) . ?
C27 C32 1.398(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.395(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.384(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.384(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.391(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.387(3) . ?
C33 C38 1.398(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.398(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.381(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.378(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.395(3) . ?
C38 H38 0.9500 . ?
Cl1A C51A 1.760(5) . ?
Cl2A C51A 1.771(5) . ?
C51A H51A 0.9900 . ?
C51A H51B 0.9900 . ?
Cl1B C51B 1.791(9) . ?
Cl2B C51B 1.767(7) . ?
C51B H51C 0.9900 . ?
C51B H51D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I2 Zr I1 86.893(18) . . ?
I2 Zr P1 82.01(2) . . ?
I3 Zr I1 101.91(3) . . ?
I3 Zr I2 92.892(14) . . ?
I3 Zr P1 85.06(3) . . ?
P1 Zr I1 167.206(12) . . ?
P2 Zr I1 80.976(16) . . ?
P2 Zr I2 164.063(14) . . ?
P2 Zr I3 79.653(13) . . ?
P2 Zr P1 111.05(2) . . ?
N Zr I1 108.19(5) . . ?
N Zr I2 121.04(4) . . ?
N Zr I3 134.91(4) . . ?
N Zr P1 72.70(5) . . ?
N Zr P2 72.99(4) . . ?
N Zr C3 33.93(6) . . ?
C3 Zr I1 101.23(5) . . ?
C3 Zr I2 87.98(4) . . ?
C3 Zr I3 156.85(4) . . ?
C3 Zr P1 72.15(5) . . ?
C3 Zr P2 104.44(4) . . ?
C1 P1 Zr 102.03(6) . . ?
C8 P1 Zr 127.60(6) . . ?
C8 P1 C1 104.80(9) . . ?
C14 P1 Zr 114.18(6) . . ?
C14 P1 C1 105.49(9) . . ?
C14 P1 C8 100.74(9) . . ?
C20 P2 Zr 98.15(6) . . ?
C27 P2 Zr 122.24(7) . . ?
C27 P2 C20 100.60(9) . . ?
C33 P2 Zr 121.71(6) . . ?
C33 P2 C20 105.81(9) . . ?
C33 P2 C27 104.53(9) . . ?
C3 N Zr 93.65(10) . . ?
C22 N Zr 147.32(12) . . ?
C22 N C3 117.93(14) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C2 C1 P1 110.51(12) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C3 C2 C1 120.01(15) . . ?
C7 C2 C1 121.26(16) . . ?
C7 C2 C3 118.73(17) . . ?
N C3 Zr 52.42(8) . . ?
C2 C3 Zr 109.65(11) . . ?
C2 C3 N 120.80(15) . . ?
C4 C3 Zr 103.36(13) . . ?
C4 C3 N 119.17(16) . . ?
C4 C3 C2 119.94(16) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.40(18) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.88(19) . . ?
C6 C5 H5 120.1 . . ?
C5 C6 H6 119.9 . . ?
C5 C6 C7 120.22(18) . . ?
C7 C6 H6 119.9 . . ?
C2 C7 C6 120.82(18) . . ?
C2 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C9 C8 P1 120.55(14) . . ?
C9 C8 C13 118.75(18) . . ?
C13 C8 P1 120.60(15) . . ?
C8 C9 H9 119.7 . . ?
C8 C9 C10 120.63(18) . . ?
C10 C9 H9 119.7 . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.11(19) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 H11 120.1 . . ?
C10 C11 C12 119.74(19) . . ?
C12 C11 H11 120.1 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.5(2) . . ?
C13 C12 H12 119.8 . . ?
C8 C13 H13 119.9 . . ?
C12 C13 C8 120.3(2) . . ?
C12 C13 H13 119.9 . . ?
C15 C14 P1 124.22(14) . . ?
C15 C14 C19 118.78(16) . . ?
C19 C14 P1 116.96(13) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 C14 120.24(18) . . ?
C16 C15 H15 119.9 . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.4(2) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.0(2) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 120.1 . . ?
C19 C18 C17 119.89(18) . . ?
C19 C18 H18 120.1 . . ?
C14 C19 H19 119.7 . . ?
C18 C19 C14 120.68(17) . . ?
C18 C19 H19 119.7 . . ?
P2 C20 H20A 109.2 . . ?
P2 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C21 C20 P2 111.85(13) . . ?
C21 C20 H20A 109.2 . . ?
C21 C20 H20B 109.2 . . ?
C22 C21 C20 123.21(16) . . ?
C26 C21 C20 117.99(17) . . ?
C26 C21 C22 118.79(17) . . ?
C21 C22 N 120.86(15) . . ?
C23 C22 N 120.53(17) . . ?
C23 C22 C21 118.61(17) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 C22 121.14(19) . . ?
C24 C23 H23 119.4 . . ?
C23 C24 H24 119.8 . . ?
C23 C24 C25 120.35(19) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 120.4 . . ?
C26 C25 C24 119.11(19) . . ?
C26 C25 H25 120.4 . . ?
C21 C26 H26 119.0 . . ?
C25 C26 C21 122.00(19) . . ?
C25 C26 H26 119.0 . . ?
C28 C27 P2 121.09(14) . . ?
C28 C27 C32 119.01(17) . . ?
C32 C27 P2 119.53(15) . . ?
C27 C28 H28 119.7 . . ?
C27 C28 C29 120.70(18) . . ?
C29 C28 H28 119.7 . . ?
C28 C29 H29 120.1 . . ?
C30 C29 C28 119.7(2) . . ?
C30 C29 H29 120.1 . . ?
C29 C30 H30 119.9 . . ?
C29 C30 C31 120.13(18) . . ?
C31 C30 H30 119.9 . . ?
C30 C31 H31 119.8 . . ?
C30 C31 C32 120.34(19) . . ?
C32 C31 H31 119.8 . . ?
C27 C32 H32 120.0 . . ?
C31 C32 C27 120.1(2) . . ?
C31 C32 H32 120.0 . . ?
C34 C33 P2 122.93(16) . . ?
C34 C33 C38 119.41(19) . . ?
C38 C33 P2 117.53(16) . . ?
C33 C34 H34 119.9 . . ?
C33 C34 C35 120.1(2) . . ?
C35 C34 H34 119.9 . . ?
C34 C35 H35 119.9 . . ?
C36 C35 C34 120.2(2) . . ?
C36 C35 H35 119.9 . . ?
C35 C36 H36 120.0 . . ?
C37 C36 C35 119.9(2) . . ?
C37 C36 H36 120.0 . . ?
C36 C37 H37 119.7 . . ?
C36 C37 C38 120.5(2) . . ?
C38 C37 H37 119.7 . . ?
C33 C38 H38 120.1 . . ?
C37 C38 C33 119.8(2) . . ?
C37 C38 H38 120.1 . . ?
Cl1A C51A Cl2A 110.2(3) . . ?
Cl1A C51A H51A 109.6 . . ?
Cl1A C51A H51B 109.6 . . ?
Cl2A C51A H51A 109.6 . . ?
Cl2A C51A H51B 109.6 . . ?
H51A C51A H51B 108.1 . . ?
Cl1B C51B H51C 109.2 . . ?
Cl1B C51B H51D 109.2 . . ?
Cl2B C51B Cl1B 112.2(4) . . ?
Cl2B C51B H51C 109.2 . . ?
Cl2B C51B H51D 109.2 . . ?
H51C C51B H51D 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr P1 C1 C2 20.45(13) . . . . ?
Zr P1 C8 C9 27.3(2) . . . . ?
Zr P1 C8 C13 -156.30(17) . . . . ?
Zr P1 C14 C15 97.26(17) . . . . ?
Zr P1 C14 C19 -80.36(15) . . . . ?
Zr P2 C20 C21 -72.89(12) . . . . ?
Zr P2 C27 C28 2.51(18) . . . . ?
Zr P2 C27 C32 175.40(12) . . . . ?
Zr P2 C33 C34 -103.24(16) . . . . ?
Zr P2 C33 C38 72.59(16) . . . . ?
Zr N C3 C2 92.02(16) . . . . ?
Zr N C3 C4 -84.51(17) . . . . ?
Zr N C22 C21 9.8(3) . . . . ?
Zr N C22 C23 -170.37(17) . . . . ?
Zr C3 C4 C5 121.2(2) . . . . ?
P1 C1 C2 C3 -56.1(2) . . . . ?
P1 C1 C2 C7 122.77(16) . . . . ?
P1 C8 C9 C10 175.24(17) . . . . ?
P1 C8 C13 C12 -176.3(2) . . . . ?
P1 C14 C15 C16 -177.3(2) . . . . ?
P1 C14 C19 C18 177.89(16) . . . . ?
P2 C20 C21 C22 46.3(2) . . . . ?
P2 C20 C21 C26 -134.62(15) . . . . ?
P2 C27 C28 C29 173.08(15) . . . . ?
P2 C27 C32 C31 -172.82(16) . . . . ?
P2 C33 C34 C35 176.04(17) . . . . ?
P2 C33 C38 C37 -176.36(16) . . . . ?
N C3 C4 C5 175.37(19) . . . . ?
N C22 C23 C24 -179.88(19) . . . . ?
C1 P1 C8 C9 145.72(16) . . . . ?
C1 P1 C8 C13 -37.9(2) . . . . ?
C1 P1 C14 C15 -13.93(19) . . . . ?
C1 P1 C14 C19 168.44(14) . . . . ?
C1 C2 C3 Zr 59.95(18) . . . . ?
C1 C2 C3 N 2.7(3) . . . . ?
C1 C2 C3 C4 179.21(17) . . . . ?
C1 C2 C7 C6 -178.08(19) . . . . ?
C2 C3 C4 C5 -1.2(3) . . . . ?
C3 N C22 C21 173.45(16) . . . . ?
C3 N C22 C23 -6.7(2) . . . . ?
C3 C2 C7 C6 0.8(3) . . . . ?
C3 C4 C5 C6 1.0(4) . . . . ?
C4 C5 C6 C7 0.2(4) . . . . ?
C5 C6 C7 C2 -1.1(3) . . . . ?
C7 C2 C3 Zr -118.96(16) . . . . ?
C7 C2 C3 N -176.20(16) . . . . ?
C7 C2 C3 C4 0.3(3) . . . . ?
C8 P1 C1 C2 -114.11(13) . . . . ?
C8 P1 C14 C15 -122.75(17) . . . . ?
C8 P1 C14 C19 59.63(16) . . . . ?
C8 C9 C10 C11 0.8(3) . . . . ?
C9 C8 C13 C12 0.2(4) . . . . ?
C9 C10 C11 C12 0.8(4) . . . . ?
C10 C11 C12 C13 -1.8(5) . . . . ?
C11 C12 C13 C8 1.4(5) . . . . ?
C13 C8 C9 C10 -1.2(3) . . . . ?
C14 P1 C1 C2 140.02(13) . . . . ?
C14 P1 C8 C9 -104.93(17) . . . . ?
C14 P1 C8 C13 71.5(2) . . . . ?
C14 C15 C16 C17 -0.8(4) . . . . ?
C15 C14 C19 C18 0.1(3) . . . . ?
C15 C16 C17 C18 0.8(5) . . . . ?
C16 C17 C18 C19 -0.4(4) . . . . ?
C17 C18 C19 C14 -0.1(3) . . . . ?
C19 C14 C15 C16 0.3(3) . . . . ?
C20 P2 C27 C28 -104.27(16) . . . . ?
C20 P2 C27 C32 68.62(16) . . . . ?
C20 P2 C33 C34 7.14(19) . . . . ?
C20 P2 C33 C38 -177.03(14) . . . . ?
C20 C21 C22 N -1.6(3) . . . . ?
C20 C21 C22 C23 178.52(17) . . . . ?
C20 C21 C26 C25 -178.01(18) . . . . ?
C21 C22 C23 C24 0.0(3) . . . . ?
C22 N C3 Zr -171.26(17) . . . . ?
C22 N C3 C2 -79.2(2) . . . . ?
C22 N C3 C4 104.2(2) . . . . ?
C22 C21 C26 C25 1.1(3) . . . . ?
C22 C23 C24 C25 0.0(3) . . . . ?
C23 C24 C25 C26 0.5(3) . . . . ?
C24 C25 C26 C21 -1.1(3) . . . . ?
C26 C21 C22 N 179.32(16) . . . . ?
C26 C21 C22 C23 -0.6(3) . . . . ?
C27 P2 C20 C21 52.23(14) . . . . ?
C27 P2 C33 C34 112.86(17) . . . . ?
C27 P2 C33 C38 -71.31(16) . . . . ?
C27 C28 C29 C30 -0.2(3) . . . . ?
C28 C27 C32 C31 0.2(3) . . . . ?
C28 C29 C30 C31 -0.2(3) . . . . ?
C29 C30 C31 C32 0.6(3) . . . . ?
C30 C31 C32 C27 -0.6(3) . . . . ?
C32 C27 C28 C29 0.2(3) . . . . ?
C33 P2 C20 C21 160.78(12) . . . . ?
C33 P2 C27 C28 146.16(15) . . . . ?
C33 P2 C27 C32 -40.95(17) . . . . ?
C33 C34 C35 C36 0.1(3) . . . . ?
C34 C33 C38 C37 -0.4(3) . . . . ?
C34 C35 C36 C37 -0.4(4) . . . . ?
C35 C36 C37 C38 0.3(3) . . . . ?
C36 C37 C38 C33 0.1(3) . . . . ?
C38 C33 C34 C35 0.3(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            CCD-PXL-KAF2
####################################################################### 
# 
# 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_ba_sb57
_database_code_depnum_ccdc_archive 'CCDC 1530466'
_audit_update_record             
;
2017-03-17 deposited with the CCDC.
2017-04-05 downloaded from the CCDC.
;
_audit_creation_date             2016-04-11

_audit_block_code                ba_sb57
_audit_block_refno               2698
_audit_block_usercomment         sb_dh_04


# start Validation Reply Form
_vrf_PLAT910_ba_sb57             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          13 Note
RESPONSE: limited by diffractometer.
;
# end Validation Reply Form

_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C44 H50 Hf N4 P2'
_chemical_formula_sum            'C44 H50 Hf N4 P2'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         875.31
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            'light yellow'
_diffrn_ambient_temperature      120(1)
_chemical_oxdiff_formula         'C44 H50 N4 P Hf'
_chemical_oxdiff_usercomment     sb_dh_04
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'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration .

_space_group_name_Hall           '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.47419(13)
_cell_length_b                   12.67913(18)
_cell_length_c                   14.64329(19)
_cell_angle_alpha                81.2172(11)
_cell_angle_beta                 85.5974(9)
_cell_angle_gamma                61.4891(12)
_cell_volume                     2011.26(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    52008
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      32.0980
_cell_measurement_theta_min      3.3040
_shelx_estimated_absorpt_T_max   0.773
_shelx_estimated_absorpt_T_min   0.773
_exptl_absorpt_coefficient_mu    2.708
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41p (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             888
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 -15 -13 0.0500
3 0 20 0.0427
-3 -16 5 0.0351
-7 -17 2 0.0377
5 11 -14 0.0333
-2 -1 20 0.0373
-14 -12 -12 0.0551
14 12 12 0.0551
7 -10 -8 0.0502
-12 6 4 0.0630
4 15 13 0.0500
7 -7 12 0.0490
-8 0 18 0.0403
-12 -17 -2 0.0369
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.079
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.9958 -15.0413 -12.9431 -0.0206 0.0723 0.9985
3.0300 0.0794 20.0147 -0.8389 0.2211 -0.4942
-2.9684 -15.9709 5.0739 -0.8093 0.1855 0.5860
-6.9741 -16.9858 2.0747 -0.7124 -0.0522 0.6771
4.9660 10.9430 -14.0566 0.9878 0.0458 -0.1046
-1.9722 -0.9252 20.0170 -0.8641 -0.0764 -0.4892
-14.0073 -12.0508 -11.9601 0.0778 -0.6372 0.7512
14.0073 12.0508 11.9601 -0.0778 0.6372 -0.7512
7.0113 -10.0146 -7.9575 -0.0663 0.6693 0.7282
-12.0140 5.9972 3.9707 0.0931 -0.9031 -0.4806
3.9958 15.0413 12.9431 0.0206 -0.0723 -0.9985
7.0000 -7.0000 12.0000 -0.7836 0.6276 0.0740
-8.0000 -0.0000 18.0000 -0.7293 -0.4872 -0.5303
-12.0000 -17.0000 -2.0000 -0.5301 -0.3800 0.7410

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            128166
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.437
_diffrn_reflns_theta_min         3.155
_diffrn_ambient_environment      perfluoro
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  97.00   0.50   20.00    --   26.43  77.00-120.00  202
  2  ω      1.00  99.00   0.50   20.00    --   26.43  38.00 150.00  196
  3  ω      5.00  95.00   0.50   20.00    --   26.43  57.00   0.00  180
  4  ω    -42.00  47.00   0.50   20.00    --   26.43 -57.00 -30.00  178
  5  ω    -42.00  47.00   0.50   20.00    --   26.43 -57.00 120.00  178
  6  ω     -4.00  97.00   0.50   20.00    --   26.43  77.00  90.00  202
  7  ω    -20.00  68.00   0.50   20.00    --   26.43 -99.00 -90.00  176
  8  ω    -46.00  52.00   0.50   20.00    --   26.43 -38.00  30.00  196
  9  ω     -4.00  97.00   0.50   20.00    --   26.43  77.00  30.00  202
 10  ω    -20.00  68.00   0.50   20.00    --   26.43 -99.00-150.00  176
 11  ω    -20.00  68.00   0.50   20.00    --   26.43 -99.00 -60.00  176
 12  ω      1.00  99.00   0.50   20.00    --   26.43  38.00 -30.00  196
 13  ω     -4.00  97.00   0.50   20.00    --   26.43  77.00-180.00  202
 14  ω     -4.00  97.00   0.50   20.00    --   26.43  77.00 -60.00  202
 15  ω      6.00  88.00   0.50   20.00    --   26.43-132.00 114.45  164
 16  φ      0.00 120.00   0.50   20.00  26.43  26.43  40.00    --   240
 17  φ      0.00 120.00   0.50   20.00  26.43  26.43 -60.00    --   240
 18  φ      0.00 120.00   0.50   20.00  26.43  26.43  60.00    --   240
 19  φ    120.00 240.00   0.50   20.00  26.43  26.43 -40.00    --   240
 20  φ    120.00 240.00   0.50   20.00  26.43  26.43  40.00    --   240
 21  φ    120.00 240.00   0.50   20.00  26.43  26.43 -60.00    --   240
 22  φ    120.00 240.00   0.50   20.00  26.43  26.43  60.00    --   240
 23  φ    240.00 360.00   0.50   20.00  26.43  26.43 -40.00    --   240
 24  φ    240.00 360.00   0.50   20.00  26.43  26.43  40.00    --   240
 25  φ    240.00 310.00   0.50   20.00  26.43  26.43 -60.00    --   140
 26  φ      0.00 120.00   0.50   20.00  26.43  26.43 -40.00    --   240
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0025937000
_diffrn_orient_matrix_UB_12      0.0379168000
_diffrn_orient_matrix_UB_13      -0.0416707000
_diffrn_orient_matrix_UB_21      0.0641211000
_diffrn_orient_matrix_UB_22      -0.0230768000
_diffrn_orient_matrix_UB_23      0.0014332000
_diffrn_orient_matrix_UB_31      0.0083116000
_diffrn_orient_matrix_UB_32      -0.0464233000
_diffrn_orient_matrix_UB_33      -0.0257653000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12875
_reflns_number_total             13994
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         13994
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0237
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0198P)²+1.7199P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0527
_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), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
2.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Hf Hf 0.11888(2) 0.67431(2) 0.16660(2) 0.01536(2) Uani 1 1 d . . . . .
P1 P 0.24066(4) 0.40052(4) 0.21655(3) 0.01586(8) Uani 1 1 d . . . . .
P2 P 0.32560(4) 0.79654(4) 0.40054(3) 0.01642(8) Uani 1 1 d . . . . .
N1 N 0.27136(13) 0.61848(14) 0.25314(10) 0.0163(3) Uani 1 1 d . . . . .
N2 N 0.08208(15) 0.85116(14) 0.14616(11) 0.0214(3) Uani 1 1 d . . . . .
N3 N -0.04894(14) 0.69106(15) 0.20634(11) 0.0212(3) Uani 1 1 d . . . . .
N4 N 0.14546(15) 0.64221(14) 0.03191(10) 0.0197(3) Uani 1 1 d . . . . .
C1 C 0.33108(17) 0.37395(16) 0.32085(12) 0.0195(3) Uani 1 1 d . . . . .
H1A H 0.3506 0.2941 0.3566 0.023 Uiso 1 1 calc R . . . .
H1B H 0.4084 0.3756 0.3028 0.023 Uiso 1 1 calc R . . . .
C2 C 0.25376(17) 0.47380(17) 0.37777(12) 0.0190(3) Uani 1 1 d . . . . .
C3 C 0.22452(16) 0.59421(16) 0.34106(12) 0.0171(3) Uani 1 1 d . . . . .
C4 C 0.13786(18) 0.68998(18) 0.38648(13) 0.0225(4) Uani 1 1 d . . . . .
H4 H 0.1128 0.7713 0.3596 0.027 Uiso 1 1 calc R . . . .
C5 C 0.0882(2) 0.6666(2) 0.47095(15) 0.0311(4) Uani 1 1 d . . . . .
H5 H 0.0312 0.7318 0.5021 0.037 Uiso 1 1 calc R . . . .
C6 C 0.1220(2) 0.5488(2) 0.50915(14) 0.0339(5) Uani 1 1 d . . . . .
H6 H 0.0902 0.5330 0.5677 0.041 Uiso 1 1 calc R . . . .
C7 C 0.2024(2) 0.4527(2) 0.46234(13) 0.0279(4) Uani 1 1 d . . . . .
H7 H 0.2225 0.3721 0.4881 0.033 Uiso 1 1 calc R . . . .
C8 C 0.35174(16) 0.29831(16) 0.13928(12) 0.0180(3) Uani 1 1 d . . . . .
C9 C 0.31280(18) 0.24730(17) 0.07920(13) 0.0231(4) Uani 1 1 d . . . . .
H9 H 0.2304 0.2624 0.0814 0.028 Uiso 1 1 calc R . . . .
C10 C 0.39376(19) 0.17474(18) 0.01633(14) 0.0256(4) Uani 1 1 d . . . . .
H10 H 0.3659 0.1414 -0.0244 0.031 Uiso 1 1 calc R . . . .
C11 C 0.51417(19) 0.15091(18) 0.01272(14) 0.0262(4) Uani 1 1 d . . . . .
H11 H 0.5693 0.1009 -0.0299 0.031 Uiso 1 1 calc R . . . .
C12 C 0.55384(19) 0.2007(2) 0.07184(14) 0.0272(4) Uani 1 1 d . . . . .
H12 H 0.6366 0.1842 0.0699 0.033 Uiso 1 1 calc R . . . .
C13 C 0.47327(18) 0.27452(18) 0.13409(13) 0.0233(4) Uani 1 1 d . . . . .
H13 H 0.5014 0.3091 0.1735 0.028 Uiso 1 1 calc R . . . .
C14 C 0.15075(16) 0.32269(16) 0.25482(12) 0.0173(3) Uani 1 1 d . . . . .
C15 C 0.20524(18) 0.19964(17) 0.29130(14) 0.0232(4) Uani 1 1 d . . . . .
H15 H 0.2911 0.1554 0.2997 0.028 Uiso 1 1 calc R . . . .
C16 C 0.13400(18) 0.14246(17) 0.31522(14) 0.0245(4) Uani 1 1 d . . . . .
H16 H 0.1716 0.0588 0.3387 0.029 Uiso 1 1 calc R . . . .
C17 C 0.00817(18) 0.20686(18) 0.30498(13) 0.0236(4) Uani 1 1 d . . . . .
H17 H -0.0403 0.1677 0.3227 0.028 Uiso 1 1 calc R . . . .
C18 C -0.04678(18) 0.32850(18) 0.26881(14) 0.0235(4) Uani 1 1 d . . . . .
H18 H -0.1328 0.3725 0.2614 0.028 Uiso 1 1 calc R . . . .
C19 C 0.02452(16) 0.38598(16) 0.24342(13) 0.0198(3) Uani 1 1 d . . . . .
H19 H -0.0133 0.4690 0.2181 0.024 Uiso 1 1 calc R . . . .
C20 C 0.42905(16) 0.63137(15) 0.40010(12) 0.0171(3) Uani 1 1 d . . . . .
H20A H 0.5023 0.6061 0.4374 0.021 Uiso 1 1 calc R . . . .
H20B H 0.3867 0.5853 0.4285 0.021 Uiso 1 1 calc R . . . .
C21 C 0.46727(15) 0.60286(15) 0.30262(11) 0.0157(3) Uani 1 1 d . . . . .
C22 C 0.39166(15) 0.59737(15) 0.23792(11) 0.0150(3) Uani 1 1 d . . . . .
C23 C 0.43742(17) 0.57719(16) 0.14741(12) 0.0191(3) Uani 1 1 d . . . . .
H23 H 0.3890 0.5707 0.1038 0.023 Uiso 1 1 calc R . . . .
C24 C 0.55078(17) 0.56661(17) 0.12017(13) 0.0218(3) Uani 1 1 d . . . . .
H24 H 0.5782 0.5547 0.0584 0.026 Uiso 1 1 calc R . . . .
C25 C 0.62436(17) 0.57339(17) 0.18341(14) 0.0228(4) Uani 1 1 d . . . . .
H25 H 0.7019 0.5667 0.1654 0.027 Uiso 1 1 calc R . . . .
C26 C 0.58214(16) 0.59014(16) 0.27318(13) 0.0198(3) Uani 1 1 d . . . . .
H26 H 0.6331 0.5931 0.3166 0.024 Uiso 1 1 calc R . . . .
C27 C 0.43220(17) 0.85765(16) 0.36726(12) 0.0189(3) Uani 1 1 d . . . . .
C28 C 0.43866(18) 0.89569(18) 0.27324(13) 0.0235(4) Uani 1 1 d . . . . .
H28 H 0.3916 0.8859 0.2304 0.028 Uiso 1 1 calc R . . . .
C29 C 0.51281(19) 0.94766(19) 0.24138(15) 0.0286(4) Uani 1 1 d . . . . .
H29 H 0.5165 0.9728 0.1772 0.034 Uiso 1 1 calc R . . . .
C30 C 0.5811(2) 0.9626(2) 0.30318(17) 0.0315(4) Uani 1 1 d . . . . .
H30 H 0.6305 0.9997 0.2817 0.038 Uiso 1 1 calc R . . . .
C31 C 0.5774(2) 0.9235(2) 0.39655(17) 0.0353(5) Uani 1 1 d . . . . .
H31 H 0.6255 0.9329 0.4388 0.042 Uiso 1 1 calc R . . . .
C32 C 0.50389(19) 0.8707(2) 0.42877(14) 0.0273(4) Uani 1 1 d . . . . .
H32 H 0.5025 0.8435 0.4928 0.033 Uiso 1 1 calc R . . . .
C33 C 0.30474(16) 0.80821(16) 0.52452(12) 0.0171(3) Uani 1 1 d . . . . .
C34 C 0.23165(18) 0.92367(17) 0.55108(13) 0.0228(4) Uani 1 1 d . . . . .
H34 H 0.1983 0.9921 0.5049 0.027 Uiso 1 1 calc R . . . .
C35 C 0.20719(18) 0.93967(17) 0.64361(14) 0.0243(4) Uani 1 1 d . . . . .
H35 H 0.1580 1.0185 0.6603 0.029 Uiso 1 1 calc R . . . .
C36 C 0.25501(17) 0.83978(18) 0.71176(13) 0.0224(3) Uani 1 1 d . . . . .
H36 H 0.2394 0.8505 0.7751 0.027 Uiso 1 1 calc R . . . .
C37 C 0.32552(17) 0.72457(17) 0.68688(13) 0.0210(3) Uani 1 1 d . . . . .
H37 H 0.3571 0.6561 0.7332 0.025 Uiso 1 1 calc R . . . .
C38 C 0.34995(17) 0.70941(16) 0.59415(12) 0.0196(3) Uani 1 1 d . . . . .
H38 H 0.3984 0.6302 0.5778 0.024 Uiso 1 1 calc R . . . .
C39 C -0.0354(2) 0.9571(2) 0.1393(2) 0.0417(6) Uani 1 1 d . . . . .
H39A H -0.0473 0.9995 0.0761 0.062 Uiso 1 1 calc GR . . . .
H39B H -0.0397 1.0109 0.1825 0.062 Uiso 1 1 calc GR . . . .
H39C H -0.0992 0.9331 0.1546 0.062 Uiso 1 1 calc GR . . . .
C40 C 0.1771(2) 0.8883(2) 0.13546(17) 0.0333(5) Uani 1 1 d . . . . .
H40A H 0.1702 0.9344 0.1856 0.050 Uiso 1 1 calc GR . . . .
H40B H 0.1673 0.9391 0.0759 0.050 Uiso 1 1 calc GR . . . .
H40C H 0.2574 0.8164 0.1377 0.050 Uiso 1 1 calc GR . . . .
C41 C -0.10261(19) 0.6766(2) 0.29607(14) 0.0272(4) Uani 1 1 d . . . . .
H41A H -0.0376 0.6277 0.3414 0.041 Uiso 1 1 calc GR . . . .
H41B H -0.1516 0.6360 0.2916 0.041 Uiso 1 1 calc GR . . . .
H41C H -0.1548 0.7564 0.3157 0.041 Uiso 1 1 calc GR . . . .
C42 C -0.14145(19) 0.7410(2) 0.13421(16) 0.0308(4) Uani 1 1 d . . . . .
H42A H -0.2091 0.8177 0.1495 0.046 Uiso 1 1 calc GR . . . .
H42B H -0.1719 0.6836 0.1299 0.046 Uiso 1 1 calc GR . . . .
H42C H -0.1054 0.7554 0.0749 0.046 Uiso 1 1 calc GR . . . .
C43 C 0.1084(2) 0.56116(18) -0.00070(13) 0.0248(4) Uani 1 1 d . . . . .
H43A H 0.0800 0.5229 0.0518 0.037 Uiso 1 1 calc GR . . . .
H43B H 0.1781 0.4986 -0.0302 0.037 Uiso 1 1 calc GR . . . .
H43C H 0.0422 0.6077 -0.0456 0.037 Uiso 1 1 calc GR . . . .
C44 C 0.1719(2) 0.71255(18) -0.04584(13) 0.0268(4) Uani 1 1 d . . . . .
H44A H 0.0999 0.7584 -0.0854 0.040 Uiso 1 1 calc GR . . . .
H44B H 0.2404 0.6579 -0.0816 0.040 Uiso 1 1 calc GR . . . .
H44C H 0.1934 0.7688 -0.0229 0.040 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
Hf P1 3.0420(4) . ?
Hf N1 2.1297(14) . ?
Hf N2 2.0401(16) . ?
Hf N3 2.0476(16) . ?
Hf N4 2.0448(15) . ?
Hf C3 2.7824(17) . ?
P1 C1 1.8608(18) . ?
P1 C8 1.8366(18) . ?
P1 C14 1.8268(18) . ?
P2 C20 1.8639(17) . ?
P2 C27 1.8370(19) . ?
P2 C33 1.8326(18) . ?
N1 C3 1.424(2) . ?
N1 C22 1.399(2) . ?
N2 C39 1.436(3) . ?
N2 C40 1.460(3) . ?
N3 C41 1.455(3) . ?
N3 C42 1.461(3) . ?
N4 C43 1.461(2) . ?
N4 C44 1.454(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.504(3) . ?
C2 C3 1.414(3) . ?
C2 C7 1.399(3) . ?
C3 C4 1.403(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.395(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.380(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.394(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.403(2) . ?
C8 C13 1.396(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.394(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.382(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.387(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.393(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.404(2) . ?
C14 C19 1.394(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.389(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.389(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.388(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.395(3) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.511(2) . ?
C21 C22 1.418(2) . ?
C21 C26 1.404(2) . ?
C22 C23 1.413(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.387(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.392(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.387(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.397(3) . ?
C27 C32 1.396(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.389(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.380(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.386(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.391(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.404(2) . ?
C33 C38 1.397(2) . ?
C34 H34 0.9500 . ?
C34 C35 1.390(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.393(3) . ?
C36 H36 0.9500 . ?
C36 C37 1.388(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.391(2) . ?
C38 H38 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
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 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 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
N1 Hf P1 70.97(4) . . ?
N1 Hf C3 30.14(5) . . ?
N2 Hf P1 163.99(5) . . ?
N2 Hf N1 93.57(6) . . ?
N2 Hf N3 101.14(6) . . ?
N2 Hf N4 98.62(6) . . ?
N2 Hf C3 102.34(6) . . ?
N3 Hf P1 91.87(5) . . ?
N3 Hf N1 127.18(6) . . ?
N3 Hf C3 97.04(6) . . ?
N4 Hf P1 86.15(4) . . ?
N4 Hf N1 120.09(6) . . ?
N4 Hf N3 107.46(6) . . ?
N4 Hf C3 143.82(6) . . ?
C3 Hf P1 66.46(4) . . ?
C1 P1 Hf 103.08(6) . . ?
C8 P1 Hf 121.77(6) . . ?
C8 P1 C1 104.03(8) . . ?
C14 P1 Hf 121.09(6) . . ?
C14 P1 C1 103.09(8) . . ?
C14 P1 C8 101.20(8) . . ?
C27 P2 C20 100.93(8) . . ?
C33 P2 C20 101.94(8) . . ?
C33 P2 C27 102.34(8) . . ?
C3 N1 Hf 101.19(10) . . ?
C22 N1 Hf 134.74(11) . . ?
C22 N1 C3 123.89(14) . . ?
C39 N2 Hf 127.73(15) . . ?
C39 N2 C40 109.14(17) . . ?
C40 N2 Hf 123.13(13) . . ?
C41 N3 Hf 132.90(13) . . ?
C41 N3 C42 110.33(16) . . ?
C42 N3 Hf 116.31(13) . . ?
C43 N4 Hf 120.82(12) . . ?
C44 N4 Hf 127.08(12) . . ?
C44 N4 C43 110.45(15) . . ?
P1 C1 H1A 110.4 . . ?
P1 C1 H1B 110.4 . . ?
H1A C1 H1B 108.6 . . ?
C2 C1 P1 106.76(12) . . ?
C2 C1 H1A 110.4 . . ?
C2 C1 H1B 110.4 . . ?
C3 C2 C1 118.67(15) . . ?
C7 C2 C1 122.17(17) . . ?
C7 C2 C3 118.98(17) . . ?
N1 C3 Hf 48.67(8) . . ?
C2 C3 Hf 115.82(11) . . ?
C2 C3 N1 120.00(15) . . ?
C4 C3 Hf 98.17(12) . . ?
C4 C3 N1 120.20(16) . . ?
C4 C3 C2 119.35(16) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.42(19) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 119.99(19) . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.37(19) . . ?
C7 C6 H6 119.8 . . ?
C2 C7 H7 119.7 . . ?
C6 C7 C2 120.7(2) . . ?
C6 C7 H7 119.7 . . ?
C9 C8 P1 119.48(14) . . ?
C13 C8 P1 122.24(14) . . ?
C13 C8 C9 118.17(17) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 C8 120.65(18) . . ?
C10 C9 H9 119.7 . . ?
C9 C10 H10 119.7 . . ?
C11 C10 C9 120.51(18) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 H11 120.3 . . ?
C10 C11 C12 119.40(18) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 H12 119.7 . . ?
C11 C12 C13 120.52(19) . . ?
C13 C12 H12 119.7 . . ?
C8 C13 H13 119.6 . . ?
C12 C13 C8 120.74(18) . . ?
C12 C13 H13 119.6 . . ?
C15 C14 P1 122.05(14) . . ?
C19 C14 P1 118.96(13) . . ?
C19 C14 C15 118.92(17) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 C14 120.18(17) . . ?
C16 C15 H15 119.9 . . ?
C15 C16 H16 119.8 . . ?
C15 C16 C17 120.40(18) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 119.96(18) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 120.1 . . ?
C17 C18 C19 119.88(18) . . ?
C19 C18 H18 120.1 . . ?
C14 C19 C18 120.64(17) . . ?
C14 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
P2 C20 H20A 109.5 . . ?
P2 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
C21 C20 P2 110.74(11) . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
C22 C21 C20 124.39(15) . . ?
C26 C21 C20 116.87(15) . . ?
C26 C21 C22 118.56(15) . . ?
N1 C22 C21 126.02(15) . . ?
N1 C22 C23 115.95(15) . . ?
C23 C22 C21 117.87(15) . . ?
C22 C23 H23 118.9 . . ?
C24 C23 C22 122.12(17) . . ?
C24 C23 H23 118.9 . . ?
C23 C24 H24 120.0 . . ?
C23 C24 C25 119.96(17) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 120.7 . . ?
C26 C25 C24 118.67(17) . . ?
C26 C25 H25 120.7 . . ?
C21 C26 H26 118.6 . . ?
C25 C26 C21 122.79(17) . . ?
C25 C26 H26 118.6 . . ?
C28 C27 P2 116.51(14) . . ?
C32 C27 P2 124.89(14) . . ?
C32 C27 C28 118.58(17) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 C27 121.00(19) . . ?
C29 C28 H28 119.5 . . ?
C28 C29 H29 120.1 . . ?
C30 C29 C28 119.8(2) . . ?
C30 C29 H29 120.1 . . ?
C29 C30 H30 120.0 . . ?
C29 C30 C31 120.0(2) . . ?
C31 C30 H30 120.0 . . ?
C30 C31 H31 119.8 . . ?
C30 C31 C32 120.4(2) . . ?
C32 C31 H31 119.8 . . ?
C27 C32 H32 119.9 . . ?
C31 C32 C27 120.16(19) . . ?
C31 C32 H32 119.9 . . ?
C34 C33 P2 117.63(13) . . ?
C38 C33 P2 124.47(13) . . ?
C38 C33 C34 117.76(16) . . ?
C33 C34 H34 119.4 . . ?
C35 C34 C33 121.22(17) . . ?
C35 C34 H34 119.4 . . ?
C34 C35 H35 120.1 . . ?
C34 C35 C36 119.84(17) . . ?
C36 C35 H35 120.1 . . ?
C35 C36 H36 120.1 . . ?
C37 C36 C35 119.84(17) . . ?
C37 C36 H36 120.1 . . ?
C36 C37 H37 120.0 . . ?
C36 C37 C38 119.95(17) . . ?
C38 C37 H37 120.0 . . ?
C33 C38 H38 119.3 . . ?
C37 C38 C33 121.37(17) . . ?
C37 C38 H38 119.3 . . ?
N2 C39 H39A 109.5 . . ?
N2 C39 H39B 109.5 . . ?
N2 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N2 C40 H40A 109.5 . . ?
N2 C40 H40B 109.5 . . ?
N2 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N3 C41 H41A 109.5 . . ?
N3 C41 H41B 109.5 . . ?
N3 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N3 C42 H42A 109.5 . . ?
N3 C42 H42B 109.5 . . ?
N3 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N4 C43 H43A 109.5 . . ?
N4 C43 H43B 109.5 . . ?
N4 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N4 C44 H44A 109.5 . . ?
N4 C44 H44B 109.5 . . ?
N4 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 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
Hf P1 C1 C2 39.54(13) . . . . ?
Hf P1 C8 C9 -96.51(15) . . . . ?
Hf P1 C8 C13 79.70(16) . . . . ?
Hf P1 C14 C15 -170.25(13) . . . . ?
Hf P1 C14 C19 12.83(17) . . . . ?
Hf N1 C3 C2 99.31(15) . . . . ?
Hf N1 C3 C4 -72.97(16) . . . . ?
Hf N1 C22 C21 155.60(14) . . . . ?
Hf N1 C22 C23 -19.7(2) . . . . ?
Hf C3 C4 C5 131.03(17) . . . . ?
P1 C1 C2 C3 -64.97(18) . . . . ?
P1 C1 C2 C7 110.07(18) . . . . ?
P1 C8 C9 C10 176.49(15) . . . . ?
P1 C8 C13 C12 -177.20(16) . . . . ?
P1 C14 C15 C16 -176.73(15) . . . . ?
P1 C14 C19 C18 177.76(14) . . . . ?
P2 C20 C21 C22 -76.27(18) . . . . ?
P2 C20 C21 C26 98.79(16) . . . . ?
P2 C27 C28 C29 177.43(16) . . . . ?
P2 C27 C32 C31 -176.92(17) . . . . ?
P2 C33 C34 C35 177.34(15) . . . . ?
P2 C33 C38 C37 -176.78(14) . . . . ?
N1 C3 C4 C5 177.53(17) . . . . ?
N1 C22 C23 C24 173.71(16) . . . . ?
C1 P1 C8 C9 148.07(15) . . . . ?
C1 P1 C8 C13 -35.72(17) . . . . ?
C1 P1 C14 C15 -55.94(17) . . . . ?
C1 P1 C14 C19 127.13(15) . . . . ?
C1 C2 C3 Hf 53.40(19) . . . . ?
C1 C2 C3 N1 -2.0(2) . . . . ?
C1 C2 C3 C4 170.35(16) . . . . ?
C1 C2 C7 C6 -173.95(19) . . . . ?
C2 C3 C4 C5 5.2(3) . . . . ?
C3 N1 C22 C21 -30.3(3) . . . . ?
C3 N1 C22 C23 154.43(16) . . . . ?
C3 C2 C7 C6 1.1(3) . . . . ?
C3 C4 C5 C6 -1.7(3) . . . . ?
C4 C5 C6 C7 -2.2(3) . . . . ?
C5 C6 C7 C2 2.5(3) . . . . ?
C7 C2 C3 Hf -121.80(16) . . . . ?
C7 C2 C3 N1 -177.20(16) . . . . ?
C7 C2 C3 C4 -4.8(3) . . . . ?
C8 P1 C1 C2 167.51(12) . . . . ?
C8 P1 C14 C15 51.50(17) . . . . ?
C8 P1 C14 C19 -125.42(15) . . . . ?
C8 C9 C10 C11 0.6(3) . . . . ?
C9 C8 C13 C12 -0.9(3) . . . . ?
C9 C10 C11 C12 -0.5(3) . . . . ?
C10 C11 C12 C13 -0.3(3) . . . . ?
C11 C12 C13 C8 1.1(3) . . . . ?
C13 C8 C9 C10 0.1(3) . . . . ?
C14 P1 C1 C2 -87.21(13) . . . . ?
C14 P1 C8 C9 41.37(16) . . . . ?
C14 P1 C8 C13 -142.42(16) . . . . ?
C14 C15 C16 C17 -1.3(3) . . . . ?
C15 C14 C19 C18 0.7(3) . . . . ?
C15 C16 C17 C18 1.4(3) . . . . ?
C16 C17 C18 C19 -0.4(3) . . . . ?
C17 C18 C19 C14 -0.6(3) . . . . ?
C19 C14 C15 C16 0.2(3) . . . . ?
C20 P2 C27 C28 93.93(15) . . . . ?
C20 P2 C27 C32 -87.49(18) . . . . ?
C20 P2 C33 C34 178.81(14) . . . . ?
C20 P2 C33 C38 -5.55(17) . . . . ?
C20 C21 C22 N1 0.8(3) . . . . ?
C20 C21 C22 C23 176.06(16) . . . . ?
C20 C21 C26 C25 -174.84(17) . . . . ?
C21 C22 C23 C24 -2.0(3) . . . . ?
C22 N1 C3 Hf -175.76(19) . . . . ?
C22 N1 C3 C2 -76.4(2) . . . . ?
C22 N1 C3 C4 111.26(19) . . . . ?
C22 C21 C26 C25 0.5(3) . . . . ?
C22 C23 C24 C25 1.3(3) . . . . ?
C23 C24 C25 C26 0.3(3) . . . . ?
C24 C25 C26 C21 -1.2(3) . . . . ?
C26 C21 C22 N1 -174.16(16) . . . . ?
C26 C21 C22 C23 1.1(2) . . . . ?
C27 P2 C20 C21 -69.87(13) . . . . ?
C27 P2 C33 C34 74.65(16) . . . . ?
C27 P2 C33 C38 -109.71(16) . . . . ?
C27 C28 C29 C30 -0.2(3) . . . . ?
C28 C27 C32 C31 1.6(3) . . . . ?
C28 C29 C30 C31 1.3(3) . . . . ?
C29 C30 C31 C32 -0.9(4) . . . . ?
C30 C31 C32 C27 -0.6(4) . . . . ?
C32 C27 C28 C29 -1.2(3) . . . . ?
C33 P2 C20 C21 -175.14(12) . . . . ?
C33 P2 C27 C28 -161.12(14) . . . . ?
C33 P2 C27 C32 17.47(19) . . . . ?
C33 C34 C35 C36 -0.4(3) . . . . ?
C34 C33 C38 C37 -1.1(3) . . . . ?
C34 C35 C36 C37 -0.8(3) . . . . ?
C35 C36 C37 C38 1.1(3) . . . . ?
C36 C37 C38 C33 -0.1(3) . . . . ?
C38 C33 C34 C35 1.4(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.104
_oxdiff_exptl_absorpt_empirical_full_min 0.906
_cell_oxdiff_length_a            12.47419(13)
_cell_oxdiff_length_b            12.67913(18)
_cell_oxdiff_length_c            14.64329(19)
_cell_oxdiff_angle_alpha         81.2172(11)
_cell_oxdiff_angle_beta          85.5974(9)
_cell_oxdiff_angle_gamma         61.4891(12)
_cell_oxdiff_volume              2011.26(4)
_cell_oxdiff_measurement_reflns_used 52008
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ba_sb17
_database_code_depnum_ccdc_archive 'CCDC 1530465'
_audit_update_record             
;
2017-03-17 deposited with the CCDC.
2017-04-05 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed Oct 29 13:37:29 2014'
;

_audit_block_code                ba_sb17
_audit_block_refno               2227
_audit_block_usercomment         'sb_jb198, irregular, colourless'


# start Validation Reply Form
_vrf_PLAT910_ba_sb17             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          13 Note
RESPONSE: limited by diffractometer.
;
# end Validation Reply Form


_audit_creation_method           
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C38 H33 N P2'
_chemical_formula_sum            'C38 H33 N P2'
_chemical_properties_physical    air-sensitive
_chemical_formula_weight         565.59
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      120(1)
_chemical_oxdiff_formula         'C38 H33 N P2'
_chemical_oxdiff_usercomment     'sb_jb198, irregular, colourless'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration .

_space_group_name_Hall           '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.66534(12)
_cell_length_b                   12.26799(17)
_cell_length_c                   13.52930(18)
_cell_angle_alpha                111.4620(12)
_cell_angle_beta                 107.2399(11)
_cell_angle_gamma                96.1928(10)
_cell_volume                     1526.14(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    42383
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.7950
_cell_measurement_theta_min      3.7870
_shelx_estimated_absorpt_T_max   0.983
_shelx_estimated_absorpt_T_min   0.983
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,16:31:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.2317
_exptl_crystal_size_mid          0.2162
_exptl_crystal_size_min          0.1815
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            161760
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.100
_diffrn_reflns_theta_min         3.315
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -46.00   51.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000  -35.1244 194

#__ type_ start__ end____ width___ exp.time_
  2 omega  -10.00   81.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   77.0000   90.0000 182

#__ type_ start__ end____ width___ exp.time_
  3 omega   -6.00   88.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   77.0000 -120.0000 188

#__ type_ start__ end____ width___ exp.time_
  4 omega  -50.00  -11.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -57.0000    0.0000 78

#__ type_ start__ end____ width___ exp.time_
  5 omega   -2.00   82.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   57.0000    0.0000 168

#__ type_ start__ end____ width___ exp.time_
  6 omega    0.00   38.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   57.0000 -150.0000 76

#__ type_ start__ end____ width___ exp.time_
  7 omega  -51.00   48.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000   60.0000 198

#__ type_ start__ end____ width___ exp.time_
  8 omega  -45.00  -19.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000 -150.0000 52

#__ type_ start__ end____ width___ exp.time_
  9 omega   21.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000 -150.0000 56

#__ type_ start__ end____ width___ exp.time_
 10 omega  -46.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000 -120.0000 190

#__ type_ start__ end____ width___ exp.time_
 11 omega    6.00   33.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -38.0000   30.0000 54

#__ type_ start__ end____ width___ exp.time_
 12 omega  -45.00   51.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000  133.9178 192

#__ type_ start__ end____ width___ exp.time_
 13 omega  -50.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -57.0000   60.0000 180

#__ type_ start__ end____ width___ exp.time_
 14 omega  -25.00   92.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   19.0000   90.0000 234

#__ type_ start__ end____ width___ exp.time_
 15 omega   -3.00   88.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   57.0000 -150.0000 182

#__ type_ start__ end____ width___ exp.time_
 16 omega   -3.00   88.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   57.0000  -30.0000 182

#__ type_ start__ end____ width___ exp.time_
 17 omega  -50.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -57.0000 -120.0000 180

#__ type_ start__ end____ width___ exp.time_
 18 omega  -11.00   89.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   77.0000   60.0000 200

#__ type_ start__ end____ width___ exp.time_
 19 omega  -51.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000   90.0000 200

#__ type_ start__ end____ width___ exp.time_
 20 omega  -54.00   44.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -38.0000  -30.0000 196

#__ type_ start__ end____ width___ exp.time_
 21 omega  -51.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000 -120.0000 200

#__ type_ start__ end____ width___ exp.time_
 22 omega  -50.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -57.0000  150.0000 180

#__ type_ start__ end____ width___ exp.time_
 23 omega  -50.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -57.0000  -90.0000 180

#__ type_ start__ end____ width___ exp.time_
 24 omega  -46.00   51.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000  -35.1244 194

#__ type_ start__ end____ width___ exp.time_
 25 omega  -51.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000 -150.0000 200

#__ type_ start__ end____ width___ exp.time_
 26 omega  -51.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000    0.0000 200

#__ type_ start__ end____ width___ exp.time_
 27 omega  -54.00   92.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505    0.0000    0.0000 292

#__ type_ start__ end____ width___ exp.time_
 28 omega  -54.00   92.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505    0.0000  120.0000 292

#__ type_ start__ end____ width___ exp.time_
 29 omega  -54.00   92.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505    0.0000  240.0000 292

#__ type_ start__ end____ width___ exp.time_
 30 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  40.0000   18.8505    0.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 31 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -20.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 32 omega  -46.00   51.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000  133.9178 194

#__ type_ start__ end____ width___ exp.time_
 33 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -40.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 34 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   40.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 35 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -60.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 36 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   60.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 37 phi    120.00  240.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  40.0000   18.8505    0.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 38 phi    120.00  240.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -20.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 39 phi    120.00  240.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   20.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 40 phi    120.00  240.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -40.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 41 phi    120.00  240.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   40.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 42 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   20.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 43 phi    120.00  240.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   60.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 44 phi    240.00  360.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  40.0000   18.8505    0.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 45 phi    240.00  360.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -20.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 46 phi    240.00  360.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   20.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 47 phi    240.00  360.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -40.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 48 phi    240.00  360.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   40.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 49 phi    240.00  360.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -60.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 50 phi    240.00  360.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   60.0000     -     240

#__ type_ start__ end____ width___ exp.time_
 51 omega  -25.00   44.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   19.0000 -180.0000 138

#__ type_ start__ end____ width___ exp.time_
 52 phi    120.00  240.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -60.0000     -     240

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω and π scans'
_diffrn_orient_matrix_UB_11      0.0018146000
_diffrn_orient_matrix_UB_12      0.0461112000
_diffrn_orient_matrix_UB_13      0.0511959000
_diffrn_orient_matrix_UB_21      0.0666681000
_diffrn_orient_matrix_UB_22      -0.0021681000
_diffrn_orient_matrix_UB_23      0.0283132000
_diffrn_orient_matrix_UB_31      0.0265738000
_diffrn_orient_matrix_UB_32      0.0444019000
_diffrn_orient_matrix_UB_33      -0.0152421000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus X-Ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7293
_reflns_number_total             7949
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,16:31:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,16:31:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,16:31:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_shelxl_version_number           2014/6
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         7949
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0520
_refine_ls_restrained_S_all      1.187
_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)+(0.0273P)²+1.0441P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1078
_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
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.34052(4) 0.82324(4) 0.21516(3) 0.01948(10) Uani 1 1 d . . . . .
P2 P 0.20804(4) 0.62088(4) -0.10614(3) 0.01964(10) Uani 1 1 d . . . . .
N N 0.38571(15) 0.53890(13) 0.11581(11) 0.0238(3) Uani 1 1 d . . . . .
H H 0.381(2) 0.6028(19) 0.1031(17) 0.029 Uiso 1 1 d R . . . .
C1 C 0.48030(16) 0.77740(14) 0.30031(13) 0.0212(3) Uani 1 1 d . . . . .
H1A H 0.5465 0.7613 0.2619 0.025 Uiso 1 1 calc R . . . .
H1B H 0.5277 0.8450 0.3765 0.025 Uiso 1 1 calc R . . . .
C2 C 0.42988(15) 0.66668(14) 0.31469(13) 0.0197(3) Uani 1 1 d . . . . .
C3 C 0.38289(15) 0.55098(14) 0.22245(13) 0.0196(3) Uani 1 1 d . . . . .
C4 C 0.33743(17) 0.45097(15) 0.24041(14) 0.0240(3) Uani 1 1 d . . . . .
H4 H 0.3060 0.3730 0.1790 0.029 Uiso 1 1 calc R . . . .
C5 C 0.33769(19) 0.46428(17) 0.34676(15) 0.0283(4) Uani 1 1 d . . . . .
H5 H 0.3063 0.3954 0.3573 0.034 Uiso 1 1 calc R . . . .
C6 C 0.38339(18) 0.57722(17) 0.43796(15) 0.0283(4) Uani 1 1 d . . . . .
H6 H 0.3835 0.5862 0.5108 0.034 Uiso 1 1 calc R . . . .
C7 C 0.42906(17) 0.67694(16) 0.42081(14) 0.0239(3) Uani 1 1 d . . . . .
H7 H 0.4606 0.7543 0.4831 0.029 Uiso 1 1 calc R . . . .
C8 C 0.27118(15) 0.90289(14) 0.32304(13) 0.0203(3) Uani 1 1 d . . . . .
C9 C 0.27882(17) 1.02661(16) 0.36224(15) 0.0264(4) Uani 1 1 d . . . . .
H9 H 0.3232 1.0732 0.3341 0.032 Uiso 1 1 calc R . . . .
C10 C 0.22219(18) 1.08242(17) 0.44205(16) 0.0320(4) Uani 1 1 d . . . . .
H10 H 0.2287 1.1668 0.4683 0.038 Uiso 1 1 calc R . . . .
C11 C 0.15673(18) 1.01632(19) 0.48335(16) 0.0337(4) Uani 1 1 d . . . . .
H11 H 0.1195 1.0551 0.5388 0.040 Uiso 1 1 calc R . . . .
C12 C 0.14538(18) 0.89301(18) 0.44370(16) 0.0315(4) Uani 1 1 d . . . . .
H12 H 0.0993 0.8470 0.4713 0.038 Uiso 1 1 calc R . . . .
C13 C 0.20132(16) 0.83628(16) 0.36357(15) 0.0260(3) Uani 1 1 d . . . . .
H13 H 0.1920 0.7515 0.3361 0.031 Uiso 1 1 calc R . . . .
C14 C 0.43508(17) 0.95177(14) 0.20721(14) 0.0219(3) Uani 1 1 d . . . . .
C15 C 0.37715(19) 0.97655(17) 0.11351(16) 0.0291(4) Uani 1 1 d . . . . .
H15 H 0.2955 0.9239 0.0545 0.035 Uiso 1 1 calc R . . . .
C16 C 0.4376(2) 1.0773(2) 0.10555(19) 0.0406(5) Uani 1 1 d . . . . .
H16 H 0.3967 1.0935 0.0414 0.049 Uiso 1 1 calc R . . . .
C17 C 0.5567(2) 1.1543(2) 0.1901(2) 0.0437(5) Uani 1 1 d . . . . .
H17 H 0.5973 1.2238 0.1849 0.052 Uiso 1 1 calc R . . . .
C18 C 0.6166(2) 1.12928(19) 0.2828(2) 0.0404(5) Uani 1 1 d . . . . .
H18 H 0.6996 1.1810 0.3404 0.048 Uiso 1 1 calc R . . . .
C19 C 0.55615(19) 1.02926(17) 0.29179(16) 0.0308(4) Uani 1 1 d . . . . .
H19 H 0.5975 1.0134 0.3560 0.037 Uiso 1 1 calc R . . . .
C20 C 0.13218(17) 0.51353(16) -0.05918(14) 0.0243(3) Uani 1 1 d . . . . .
H20A H 0.1398 0.5570 0.0209 0.029 Uiso 1 1 calc R . . . .
H20B H 0.0350 0.4792 -0.1071 0.029 Uiso 1 1 calc R . . . .
C21 C 0.20430(16) 0.41333(15) -0.06909(13) 0.0217(3) Uani 1 1 d . . . . .
C22 C 0.32648(16) 0.42834(14) 0.01626(13) 0.0207(3) Uani 1 1 d . . . . .
C23 C 0.39311(18) 0.33497(16) 0.00283(15) 0.0261(3) Uani 1 1 d . . . . .
H23 H 0.4766 0.3460 0.0604 0.031 Uiso 1 1 calc R . . . .
C24 C 0.3391(2) 0.22647(16) -0.09324(15) 0.0311(4) Uani 1 1 d . . . . .
H24 H 0.3852 0.1635 -0.1014 0.037 Uiso 1 1 calc R . . . .
C25 C 0.2175(2) 0.21023(17) -0.17748(15) 0.0345(4) Uani 1 1 d . . . . .
H25 H 0.1793 0.1357 -0.2432 0.041 Uiso 1 1 calc R . . . .
C26 C 0.1521(2) 0.30318(16) -0.16546(15) 0.0306(4) Uani 1 1 d . . . . .
H26 H 0.0696 0.2918 -0.2242 0.037 Uiso 1 1 calc R . . . .
C27 C 0.15896(16) 0.52165(14) -0.25821(13) 0.0211(3) Uani 1 1 d . . . . .
C28 C 0.26119(18) 0.48979(15) -0.29926(15) 0.0248(3) Uani 1 1 d . . . . .
H28 H 0.3531 0.5207 -0.2490 0.030 Uiso 1 1 calc R . . . .
C29 C 0.2301(2) 0.41314(17) -0.41327(16) 0.0320(4) Uani 1 1 d . . . . .
H29 H 0.3005 0.3922 -0.4406 0.038 Uiso 1 1 calc R . . . .
C30 C 0.0964(2) 0.36770(16) -0.48656(15) 0.0346(4) Uani 1 1 d . . . . .
H30 H 0.0749 0.3156 -0.5644 0.042 Uiso 1 1 calc R . . . .
C31 C -0.0061(2) 0.39824(16) -0.44640(15) 0.0322(4) Uani 1 1 d . . . . .
H31 H -0.0978 0.3665 -0.4970 0.039 Uiso 1 1 calc R . . . .
C32 C 0.02391(17) 0.47471(15) -0.33304(14) 0.0254(3) Uani 1 1 d . . . . .
H32 H -0.0470 0.4952 -0.3063 0.030 Uiso 1 1 calc R . . . .
C33 C 0.08724(16) 0.71588(14) -0.11340(14) 0.0218(3) Uani 1 1 d . . . . .
C34 C 0.08090(18) 0.77600(16) -0.18404(15) 0.0283(4) Uani 1 1 d . . . . .
H34 H 0.1349 0.7630 -0.2299 0.034 Uiso 1 1 calc R . . . .
C35 C -0.0030(2) 0.85431(17) -0.18830(17) 0.0349(4) Uani 1 1 d . . . . .
H35 H -0.0066 0.8940 -0.2372 0.042 Uiso 1 1 calc R . . . .
C36 C -0.08181(19) 0.87471(17) -0.12093(17) 0.0365(5) Uani 1 1 d . . . . .
H36 H -0.1401 0.9276 -0.1242 0.044 Uiso 1 1 calc R . . . .
C37 C -0.07476(19) 0.81771(17) -0.04942(17) 0.0346(4) Uani 1 1 d . . . . .
H37 H -0.1277 0.8324 -0.0026 0.042 Uiso 1 1 calc R . . . .
C38 C 0.00908(17) 0.73873(16) -0.04487(15) 0.0278(4) Uani 1 1 d . . . . .
H38 H 0.0131 0.7002 0.0051 0.033 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.8716(16) . ?
P1 C8 1.8395(16) . ?
P1 C14 1.8330(17) . ?
P2 C20 1.8653(17) . ?
P2 C27 1.8386(16) . ?
P2 C33 1.8331(16) . ?
N H 0.87(2) . ?
N C3 1.405(2) . ?
N C22 1.424(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.507(2) . ?
C2 C3 1.415(2) . ?
C2 C7 1.397(2) . ?
C3 C4 1.400(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.386(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.391(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.397(2) . ?
C8 C13 1.401(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.391(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.378(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.385(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.392(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.393(2) . ?
C14 C19 1.394(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.386(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.380(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.387(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.386(3) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.505(2) . ?
C21 C22 1.402(2) . ?
C21 C26 1.398(2) . ?
C22 C23 1.396(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.385(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.386(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.385(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.394(2) . ?
C27 C32 1.400(2) . ?
C28 H28 0.9500 . ?
C28 C29 1.393(2) . ?
C29 H29 0.9500 . ?
C29 C30 1.383(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.387(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.388(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.397(2) . ?
C33 C38 1.397(2) . ?
C34 H34 0.9500 . ?
C34 C35 1.387(2) . ?
C35 H35 0.9500 . ?
C35 C36 1.390(3) . ?
C36 H36 0.9500 . ?
C36 C37 1.376(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.393(3) . ?
C38 H38 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 P1 C1 101.33(7) . . ?
C14 P1 C1 101.49(7) . . ?
C14 P1 C8 100.36(7) . . ?
C27 P2 C20 99.47(7) . . ?
C33 P2 C20 102.42(8) . . ?
C33 P2 C27 100.48(7) . . ?
C3 N H 114.8(14) . . ?
C3 N C22 122.41(14) . . ?
C22 N H 114.2(14) . . ?
P1 C1 H1A 109.1 . . ?
P1 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 P1 112.58(11) . . ?
C2 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
C3 C2 C1 121.36(14) . . ?
C7 C2 C1 120.01(14) . . ?
C7 C2 C3 118.63(15) . . ?
N C3 C2 119.27(14) . . ?
C4 C3 N 121.62(14) . . ?
C4 C3 C2 119.10(14) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.83(16) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.69(16) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 H6 120.6 . . ?
C5 C6 C7 118.79(16) . . ?
C7 C6 H6 120.6 . . ?
C2 C7 H7 119.0 . . ?
C6 C7 C2 121.96(16) . . ?
C6 C7 H7 119.0 . . ?
C9 C8 P1 122.76(13) . . ?
C9 C8 C13 118.15(15) . . ?
C13 C8 P1 119.00(12) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 C8 120.71(17) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 H10 119.8 . . ?
C11 C10 C9 120.49(17) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 H11 120.1 . . ?
C10 C11 C12 119.72(17) . . ?
C12 C11 H11 120.1 . . ?
C11 C12 H12 119.9 . . ?
C11 C12 C13 120.20(17) . . ?
C13 C12 H12 119.9 . . ?
C8 C13 H13 119.7 . . ?
C12 C13 C8 120.68(17) . . ?
C12 C13 H13 119.7 . . ?
C15 C14 P1 117.21(13) . . ?
C15 C14 C19 118.62(16) . . ?
C19 C14 P1 124.06(13) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.62(18) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.45(19) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 120.3 . . ?
C16 C17 C18 119.42(19) . . ?
C18 C17 H17 120.3 . . ?
C17 C18 H18 119.8 . . ?
C19 C18 C17 120.44(19) . . ?
C19 C18 H18 119.8 . . ?
C14 C19 H19 119.8 . . ?
C18 C19 C14 120.42(18) . . ?
C18 C19 H19 119.8 . . ?
P2 C20 H20A 109.7 . . ?
P2 C20 H20B 109.7 . . ?
H20A C20 H20B 108.2 . . ?
C21 C20 P2 109.94(11) . . ?
C21 C20 H20A 109.7 . . ?
C21 C20 H20B 109.7 . . ?
C22 C21 C20 121.28(15) . . ?
C26 C21 C20 120.51(15) . . ?
C26 C21 C22 118.19(16) . . ?
C21 C22 N 120.89(15) . . ?
C23 C22 N 119.21(15) . . ?
C23 C22 C21 119.88(15) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 C22 120.86(16) . . ?
C24 C23 H23 119.6 . . ?
C23 C24 H24 120.2 . . ?
C23 C24 C25 119.69(17) . . ?
C25 C24 H24 120.2 . . ?
C24 C25 H25 120.1 . . ?
C26 C25 C24 119.70(17) . . ?
C26 C25 H25 120.1 . . ?
C21 C26 H26 119.2 . . ?
C25 C26 C21 121.66(17) . . ?
C25 C26 H26 119.2 . . ?
C28 C27 P2 118.08(12) . . ?
C28 C27 C32 119.06(15) . . ?
C32 C27 P2 122.84(13) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 C27 120.70(17) . . ?
C29 C28 H28 119.7 . . ?
C28 C29 H29 120.1 . . ?
C30 C29 C28 119.79(17) . . ?
C30 C29 H29 120.1 . . ?
C29 C30 H30 120.0 . . ?
C29 C30 C31 119.97(17) . . ?
C31 C30 H30 120.0 . . ?
C30 C31 H31 119.7 . . ?
C30 C31 C32 120.64(17) . . ?
C32 C31 H31 119.7 . . ?
C27 C32 H32 120.1 . . ?
C31 C32 C27 119.84(17) . . ?
C31 C32 H32 120.1 . . ?
C34 C33 P2 118.43(13) . . ?
C34 C33 C38 118.28(16) . . ?
C38 C33 P2 123.09(13) . . ?
C33 C34 H34 119.5 . . ?
C35 C34 C33 121.07(17) . . ?
C35 C34 H34 119.5 . . ?
C34 C35 H35 120.0 . . ?
C34 C35 C36 120.00(19) . . ?
C36 C35 H35 120.0 . . ?
C35 C36 H36 120.2 . . ?
C37 C36 C35 119.55(17) . . ?
C37 C36 H36 120.2 . . ?
C36 C37 H37 119.6 . . ?
C36 C37 C38 120.77(18) . . ?
C38 C37 H37 119.6 . . ?
C33 C38 H38 119.8 . . ?
C37 C38 C33 120.32(18) . . ?
C37 C38 H38 119.8 . . ?

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
P1 C1 C2 C3 71.75(17) . . . . ?
P1 C1 C2 C7 -108.35(15) . . . . ?
P1 C8 C9 C10 178.53(13) . . . . ?
P1 C8 C13 C12 -178.87(13) . . . . ?
P1 C14 C15 C16 175.29(15) . . . . ?
P1 C14 C19 C18 -175.58(15) . . . . ?
P2 C20 C21 C22 82.35(17) . . . . ?
P2 C20 C21 C26 -96.29(17) . . . . ?
P2 C27 C28 C29 178.86(13) . . . . ?
P2 C27 C32 C31 -178.65(13) . . . . ?
P2 C33 C34 C35 -176.40(14) . . . . ?
P2 C33 C38 C37 176.01(13) . . . . ?
N C3 C4 C5 178.80(16) . . . . ?
N C22 C23 C24 -179.52(16) . . . . ?
C1 P1 C8 C9 113.97(14) . . . . ?
C1 P1 C8 C13 -69.54(14) . . . . ?
C1 P1 C14 C15 152.74(13) . . . . ?
C1 P1 C14 C19 -31.13(16) . . . . ?
C1 C2 C3 N 1.2(2) . . . . ?
C1 C2 C3 C4 179.84(14) . . . . ?
C1 C2 C7 C6 179.98(15) . . . . ?
C2 C3 C4 C5 0.2(2) . . . . ?
C3 N C22 C21 105.64(18) . . . . ?
C3 N C22 C23 -75.8(2) . . . . ?
C3 C2 C7 C6 -0.1(2) . . . . ?
C3 C4 C5 C6 -0.1(3) . . . . ?
C4 C5 C6 C7 0.0(3) . . . . ?
C5 C6 C7 C2 0.2(3) . . . . ?
C7 C2 C3 N -178.70(14) . . . . ?
C7 C2 C3 C4 -0.1(2) . . . . ?
C8 P1 C1 C2 79.83(12) . . . . ?
C8 P1 C14 C15 -103.32(14) . . . . ?
C8 P1 C14 C19 72.81(16) . . . . ?
C8 C9 C10 C11 -0.4(3) . . . . ?
C9 C8 C13 C12 -2.2(2) . . . . ?
C9 C10 C11 C12 -1.0(3) . . . . ?
C10 C11 C12 C13 0.8(3) . . . . ?
C11 C12 C13 C8 0.8(3) . . . . ?
C13 C8 C9 C10 2.0(2) . . . . ?
C14 P1 C1 C2 -177.00(11) . . . . ?
C14 P1 C8 C9 9.90(15) . . . . ?
C14 P1 C8 C13 -173.61(13) . . . . ?
C14 C15 C16 C17 0.5(3) . . . . ?
C15 C14 C19 C18 0.5(3) . . . . ?
C15 C16 C17 C18 0.7(3) . . . . ?
C16 C17 C18 C19 -1.3(3) . . . . ?
C17 C18 C19 C14 0.7(3) . . . . ?
C19 C14 C15 C16 -1.1(3) . . . . ?
C20 P2 C27 C28 -113.81(14) . . . . ?
C20 P2 C27 C32 64.46(15) . . . . ?
C20 P2 C33 C34 -156.43(13) . . . . ?
C20 P2 C33 C38 28.88(16) . . . . ?
C20 C21 C22 N 0.6(2) . . . . ?
C20 C21 C22 C23 -177.95(15) . . . . ?
C20 C21 C26 C25 178.99(17) . . . . ?
C21 C22 C23 C24 -1.0(2) . . . . ?
C22 N C3 C2 -172.80(15) . . . . ?
C22 N C3 C4 8.6(2) . . . . ?
C22 C21 C26 C25 0.3(3) . . . . ?
C22 C23 C24 C25 0.2(3) . . . . ?
C23 C24 C25 C26 0.8(3) . . . . ?
C24 C25 C26 C21 -1.1(3) . . . . ?
C26 C21 C22 N 179.24(15) . . . . ?
C26 C21 C22 C23 0.7(2) . . . . ?
C27 P2 C20 C21 66.58(13) . . . . ?
C27 P2 C33 C34 -54.19(14) . . . . ?
C27 P2 C33 C38 131.12(14) . . . . ?
C27 C28 C29 C30 -0.2(3) . . . . ?
C28 C27 C32 C31 -0.4(2) . . . . ?
C28 C29 C30 C31 -0.2(3) . . . . ?
C29 C30 C31 C32 0.3(3) . . . . ?
C30 C31 C32 C27 0.0(3) . . . . ?
C32 C27 C28 C29 0.5(3) . . . . ?
C33 P2 C20 C21 169.62(11) . . . . ?
C33 P2 C27 C28 141.56(13) . . . . ?
C33 P2 C27 C32 -40.17(15) . . . . ?
C33 C34 C35 C36 0.5(3) . . . . ?
C34 C33 C38 C37 1.3(2) . . . . ?
C34 C35 C36 C37 0.7(3) . . . . ?
C35 C36 C37 C38 -0.8(3) . . . . ?
C36 C37 C38 C33 -0.2(3) . . . . ?
C38 C33 C34 C35 -1.5(3) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1 15 1 0.0824 1.0027 14.9985 0.9990 0.7446 0.0626 0.6774
-5 14 -13 0.0879 -4.9993 14.0009 -12.9977 -0.0289 -0.7317 0.6869
-6 2 17 0.0908 -5.9969 1.9975 16.9991 0.9515 0.0772 -0.3298
7 5 -19 0.0973 6.9978 5.0021 -18.9993 -0.7293 -0.0822 0.6976
-14 7 0 0.1235 -13.9983 7.0000 0.0029 0.2975 -0.9483 -0.0612
2 -12 -7 0.0826 1.9968 -11.9980 -6.9991 -0.9079 -0.0390 -0.3730
4 -15 13 0.1045 3.9992 -15.0008 12.9980 -0.0190 0.6672 -0.7579
14 2 -1 0.0883 13.9997 1.9993 -1.0031 0.0662 0.9006 0.4761
7 14 -13 0.1099 7.0002 14.0004 -13.0005 -0.0073 0.0683 1.0058
11 -8 -11 0.0612 10.9966 -7.9981 -11.0007 -0.9120 0.4390 0.1048
5 -16 0 0.0908 4.9970 -15.9988 -0.0005 -0.7287 0.3678 -0.5776
-12 2 15 0.1161 -11.9970 1.9981 15.0007 0.8383 -0.3794 -0.4587
-4 16 -1 0.0913 -3.9972 15.9989 -0.9996 0.6793 -0.3295 0.6194
-6 -2 -12 0.0879 -6.0019 -1.9978 -11.9970 -0.7172 -0.7355 -0.0653
6 1 13 0.1031 6.0019 0.9977 12.9969 0.7223 0.7660 0.0057
-6 -15 12 0.1111 -6.0006 -15.0002 12.0004 -0.0882 -0.0278 -1.0084
-12 -8 7 0.0903 -11.9999 -7.9998 7.0021 -0.0322 -0.5844 -0.7808

_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            10.66534(12)
_cell_oxdiff_length_b            12.26799(17)
_cell_oxdiff_length_c            13.52930(18)
_cell_oxdiff_angle_alpha         111.4620(12)
_cell_oxdiff_angle_beta          107.2399(11)
_cell_oxdiff_angle_gamma         96.1928(10)
_cell_oxdiff_volume              1526.14(3)
_cell_oxdiff_measurement_reflns_used 42383
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ba_sb60
_database_code_depnum_ccdc_archive 'CCDC 1530473'
_audit_update_record             
;
2017-03-17 deposited with the CCDC.
2017-04-05 downloaded from the CCDC.
;
_audit_creation_date             2016-04-27

_audit_block_code                ba_sb60
_audit_block_refno               2711
_audit_block_usercomment         'sb_dh17, irregular, yellow'


_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C45 H38 Cl Hf N P2, C4 H10 O'
_chemical_formula_sum            'C49 H48 Cl Hf N O P2'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         942.76
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_diffrn_ambient_temperature      120(1)
_chemical_oxdiff_formula         'C49 H48 Cl1 Hf1 N1 O1 P2'
_chemical_oxdiff_usercomment     'sb_dh17, irregular, yellow'
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -6.1794 4.9776 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration .

_space_group_name_Hall           '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.05585(7)
_cell_length_b                   12.17458(6)
_cell_length_c                   28.6103(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.9077(6)
_cell_angle_gamma                90
_cell_volume                     4196.94(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    96329
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.6590
_cell_measurement_theta_min      3.9440
_shelx_estimated_absorpt_T_max   0.577
_shelx_estimated_absorpt_T_min   0.577
_exptl_absorpt_coefficient_mu    6.187
_exptl_absorpt_correction_T_max  0.738
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41p (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1904
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 7 3 0.0278
4 -4 11 0.0313
5 -3 -14 0.0347
-1 -5 -15 0.0464
2 -1 -18 0.0374
-5 5 -9 0.0342
-6 -5 1 0.0576
-2 1 18 0.0270
-5 3 14 0.0347
6 -5 -3 0.0318
-3 -2 -16 0.0416
-6 0 -11 0.0414
_exptl_crystal_size_max          0.104
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.064
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.9990 7.0002 2.9997 -0.4784 -0.8531 0.0766
4.0001 -3.9993 10.9999 -0.6552 0.5717 0.3641
5.0005 -2.9995 -13.9988 -0.3188 0.3524 -0.9294
-0.9990 -5.0002 -14.9991 0.4430 0.5652 -0.7490
2.0005 -1.0000 -17.9989 0.1019 0.0666 -0.9951
-5.0002 4.9991 -9.0001 0.7304 -0.6957 -0.2158
-5.9992 -5.0006 0.9998 0.7499 0.5991 0.2608
-2.0005 1.0000 17.9989 -0.1019 -0.0666 0.9951
-5.0005 2.9995 13.9988 0.3188 -0.3524 0.9294
5.9999 -5.0000 -3.0008 -0.6277 0.6542 -0.4296
-3.0000 -2.0000 -16.0000 0.6783 0.1710 -0.6975
-6.0000 0.0000 -10.9996 0.9312 -0.0792 -0.3098

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            179970
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.867
_diffrn_reflns_theta_min         3.668
_diffrn_ambient_environment      perfluoro
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  73.00   1.00    2.00    --    0.00  27.00  69.00  105
  2  ω    -21.00  69.00   1.00    2.00    --    0.00  57.00  60.00   90
  3  ω    -26.00  72.00   1.00    2.00    --    0.00  38.00 -30.00   98
  4  ω    -70.00  30.00   1.00    2.00    --    0.00 -77.00   0.00  100
  5  ω    -30.00  70.00   1.00    2.00    --    0.00  77.00 120.00  100
  6  ω    -49.00  -4.00   1.00    2.00    --   10.00 128.00 126.38   45
  7  ω    -30.00  17.00   1.00    2.00    --   14.00 103.00   1.08   47
  8  ω    -32.00  -3.00   1.00    2.00    --   26.00 126.00  83.83   29
  9  ω    -29.00  -3.00   1.00    6.00    --   30.00 127.00  98.59   26
 10  ω     -9.00  18.00   1.00    6.00    --   34.00 102.00-161.50   27
 11  ω     -2.00  25.00   1.00    6.00    --   38.00  95.00 -84.03   27
 12  ω      6.00  33.00   1.00    6.00    --   42.00  88.00  71.85   27
 13  ω      5.00  32.00   1.00    6.00    --   42.00  90.00 175.47   27
 14  ω      5.00  32.00   1.00    6.00    --   42.00  90.00 -58.35   27
 15  ω     13.00  40.00   1.00    6.00    --   46.00  83.00 -66.99   27
 16  ω     13.00  40.00   1.00    6.00    --   46.00  83.00-123.99   27
 17  ω     12.00  38.00   1.00    6.00    --   46.00  84.00 146.72   26
 18  ω     18.00  46.00   1.00    6.00    --   50.00  81.00  82.80   28
 19  ω     18.00  46.00   1.00    6.00    --   50.00  80.00-128.82   28
 20  ω     18.00  46.00   1.00    6.00    --   50.00  81.00  54.18   28
 21  ω     17.00  45.00   1.00    6.00    --   50.00  82.00  17.52   28
 22  ω     17.00  45.00   1.00    6.00    --   50.00  82.00 102.38   28
 23  ω     18.00  46.00   1.00    6.00    --   50.00  80.00-162.43   28
 24  ω     18.00  46.00   1.00    6.00    --   50.00  80.00 -33.94   28
 25  ω     18.00  46.00   1.00    6.00    --   50.00  80.00-100.70   28
 26  ω     18.00  46.00   1.00    6.00    --   50.00  80.00 175.15   28
 27  ω     18.00  46.00   1.00    6.00    --   50.00  81.00 -82.24   28
 28  ω      1.00  96.00   1.00    6.00    --   54.00 -99.00-180.00   95
 29  ω     25.00 124.00   1.00    6.00    --   54.00  75.00 140.63   99
 30  ω     23.00  49.00   1.00    6.00    --   54.00  78.00  -9.04   26
 31  ω     24.00 124.00   1.00    6.00    --   54.00  77.00 -30.00  100
 32  ω     23.00  49.00   1.00    6.00    --   54.00  78.00 -78.64   26
 33  ω     24.00 124.00   1.00    6.00    --   54.00  77.00 150.00  100
 34  ω     26.00 124.00   1.00    6.00    --   54.00  74.00  25.69   98
 35  ω     26.00 124.00   1.00    6.00    --   54.00  74.00 116.42   98
 36  ω     23.00  49.00   1.00    6.00    --   54.00  78.00  39.76   26
 37  ω    -15.00  75.00   1.00    6.00    --   54.00 -57.00  90.00   90
 38  ω     24.00 124.00   1.00    6.00    --   54.00  77.00-120.00  100
 39  ω     24.00 124.00   1.00    6.00    --   54.00  77.00 -90.00  100
 40  ω     23.00  49.00   1.00    6.00    --   54.00  78.00 166.63   26
 41  ω     24.00 124.00   1.00    6.00    --   54.00  77.00  90.00  100
 42  ω     26.00 123.00   1.00    6.00    --   54.00  73.00-154.91   97
 43  ω     23.00 111.00   1.00    6.00    --   54.00-125.00 -30.00   88
 44  ω      1.00  96.00   1.00    6.00    --   54.00 -99.00   0.00   95
 45  ω     24.00 124.00   1.00    6.00    --   54.00  77.00-150.00  100
 46  ω     30.00 127.00   1.00    6.00    --   58.00  73.00 -73.66   97
 47  ω     28.00 128.00   1.00    6.00    --   58.00  77.00-124.07  100
 48  ω     29.00 128.00   1.00    6.00    --   58.00  75.00 -96.53   99
 49  ω     28.00 128.00   1.00    6.00    --   58.00  77.00  -4.26  100
 50  ω     30.00 128.00   1.00    6.00    --   58.00  74.00 179.14   98
 51  ω     28.00 128.00   1.00    6.00    --   58.00  77.00-169.60  100
 52  ω     29.00 128.00   1.00    6.00    --   58.00  76.00  89.06   99
 53  ω     29.00 128.00   1.00    6.00    --   58.00  76.00  59.52   99
 54  ω     33.00 132.00   1.00    6.00    --   62.00  75.00 -33.08   99
 55  ω     32.00 132.00   1.00    6.00    --   62.00  77.00-103.05  100
 56  ω     34.00 132.00   1.00    6.00    --   62.00  74.00 103.06   98
 57  ω     32.00 132.00   1.00    6.00    --   62.00  77.00-123.00  100
 58  ω     40.00 135.00   1.00    6.00    --   66.00  70.00 127.66   95
 59  ω     42.00 134.00   1.00    6.00    --   66.00  67.00-134.11   92
 60  ω     37.00 136.00   1.00    6.00    --   66.00  75.00  96.53   99
 61  ω     40.00 135.00   1.00    6.00    --   66.00  70.00 155.83   95
 62  ω     44.00 134.00   1.00    6.00    --   66.00  62.00 -86.14   90
 63  ω     44.00 134.00   1.00    6.00    --   66.00  61.00 -92.45   90
 64  ω     44.00 134.00   1.00    6.00    --   66.00  61.00 -60.68   90
 65  ω     36.00 136.00   1.00    6.00    --   66.00  77.00 -15.57  100
 66  ω     41.00 140.00   1.00    6.00    --   70.00  75.00 -40.69   99
 67  ω     46.00 138.00   1.00    6.00    --   70.00  68.00 163.46   92
 68  ω     42.00 139.00   1.00    6.00    --   70.00  73.00  70.69   97
 69  ω     41.00 140.00   1.00    6.00    --   70.00  75.00 109.42   99
 70  ω     47.00 138.00   1.00    6.00    --   70.00  66.00  16.66   91
 71  ω     44.00 139.00   1.00    6.00    --   70.00  70.00-178.06   95
 72  ω     53.00 142.00   1.00    6.00    --   74.00  60.00 -17.92   89
 73  ω     45.00 144.00   1.00    6.00    --   74.00  76.00 107.10   99
 74  ω     45.00 144.00   1.00    6.00    --   74.00  75.00  78.69   99
 75  ω     49.00 142.00   1.00    6.00    --   74.00  69.00  -7.87   93
 76  ω     46.00 144.00   1.00    6.00    --   74.00  74.00 -72.73   98
 77  ω     44.00 144.00   1.00    6.00    --   74.00  77.00-168.39  100
 78  ω     45.00 144.00   1.00    6.00    --   74.00  75.00  32.74   99
 79  ω     54.00 149.00   1.00    6.00    --   78.00  44.00 -61.86   95
 80  ω     50.00 147.00   1.00    6.00    --   78.00  73.00  63.85   97
 81  ω     50.00 147.00   1.00    6.00    --   78.00  73.00-137.38   97
 82  ω     55.00 146.00   1.00    6.00    --   78.00  65.00 135.98   91
 83  ω     57.00 147.00   1.00    6.00    --   78.00  54.00 -46.81   90
 84  ω     53.00 152.00   1.00   10.00    --   82.00  75.00 151.14   99
 85  ω     52.00 152.00   1.00   10.00    --   82.00  77.00 -91.27  100
 86  ω     58.00 150.00   1.00   10.00    --   82.00  67.00-139.43   92
 87  ω     57.00 154.00   1.00   10.00    --   82.00  39.00  54.99   97
 88  ω     61.00 151.00   1.00   10.00    --   82.00  56.00-153.84   90
 89  ω     62.00 154.00   1.00   10.00    --   86.00  68.00-103.32   92
 90  ω     61.00 122.00   1.00   10.00    --   86.00  69.00-148.39   61
 91  ω     63.00  89.00   1.00   10.00    --   86.00  65.00  28.12   26
 92  ω     66.00 104.00   1.00   10.00    --   90.00  67.00-101.17   38
 93  ω     67.00  94.00   1.00   10.00    --   90.00  46.00  79.98   27
 94  ω     70.00 142.00   1.00   10.00    --   90.00  59.00 -30.04   72
 95  ω     70.00  96.00   1.00   10.00    --   94.00  69.00  83.45   26
 96  ω     68.00 168.00   1.00   10.00    --   98.00  77.00 -26.01  100
 97  ω     69.00  95.00   1.00   10.00    --   98.00  75.00  44.32   26
 98  ω    100.00 125.00   1.00   10.00    --   98.00  75.00  82.87   25
 99  ω     69.00  98.00   1.00   10.00    --   98.00  75.00  82.87   29
100  ω     75.00 101.00   1.00   10.00    --   98.00  48.00 -32.26   26
101  ω     82.00 117.00   1.00   10.00    --  102.00  57.00 122.76   35
102  ω     79.00 105.00   1.00   10.00    --  102.00  66.00  63.94   26
103  ω     77.00 176.00   1.00   10.00    --  106.00  75.00 -67.95   99
104  ω     85.00 112.00   1.00   10.00    --  108.00  64.00-180.00   27
105  ω     85.00 112.00   1.00   10.00    --  108.00  64.00   0.00   27
106  ω     38.00 137.00   1.00   10.00    --  108.00 -77.00 -90.00   99
107  ω     85.00 152.00   1.00   10.00    --  108.00  64.00 150.00   67
108  ω     78.00 175.00   1.00   10.00    --  108.00  77.00 -60.00   97
109  ω     78.00 104.00   1.00   10.00    --  108.00  77.00 -90.00   26
110  ω     78.00 177.00   1.00   10.00    --  108.00  77.00  90.00   99
111  ω     85.00 175.00   1.00   10.00    --  108.00  64.00  30.00   90
112  ω     90.00 116.00   1.00   10.00    --  108.00-111.00-180.00   26
113  ω     37.00  62.00   1.00   10.00    --  108.00-111.00-180.00   25
114  ω     78.00 130.00   1.00   10.00    --  108.00  77.00-180.00   52
115  ω    113.00 178.00   1.00   10.00    --  108.00  77.00-120.00   65
116  ω     79.00 107.00   1.00   10.00    --  108.00  77.00-120.00   28
117  ω     78.00 177.00   1.00   10.00    --  108.00  77.00-150.00   99
118  ω    112.00 176.00   1.00   10.00    --  108.00  77.00 120.00   64
119  ω     85.00 111.00   1.00   10.00    --  108.00  64.00 -90.00   26
120  ω     79.00 108.00   1.00   10.00    --  108.00  77.00 120.00   29
121  ω    117.00 168.00   1.00   10.00    --  108.00  77.00   0.00   51
122  ω     78.00 108.00   1.00   10.00    --  108.00  77.00   0.00   30
123  ω     78.00 177.00   1.00   10.00    --  108.00  77.00 -30.00   99
124  ω     37.00 109.00   1.00   10.00    --  108.00-111.00  90.00   72
125  ω     78.00 104.00   1.00   10.00    --  108.00 -64.00-120.00   26
126  ω     46.00  72.00   1.00   10.00    --  108.00 -64.00-120.00   26
127  ω     78.00 178.00   1.00   10.00    --  108.00  77.00 150.00  100
128  ω     49.00 138.00   1.00   10.00    --  108.00 -77.00  90.00   89
129  ω     37.00 115.00   1.00   10.00    --  108.00-111.00 -90.00   78
130  ω     77.00 104.00   1.00   10.00    --  108.00-111.00  30.00   27
131  ω    147.00 173.00   1.00   10.00    --  108.00  72.00  78.23   26
132  ω     82.00 117.00   1.00   10.00    --  108.00  72.00  78.23   35
133  ω     86.00 113.00   1.00   10.00    --  108.00  62.00-121.89   27
134  ω     84.00 110.00   1.00   10.00    --  108.00  68.00 -85.62   26
135  ω     80.00 150.00   1.00   10.00    --  108.00  76.00-167.91   70
136  ω     85.00 112.00   1.00   10.00    --  108.00  77.00  60.00   27
137  ω     82.00 178.00   1.00   10.00    --  108.00  38.00  60.00   96
138  ω     85.00 149.00   1.00   10.00    --  108.00  38.00 -60.00   64
139  ω     85.00 113.00   1.00   10.00    --  108.00  38.00-150.00   28
140  ω     82.00 109.00   1.00   10.00    --  108.00  38.00-180.00   27
141  ω     86.00 111.00   1.00   10.00    --  108.00  64.00-120.00   25
142  ω     86.00 147.00   1.00   10.00    --  108.00  64.00-150.00   61
143  ω     81.00 108.00   1.00   10.00    --  108.00  77.00  30.00   27
144  ω     85.00 111.00   1.00   10.00    --  108.00  64.00 120.00   26
145  ω    131.00 157.00   1.00   10.00    --  108.00  64.00 -90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1210275000
_diffrn_orient_matrix_UB_12      -0.0084973000
_diffrn_orient_matrix_UB_13      -0.0186400000
_diffrn_orient_matrix_UB_21      0.0059216000
_diffrn_orient_matrix_UB_22      -0.1261104000
_diffrn_orient_matrix_UB_23      0.0039660000
_diffrn_orient_matrix_UB_31      -0.0407370000
_diffrn_orient_matrix_UB_32      0.0068012000
_diffrn_orient_matrix_UB_33      0.0503833000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7722
_reflns_number_total             8028
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         1.411
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         8028
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0288
_refine_ls_restrained_S_all      1.140
_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)+(0.0282P)²+9.2216P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0700
_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 distances
 O51-C51 \\sim O51-C53
 with sigma of 0.005
 C51-C52 \\sim C53-C54
 with sigma of 0.005
 O51-C52 \\sim O51-C54
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O51, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C45(H45A,H45B), C51(H51A,H51B), C53(H53A,H53B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42),
  C43(H43), C44(H44)
4.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C54(H54A,H54B,H54C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Hf Hf 0.33154(2) 0.40735(2) 0.19792(2) 0.01870(5) Uani 1 1 d . . . . .
Cl Cl 0.28795(6) 0.23332(5) 0.23691(2) 0.02503(15) Uani 1 1 d . . . . .
P1 P 0.32589(6) 0.29988(6) 0.11845(3) 0.02035(15) Uani 1 1 d . . . . .
P2 P 0.10414(6) 0.43381(6) 0.19125(3) 0.02003(15) Uani 1 1 d . . . . .
N N 0.3188(2) 0.53221(19) 0.14759(8) 0.0207(5) Uani 1 1 d . . . . .
C1 C 0.4560(3) 0.3402(2) 0.14570(11) 0.0229(6) Uani 1 1 d . . . . .
H1 H 0.506(3) 0.287(3) 0.1476(12) 0.027 Uiso 1 1 d R . . . .
C2 C 0.5034(3) 0.4511(3) 0.14363(10) 0.0228(6) Uani 1 1 d . . . . .
C3 C 0.4358(2) 0.5462(2) 0.14422(10) 0.0227(6) Uani 1 1 d . . . . .
C4 C 0.4849(3) 0.6517(3) 0.14631(11) 0.0268(7) Uani 1 1 d . . . . .
H4 H 0.4390 0.7151 0.1458 0.032 Uiso 1 1 calc R . . . .
C5 C 0.5985(3) 0.6633(3) 0.14910(11) 0.0323(7) Uani 1 1 d . . . . .
H5 H 0.6309 0.7344 0.1500 0.039 Uiso 1 1 calc R . . . .
C6 C 0.6658(3) 0.5698(3) 0.15060(12) 0.0321(7) Uani 1 1 d . . . . .
H6 H 0.7441 0.5776 0.1535 0.039 Uiso 1 1 calc R . . . .
C7 C 0.6198(3) 0.4669(3) 0.14799(11) 0.0282(7) Uani 1 1 d . . . . .
H7 H 0.6672 0.4046 0.1491 0.034 Uiso 1 1 calc R . . . .
C8 C 0.3049(3) 0.3525(2) 0.05921(10) 0.0220(6) Uani 1 1 d . . . . .
C9 C 0.1971(3) 0.3727(2) 0.04257(11) 0.0246(6) Uani 1 1 d . . . . .
H9 H 0.1365 0.3604 0.0623 0.030 Uiso 1 1 calc R . . . .
C10 C 0.1776(3) 0.4107(3) -0.00253(11) 0.0289(7) Uani 1 1 d . . . . .
H10 H 0.1038 0.4248 -0.0136 0.035 Uiso 1 1 calc R . . . .
C11 C 0.2651(3) 0.4280(3) -0.03131(12) 0.0328(8) Uani 1 1 d . . . . .
H11 H 0.2514 0.4532 -0.0624 0.039 Uiso 1 1 calc R . . . .
C12 C 0.3734(3) 0.4090(3) -0.01516(12) 0.0351(8) Uani 1 1 d . . . . .
H12 H 0.4336 0.4216 -0.0351 0.042 Uiso 1 1 calc R . . . .
C13 C 0.3933(3) 0.3713(3) 0.03020(11) 0.0285(7) Uani 1 1 d . . . . .
H13 H 0.4672 0.3585 0.0414 0.034 Uiso 1 1 calc R . . . .
C14 C 0.3355(3) 0.1515(2) 0.11038(10) 0.0229(6) Uani 1 1 d . . . . .
C15 C 0.2776(3) 0.1028(3) 0.07284(12) 0.0293(7) Uani 1 1 d . . . . .
H15 H 0.2356 0.1474 0.0515 0.035 Uiso 1 1 calc R . . . .
C16 C 0.2807(3) -0.0101(3) 0.06623(12) 0.0316(7) Uani 1 1 d . . . . .
H16 H 0.2410 -0.0424 0.0405 0.038 Uiso 1 1 calc R . . . .
C17 C 0.3411(3) -0.0750(3) 0.09695(12) 0.0321(7) Uani 1 1 d . . . . .
H17 H 0.3441 -0.1521 0.0922 0.039 Uiso 1 1 calc R . . . .
C18 C 0.3977(3) -0.0280(3) 0.13478(12) 0.0333(8) Uani 1 1 d . . . . .
H18 H 0.4392 -0.0731 0.1560 0.040 Uiso 1 1 calc R . . . .
C19 C 0.3943(3) 0.0847(2) 0.14190(11) 0.0277(7) Uani 1 1 d . . . . .
H19 H 0.4321 0.1162 0.1683 0.033 Uiso 1 1 calc R . . . .
C20 C 0.0882(3) 0.5764(2) 0.17111(11) 0.0240(6) Uani 1 1 d . . . . .
H20A H 0.0081 0.5945 0.1696 0.029 Uiso 1 1 calc R . . . .
H20B H 0.1241 0.6253 0.1948 0.029 Uiso 1 1 calc R . . . .
C21 C 0.1359(3) 0.6017(2) 0.12416(11) 0.0228(6) Uani 1 1 d . . . . .
C22 C 0.2489(3) 0.5868(2) 0.11517(10) 0.0216(6) Uani 1 1 d . . . . .
C23 C 0.2886(3) 0.6235(2) 0.07249(11) 0.0242(6) Uani 1 1 d . . . . .
H23 H 0.3651 0.6151 0.0664 0.029 Uiso 1 1 calc R . . . .
C24 C 0.2192(3) 0.6718(3) 0.03910(11) 0.0294(7) Uani 1 1 d . . . . .
H24 H 0.2485 0.6974 0.0107 0.035 Uiso 1 1 calc R . . . .
C25 C 0.1072(3) 0.6831(3) 0.04683(11) 0.0314(7) Uani 1 1 d . . . . .
H25 H 0.0586 0.7139 0.0235 0.038 Uiso 1 1 calc R . . . .
C26 C 0.0671(3) 0.6485(2) 0.08937(11) 0.0276(7) Uani 1 1 d . . . . .
H26 H -0.0097 0.6570 0.0949 0.033 Uiso 1 1 calc R . . . .
C27 C 0.0255(2) 0.3491(2) 0.14921(10) 0.0218(6) Uani 1 1 d . . . . .
C28 C -0.0602(3) 0.3910(3) 0.12079(11) 0.0278(7) Uani 1 1 d . . . . .
H28 H -0.0785 0.4668 0.1225 0.033 Uiso 1 1 calc R . . . .
C29 C -0.1191(3) 0.3231(3) 0.09004(12) 0.0349(8) Uani 1 1 d . . . . .
H29 H -0.1769 0.3527 0.0705 0.042 Uiso 1 1 calc R . . . .
C30 C -0.0941(3) 0.2120(3) 0.08769(12) 0.0338(8) Uani 1 1 d . . . . .
H30 H -0.1345 0.1655 0.0666 0.041 Uiso 1 1 calc R . . . .
C31 C -0.0096(3) 0.1696(3) 0.11626(12) 0.0296(7) Uani 1 1 d . . . . .
H31 H 0.0075 0.0935 0.1149 0.035 Uiso 1 1 calc R . . . .
C32 C 0.0505(3) 0.2376(2) 0.14693(11) 0.0247(6) Uani 1 1 d . . . . .
H32 H 0.1086 0.2079 0.1663 0.030 Uiso 1 1 calc R . . . .
C33 C 0.0163(3) 0.4268(2) 0.24224(11) 0.0235(6) Uani 1 1 d . . . . .
C34 C 0.0465(3) 0.3562(3) 0.27889(11) 0.0279(7) Uani 1 1 d . . . . .
H34 H 0.1117 0.3127 0.2771 0.033 Uiso 1 1 calc R . . . .
C35 C -0.0179(3) 0.3493(3) 0.31782(12) 0.0351(8) Uani 1 1 d . . . . .
H35 H 0.0046 0.3025 0.3429 0.042 Uiso 1 1 calc R . . . .
C36 C -0.1144(4) 0.4092(3) 0.32082(14) 0.0405(9) Uani 1 1 d . . . . .
H36 H -0.1583 0.4034 0.3477 0.049 Uiso 1 1 calc R . . . .
C37 C -0.1467(3) 0.4776(3) 0.28438(14) 0.0423(9) Uani 1 1 d . . . . .
H37 H -0.2136 0.5186 0.2860 0.051 Uiso 1 1 calc R . . . .
C38 C -0.0815(3) 0.4868(3) 0.24529(13) 0.0338(8) Uani 1 1 d . . . . .
H38 H -0.1040 0.5344 0.2204 0.041 Uiso 1 1 calc R . . . .
C39 C 0.3871(3) 0.5374(3) 0.26708(10) 0.0238(6) Uani 1 1 d . . . . .
C40 C 0.2848(3) 0.5095(3) 0.28573(11) 0.0282(7) Uani 1 1 d . . . . .
H40 H 0.2695 0.4346 0.2923 0.034 Uiso 1 1 calc R . . . .
C41 C 0.2045(3) 0.5893(3) 0.29499(13) 0.0339(8) Uani 1 1 d . . . . .
H41 H 0.1366 0.5684 0.3084 0.041 Uiso 1 1 calc R . . . .
C42 C 0.2239(3) 0.6978(3) 0.28462(13) 0.0336(8) Uani 1 1 d . . . . .
H42 H 0.1697 0.7521 0.2908 0.040 Uiso 1 1 calc R . . . .
C43 C 0.3236(3) 0.7272(3) 0.26504(12) 0.0304(7) Uani 1 1 d . . . . .
H43 H 0.3369 0.8020 0.2577 0.036 Uiso 1 1 calc R . . . .
C44 C 0.4035(3) 0.6499(3) 0.25615(11) 0.0266(7) Uani 1 1 d . . . . .
H44 H 0.4707 0.6721 0.2425 0.032 Uiso 1 1 calc R . . . .
C45 C 0.4648(3) 0.4521(3) 0.25302(11) 0.0263(7) Uani 1 1 d . . . . .
H45A H 0.4795 0.3945 0.2769 0.032 Uiso 1 1 calc R . . . .
H45B H 0.5345 0.4804 0.2402 0.032 Uiso 1 1 calc R . . . .
O51 O 0.2604(4) -0.0042(3) -0.05050(13) 0.0818(11) Uani 1 1 d D U . . .
C51 C 0.3684(6) -0.0199(6) -0.0627(3) 0.122(3) Uani 1 1 d D U . . .
H51A H 0.4162 0.0388 -0.0490 0.146 Uiso 1 1 calc R . . . .
H51B H 0.3739 -0.0176 -0.0971 0.146 Uiso 1 1 calc R . . . .
C52 C 0.4072(5) -0.1344(7) -0.0436(3) 0.115(3) Uani 1 1 d D U . . .
H52A H 0.3658 -0.1925 -0.0603 0.172 Uiso 1 1 calc GR . . . .
H52B H 0.3934 -0.1390 -0.0101 0.172 Uiso 1 1 calc GR . . . .
H52C H 0.4867 -0.1435 -0.0486 0.172 Uiso 1 1 calc GR . . . .
C53 C 0.2131(9) 0.0937(6) -0.0656(3) 0.154(4) Uani 1 1 d D U . . .
H53A H 0.2081 0.0964 -0.1001 0.185 Uiso 1 1 calc R . . . .
H53B H 0.2579 0.1569 -0.0540 0.185 Uiso 1 1 calc R . . . .
C54 C 0.0939(8) 0.0968(7) -0.0448(3) 0.168(4) Uani 1 1 d D U . . .
H54A H 0.0380 0.1014 -0.0704 0.252 Uiso 1 1 calc GR . . . .
H54B H 0.0876 0.1611 -0.0244 0.252 Uiso 1 1 calc GR . . . .
H54C H 0.0819 0.0299 -0.0266 0.252 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
Hf Cl 2.4593(7) . ?
Hf P1 2.6224(7) . ?
Hf P2 2.7607(8) . ?
Hf N 2.096(2) . ?
Hf C1 2.302(3) . ?
Hf C2 2.684(3) . ?
Hf C3 2.632(3) . ?
Hf C39 2.604(3) . ?
Hf C45 2.279(3) . ?
P1 C1 1.797(3) . ?
P1 C8 1.822(3) . ?
P1 C14 1.825(3) . ?
P2 C20 1.837(3) . ?
P2 C27 1.825(3) . ?
P2 C33 1.833(3) . ?
N C3 1.427(4) . ?
N C22 1.400(4) . ?
C1 H1 0.89(4) . ?
C1 C2 1.469(4) . ?
C2 C3 1.416(4) . ?
C2 C7 1.418(4) . ?
C3 C4 1.414(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.376(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.399(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.370(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.390(4) . ?
C8 C13 1.392(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.384(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.376(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.390(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.390(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.394(4) . ?
C14 C19 1.391(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.388(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.373(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.384(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.387(4) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.510(4) . ?
C21 C22 1.407(5) . ?
C21 C26 1.396(4) . ?
C22 C23 1.399(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.380(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.381(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.390(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.390(4) . ?
C27 C32 1.393(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.386(5) . ?
C29 H29 0.9500 . ?
C29 C30 1.388(5) . ?
C30 H30 0.9500 . ?
C30 C31 1.384(5) . ?
C31 H31 0.9500 . ?
C31 C32 1.392(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.395(4) . ?
C33 C38 1.391(5) . ?
C34 H34 0.9500 . ?
C34 C35 1.382(5) . ?
C35 H35 0.9500 . ?
C35 C36 1.378(6) . ?
C36 H36 0.9500 . ?
C36 C37 1.381(6) . ?
C37 H37 0.9500 . ?
C37 C38 1.393(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.402(5) . ?
C39 C44 1.420(5) . ?
C39 C45 1.464(4) . ?
C40 H40 0.9500 . ?
C40 C41 1.403(5) . ?
C41 H41 0.9500 . ?
C41 C42 1.376(5) . ?
C42 H42 0.9500 . ?
C42 C43 1.390(5) . ?
C43 H43 0.9500 . ?
C43 C44 1.376(5) . ?
C44 H44 0.9500 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
O51 C51 1.373(6) . ?
O51 C53 1.384(6) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 C52 1.563(9) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.574(9) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 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
Cl Hf P1 87.91(2) . . ?
Cl Hf P2 84.56(2) . . ?
Cl Hf C2 127.90(7) . . ?
Cl Hf C3 158.67(7) . . ?
Cl Hf C39 103.45(7) . . ?
P1 Hf P2 90.07(2) . . ?
P1 Hf C2 66.15(7) . . ?
P1 Hf C3 79.25(7) . . ?
N Hf Cl 157.60(7) . . ?
N Hf P1 76.52(7) . . ?
N Hf P2 79.53(7) . . ?
N Hf C1 81.13(10) . . ?
N Hf C2 59.90(9) . . ?
N Hf C3 32.70(9) . . ?
N Hf C39 95.30(9) . . ?
N Hf C45 109.61(11) . . ?
C1 Hf Cl 98.18(8) . . ?
C1 Hf P1 42.17(8) . . ?
C1 Hf P2 131.57(8) . . ?
C1 Hf C2 33.14(10) . . ?
C1 Hf C3 60.98(10) . . ?
C1 Hf C39 123.52(10) . . ?
C2 Hf P2 136.12(6) . . ?
C3 Hf P2 112.16(7) . . ?
C3 Hf C2 30.87(9) . . ?
C39 Hf P1 163.89(7) . . ?
C39 Hf P2 102.21(7) . . ?
C39 Hf C2 97.76(9) . . ?
C39 Hf C3 86.40(9) . . ?
C45 Hf Cl 92.78(9) . . ?
C45 Hf P1 135.75(8) . . ?
C45 Hf P2 134.08(8) . . ?
C45 Hf C1 94.24(11) . . ?
C45 Hf C2 79.20(10) . . ?
C45 Hf C3 84.88(11) . . ?
C45 Hf C39 34.07(10) . . ?
C1 P1 Hf 59.34(10) . . ?
C1 P1 C8 113.58(14) . . ?
C1 P1 C14 105.52(14) . . ?
C8 P1 Hf 129.05(9) . . ?
C8 P1 C14 103.77(13) . . ?
C14 P1 Hf 127.12(10) . . ?
C20 P2 Hf 103.00(10) . . ?
C27 P2 Hf 118.19(10) . . ?
C27 P2 C20 106.29(14) . . ?
C27 P2 C33 101.37(14) . . ?
C33 P2 Hf 122.57(10) . . ?
C33 P2 C20 103.67(14) . . ?
C3 N Hf 94.78(17) . . ?
C22 N Hf 145.9(2) . . ?
C22 N C3 118.2(2) . . ?
Hf C1 H1 133(2) . . ?
P1 C1 Hf 78.49(12) . . ?
P1 C1 H1 114(2) . . ?
C2 C1 Hf 87.88(18) . . ?
C2 C1 P1 124.7(2) . . ?
C2 C1 H1 114(2) . . ?
C1 C2 Hf 58.98(16) . . ?
C3 C2 Hf 72.52(17) . . ?
C3 C2 C1 121.7(3) . . ?
C3 C2 C7 117.2(3) . . ?
C7 C2 Hf 139.2(2) . . ?
C7 C2 C1 120.5(3) . . ?
N C3 Hf 52.52(14) . . ?
C2 C3 Hf 76.60(18) . . ?
C2 C3 N 118.3(3) . . ?
C4 C3 Hf 140.0(2) . . ?
C4 C3 N 121.2(3) . . ?
C4 C3 C2 120.2(3) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.7(3) . . ?
C5 C4 H4 119.7 . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.6(3) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.6(3) . . ?
C7 C6 H6 119.7 . . ?
C2 C7 H7 119.1 . . ?
C6 C7 C2 121.7(3) . . ?
C6 C7 H7 119.1 . . ?
C9 C8 P1 118.7(2) . . ?
C9 C8 C13 119.5(3) . . ?
C13 C8 P1 121.8(2) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.0(3) . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.4(3) . . ?
C12 C11 H11 119.8 . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.8(3) . . ?
C13 C12 H12 120.1 . . ?
C8 C13 H13 120.0 . . ?
C12 C13 C8 119.9(3) . . ?
C12 C13 H13 120.0 . . ?
C15 C14 P1 119.1(2) . . ?
C19 C14 P1 122.0(2) . . ?
C19 C14 C15 118.8(3) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 C14 120.8(3) . . ?
C16 C15 H15 119.6 . . ?
C15 C16 H16 120.1 . . ?
C17 C16 C15 119.9(3) . . ?
C17 C16 H16 120.1 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.0(3) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 119.7 . . ?
C17 C18 C19 120.5(3) . . ?
C19 C18 H18 119.7 . . ?
C14 C19 H19 120.0 . . ?
C18 C19 C14 120.0(3) . . ?
C18 C19 H19 120.0 . . ?
P2 C20 H20A 108.4 . . ?
P2 C20 H20B 108.4 . . ?
H20A C20 H20B 107.4 . . ?
C21 C20 P2 115.7(2) . . ?
C21 C20 H20A 108.4 . . ?
C21 C20 H20B 108.4 . . ?
C22 C21 C20 122.4(3) . . ?
C26 C21 C20 118.9(3) . . ?
C26 C21 C22 118.6(3) . . ?
N C22 C21 120.4(3) . . ?
C23 C22 N 121.0(3) . . ?
C23 C22 C21 118.6(3) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 C22 121.6(3) . . ?
C24 C23 H23 119.2 . . ?
C23 C24 H24 119.8 . . ?
C23 C24 C25 120.3(3) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 120.6 . . ?
C24 C25 C26 118.7(3) . . ?
C26 C25 H25 120.6 . . ?
C21 C26 H26 118.9 . . ?
C25 C26 C21 122.2(3) . . ?
C25 C26 H26 118.9 . . ?
C28 C27 P2 122.5(2) . . ?
C28 C27 C32 119.2(3) . . ?
C32 C27 P2 118.2(2) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 C27 120.5(3) . . ?
C29 C28 H28 119.7 . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C30 120.3(3) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 120.3 . . ?
C31 C30 C29 119.5(3) . . ?
C31 C30 H30 120.3 . . ?
C30 C31 H31 119.7 . . ?
C30 C31 C32 120.5(3) . . ?
C32 C31 H31 119.7 . . ?
C27 C32 H32 120.0 . . ?
C31 C32 C27 120.0(3) . . ?
C31 C32 H32 120.0 . . ?
C34 C33 P2 118.9(2) . . ?
C38 C33 P2 122.6(2) . . ?
C38 C33 C34 118.5(3) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 C33 120.2(3) . . ?
C35 C34 H34 119.9 . . ?
C34 C35 H35 119.4 . . ?
C36 C35 C34 121.1(3) . . ?
C36 C35 H35 119.4 . . ?
C35 C36 H36 120.3 . . ?
C35 C36 C37 119.3(3) . . ?
C37 C36 H36 120.3 . . ?
C36 C37 H37 119.9 . . ?
C36 C37 C38 120.1(3) . . ?
C38 C37 H37 119.9 . . ?
C33 C38 C37 120.7(3) . . ?
C33 C38 H38 119.6 . . ?
C37 C38 H38 119.6 . . ?
C40 C39 Hf 86.26(18) . . ?
C40 C39 C44 116.6(3) . . ?
C40 C39 C45 120.8(3) . . ?
C44 C39 Hf 116.9(2) . . ?
C44 C39 C45 121.9(3) . . ?
C45 C39 Hf 60.72(15) . . ?
C39 C40 H40 119.1 . . ?
C39 C40 C41 121.7(3) . . ?
C41 C40 H40 119.1 . . ?
C40 C41 H41 120.0 . . ?
C42 C41 C40 120.0(3) . . ?
C42 C41 H41 120.0 . . ?
C41 C42 H42 120.3 . . ?
C41 C42 C43 119.3(3) . . ?
C43 C42 H42 120.3 . . ?
C42 C43 H43 119.4 . . ?
C44 C43 C42 121.2(3) . . ?
C44 C43 H43 119.4 . . ?
C39 C44 H44 119.5 . . ?
C43 C44 C39 121.0(3) . . ?
C43 C44 H44 119.5 . . ?
Hf C45 H45A 114.4 . . ?
Hf C45 H45B 114.4 . . ?
C39 C45 Hf 85.21(17) . . ?
C39 C45 H45A 114.4 . . ?
C39 C45 H45B 114.4 . . ?
H45A C45 H45B 111.6 . . ?
C51 O51 C53 115.2(7) . . ?
O51 C51 H51A 110.1 . . ?
O51 C51 H51B 110.1 . . ?
O51 C51 C52 108.1(5) . . ?
H51A C51 H51B 108.4 . . ?
C52 C51 H51A 110.1 . . ?
C52 C51 H51B 110.1 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O51 C53 H53A 110.5 . . ?
O51 C53 H53B 110.5 . . ?
O51 C53 C54 106.0(6) . . ?
H53A C53 H53B 108.7 . . ?
C54 C53 H53A 110.5 . . ?
C54 C53 H53B 110.5 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 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
Hf P1 C1 C2 -79.2(3) . . . . ?
Hf P1 C8 C9 -81.8(3) . . . . ?
Hf P1 C8 C13 99.1(3) . . . . ?
Hf P1 C14 C15 147.1(2) . . . . ?
Hf P1 C14 C19 -29.6(3) . . . . ?
Hf P2 C20 C21 61.5(2) . . . . ?
Hf P2 C27 C28 -137.3(2) . . . . ?
Hf P2 C27 C32 44.9(3) . . . . ?
Hf P2 C33 C34 -33.1(3) . . . . ?
Hf P2 C33 C38 148.9(2) . . . . ?
Hf N C3 C2 41.9(3) . . . . ?
Hf N C3 C4 -131.6(3) . . . . ?
Hf N C22 C21 34.0(5) . . . . ?
Hf N C22 C23 -143.5(3) . . . . ?
Hf C1 C2 C3 -38.4(3) . . . . ?
Hf C1 C2 C7 132.1(3) . . . . ?
Hf C2 C3 N -33.0(2) . . . . ?
Hf C2 C3 C4 140.5(3) . . . . ?
Hf C2 C7 C6 -97.3(4) . . . . ?
Hf C3 C4 C5 104.2(4) . . . . ?
Hf C39 C40 C41 -121.0(3) . . . . ?
Hf C39 C44 C43 102.0(3) . . . . ?
P1 C1 C2 Hf 74.4(2) . . . . ?
P1 C1 C2 C3 36.0(4) . . . . ?
P1 C1 C2 C7 -153.4(3) . . . . ?
P1 C8 C9 C10 -178.8(2) . . . . ?
P1 C8 C13 C12 178.4(3) . . . . ?
P1 C14 C15 C16 -178.4(3) . . . . ?
P1 C14 C19 C18 178.9(3) . . . . ?
P2 C20 C21 C22 -59.3(3) . . . . ?
P2 C20 C21 C26 125.1(3) . . . . ?
P2 C27 C28 C29 -178.7(3) . . . . ?
P2 C27 C32 C31 178.2(2) . . . . ?
P2 C33 C34 C35 179.9(2) . . . . ?
P2 C33 C38 C37 178.9(3) . . . . ?
N C3 C4 C5 171.6(3) . . . . ?
N C22 C23 C24 176.2(3) . . . . ?
C1 P1 C8 C9 -150.6(2) . . . . ?
C1 P1 C8 C13 30.3(3) . . . . ?
C1 P1 C14 C15 -149.8(3) . . . . ?
C1 P1 C14 C19 33.4(3) . . . . ?
C1 C2 C3 Hf 33.9(3) . . . . ?
C1 C2 C3 N 0.9(4) . . . . ?
C1 C2 C3 C4 174.5(3) . . . . ?
C1 C2 C7 C6 -173.8(3) . . . . ?
C2 C3 C4 C5 -1.8(5) . . . . ?
C3 N C22 C21 -162.0(3) . . . . ?
C3 N C22 C23 20.6(4) . . . . ?
C3 C2 C7 C6 -2.8(5) . . . . ?
C3 C4 C5 C6 -1.0(5) . . . . ?
C4 C5 C6 C7 1.9(5) . . . . ?
C5 C6 C7 C2 0.1(5) . . . . ?
C7 C2 C3 Hf -136.9(3) . . . . ?
C7 C2 C3 N -170.0(3) . . . . ?
C7 C2 C3 C4 3.6(4) . . . . ?
C8 P1 C1 Hf 122.71(12) . . . . ?
C8 P1 C1 C2 43.5(3) . . . . ?
C8 P1 C14 C15 -30.2(3) . . . . ?
C8 P1 C14 C19 153.1(3) . . . . ?
C8 C9 C10 C11 0.4(5) . . . . ?
C9 C8 C13 C12 -0.7(5) . . . . ?
C9 C10 C11 C12 -0.8(5) . . . . ?
C10 C11 C12 C13 0.5(5) . . . . ?
C11 C12 C13 C8 0.2(5) . . . . ?
C13 C8 C9 C10 0.3(4) . . . . ?
C14 P1 C1 Hf -124.30(12) . . . . ?
C14 P1 C1 C2 156.5(3) . . . . ?
C14 P1 C8 C9 95.4(3) . . . . ?
C14 P1 C8 C13 -83.7(3) . . . . ?
C14 C15 C16 C17 0.1(6) . . . . ?
C15 C14 C19 C18 2.2(5) . . . . ?
C15 C16 C17 C18 0.9(6) . . . . ?
C16 C17 C18 C19 -0.3(6) . . . . ?
C17 C18 C19 C14 -1.3(6) . . . . ?
C19 C14 C15 C16 -1.6(5) . . . . ?
C20 P2 C27 C28 -22.3(3) . . . . ?
C20 P2 C27 C32 159.9(2) . . . . ?
C20 P2 C33 C34 -148.6(2) . . . . ?
C20 P2 C33 C38 33.5(3) . . . . ?
C20 C21 C22 N 9.5(4) . . . . ?
C20 C21 C22 C23 -173.0(3) . . . . ?
C20 C21 C26 C25 174.1(3) . . . . ?
C21 C22 C23 C24 -1.2(4) . . . . ?
C22 N C3 Hf -171.1(3) . . . . ?
C22 N C3 C2 -129.1(3) . . . . ?
C22 N C3 C4 57.3(4) . . . . ?
C22 C21 C26 C25 -1.7(4) . . . . ?
C22 C23 C24 C25 -1.2(5) . . . . ?
C23 C24 C25 C26 2.2(5) . . . . ?
C24 C25 C26 C21 -0.7(5) . . . . ?
C26 C21 C22 N -174.9(3) . . . . ?
C26 C21 C22 C23 2.6(4) . . . . ?
C27 P2 C20 C21 -63.4(3) . . . . ?
C27 P2 C33 C34 101.3(3) . . . . ?
C27 P2 C33 C38 -76.6(3) . . . . ?
C27 C28 C29 C30 0.8(6) . . . . ?
C28 C27 C32 C31 0.4(5) . . . . ?
C28 C29 C30 C31 -0.1(6) . . . . ?
C29 C30 C31 C32 -0.5(5) . . . . ?
C30 C31 C32 C27 0.3(5) . . . . ?
C32 C27 C28 C29 -0.9(5) . . . . ?
C33 P2 C20 C21 -169.8(2) . . . . ?
C33 P2 C27 C28 85.7(3) . . . . ?
C33 P2 C27 C32 -92.0(3) . . . . ?
C33 C34 C35 C36 1.8(5) . . . . ?
C34 C33 C38 C37 1.0(5) . . . . ?
C34 C35 C36 C37 -0.4(5) . . . . ?
C35 C36 C37 C38 -0.7(6) . . . . ?
C36 C37 C38 C33 0.4(6) . . . . ?
C38 C33 C34 C35 -2.1(5) . . . . ?
C39 C40 C41 C42 1.7(5) . . . . ?
C40 C39 C44 C43 2.0(4) . . . . ?
C40 C39 C45 Hf 65.1(3) . . . . ?
C40 C41 C42 C43 -0.1(5) . . . . ?
C41 C42 C43 C44 -0.4(5) . . . . ?
C42 C43 C44 C39 -0.6(5) . . . . ?
C44 C39 C40 C41 -2.6(5) . . . . ?
C44 C39 C45 Hf -105.2(3) . . . . ?
C45 C39 C40 C41 -173.4(3) . . . . ?
C45 C39 C44 C43 172.7(3) . . . . ?
C51 O51 C53 C54 -176.2(7) . . . . ?
C53 O51 C51 C52 -179.1(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.205
_oxdiff_exptl_absorpt_empirical_full_min 0.864
_cell_oxdiff_length_a            12.05757(13)
_cell_oxdiff_length_b            12.17073(10)
_cell_oxdiff_length_c            28.6149(3)
_cell_oxdiff_angle_alpha         90.0070(8)
_cell_oxdiff_angle_beta          91.8888(9)
_cell_oxdiff_angle_gamma         90.0160(8)
_cell_oxdiff_volume              4196.94(8)
_cell_oxdiff_measurement_reflns_used 96329
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ba_jb32_sq
_database_code_depnum_ccdc_archive 'CCDC 1530471'
_audit_update_record             
;
2017-03-17 deposited with the CCDC.
2017-04-05 downloaded from the CCDC.
;
_audit_creation_date             2016-08-05

_audit_block_code                ba_jb32
_audit_block_refno               2750
_audit_block_usercomment         'jb300, needle, orange'


# start Validation Reply Form
_vrf_PLAT910_ba_jb32_sq          
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          14 Note
RESPONSE: limited by diffractometer.
;
# end Validation Reply Form

_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C52 H45 N P2 Zr'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_formula_weight         837.05
_chemical_melting_point          ?
_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_diffrn_ambient_temperature      120(1)
_chemical_oxdiff_formula         'C63 H45 N P2 Zr'
_chemical_oxdiff_usercomment     'jb300, needle, orange'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/n'
_symmetry_int_tables_number      14
_chemical_absolute_configuration .

_space_group_name_Hall           '-P 2yn'
loop_
_symmetry_equiv_pos_as_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                   14.04739(15)
_cell_length_b                   12.35375(14)
_cell_length_c                   28.0234(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.1365(10)
_cell_angle_gamma                90
_cell_volume                     4814.18(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    43081
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      31.7350
_cell_measurement_theta_min      3.2640
_shelx_estimated_absorpt_T_max   0.968
_shelx_estimated_absorpt_T_min   0.968
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1736
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-18 -1 21 0.0696
1 -17 -7 0.0882
-1 17 7 0.0882
18 2 -20 0.0629
-1 -2 -39 0.0337
16 -9 9 0.0792
-16 9 -9 0.0792
1 2 39 0.0337
10 -11 20 0.0665
17 2 14 0.0593
-3 8 -33 0.0677
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.067
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-18.0031 -1.0005 21.0004 -0.0648 0.6052 0.7902
1.0000 -17.0024 -7.0032 -0.0659 0.7455 -0.6517
-1.0000 17.0024 7.0032 0.0659 -0.7455 0.6517
18.0030 2.0006 -20.0001 0.0535 -0.6501 -0.7478
-0.9992 -1.9983 -39.0069 0.9107 0.0774 -0.4356
16.0019 -9.0025 9.0029 -0.7076 -0.0508 -0.7324
-16.0019 9.0025 -9.0029 0.7076 0.0508 0.7324
0.9992 1.9983 39.0069 -0.9107 -0.0774 0.4356
10.0000 -11.0000 20.0005 -0.8425 0.2321 -0.4808
17.0000 2.0000 14.0001 -0.7157 -0.5817 -0.3610
-3.0001 8.0000 -33.0001 0.9397 -0.3168 0.0146

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            169444
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.344
_diffrn_reflns_theta_min         2.937
_diffrn_ambient_environment      perfluoro
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -41.00  50.00   0.50   12.50    --   28.16 -57.00 -60.00  182
  2  ω      7.00  97.00   0.50   12.50    --   28.16  57.00 -90.00  180
  3  ω    -20.00  72.00   0.50   12.50    --   28.16 -99.00-120.00  184
  4  ω      7.00  97.00   0.50   12.50    --   28.16  57.00   0.00  180
  5  ω      7.00  97.00   0.50   12.50    --   28.16  57.00  90.00  180
  6  ω    -20.00  72.00   0.50   12.50    --   28.16 -99.00  60.00  184
  7  ω     -6.00  23.00   0.50   12.50    --   28.16  82.00 -51.01   58
  8  ω    -41.00  50.00   0.50   12.50    --   28.16 -57.00 120.00  182
  9  ω      1.00 101.00   0.50   12.50    --   28.16  38.00-150.00  200
 10  ω     -5.00  24.00   0.50   12.50    --   28.16  80.00 145.92   58
 11  ω    -58.00 -27.00   0.50   12.50    --    4.00 132.00  51.95   62
 12  ω     -3.00  99.00   0.50   12.50    --   28.16  77.00-150.00  204
 13  ω    -20.00  72.00   0.50   12.50    --   28.16 -99.00  90.00  184
 14  ω     -3.00  99.00   0.50   12.50    --   28.16  77.00  60.00  204
 15  ω     -6.00  24.00   0.50   12.50    --   28.16  81.00  -4.40   60
 16  ω    -20.00  72.00   0.50   12.50    --   28.16 -99.00   0.00  184
 17  ω    -41.00  50.00   0.50   12.50    --   28.16 -57.00 150.00  182
 18  ω    -41.00  50.00   0.50   12.50    --   28.16 -57.00-150.00  182
 19  ω      1.00  44.00   0.50   12.50    --   28.16  38.00-120.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0242983000
_diffrn_orient_matrix_UB_12      0.0120622000
_diffrn_orient_matrix_UB_13      -0.0233419000
_diffrn_orient_matrix_UB_21      -0.0297312000
_diffrn_orient_matrix_UB_22      -0.0460661000
_diffrn_orient_matrix_UB_23      0.0011361000
_diffrn_orient_matrix_UB_31      -0.0335633000
_diffrn_orient_matrix_UB_32      0.0320794000
_diffrn_orient_matrix_UB_33      0.0103845000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15033
_reflns_number_total             16744
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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,
 see _platon_squeeze_.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2014/7
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.991
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         16744
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0553
_refine_ls_restrained_S_all      1.190
_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)+(0.0353P)²+5.0742P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1118
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.54370(2) 0.20039(2) 0.13654(2) 0.01098(4) Uani 1 1 d . . . . .
P1 P 0.46477(3) 0.35711(4) 0.19356(2) 0.01240(8) Uani 1 1 d . . . . .
P2 P 0.39364(3) 0.07147(4) 0.15199(2) 0.01179(8) Uani 1 1 d . . . . .
N N 0.58080(10) 0.15362(12) 0.21067(5) 0.0123(3) Uani 1 1 d . . . . .
C1 C 0.57974(13) 0.36493(15) 0.17274(6) 0.0136(3) Uani 1 1 d . . . . .
H1 H 0.5855(17) 0.424(2) 0.1533(9) 0.016 Uiso 1 1 d R . . . .
C2 C 0.66962(13) 0.31500(14) 0.19462(6) 0.0140(3) Uani 1 1 d . . . . .
C3 C 0.67010(12) 0.20989(15) 0.21519(6) 0.0135(3) Uani 1 1 d . . . . .
C4 C 0.75842(13) 0.15933(16) 0.23233(7) 0.0169(3) Uani 1 1 d . . . . .
H4 H 0.7586 0.0903 0.2473 0.020 Uiso 1 1 calc R . . . .
C5 C 0.84463(13) 0.20902(18) 0.22758(8) 0.0219(4) Uani 1 1 d . . . . .
H5 H 0.9037 0.1735 0.2386 0.026 Uiso 1 1 calc R . . . .
C6 C 0.84484(14) 0.31203(18) 0.20650(8) 0.0235(4) Uani 1 1 d . . . . .
H6 H 0.9042 0.3465 0.2035 0.028 Uiso 1 1 calc R . . . .
C7 C 0.75954(14) 0.36335(16) 0.19015(7) 0.0191(4) Uani 1 1 d . . . . .
H7 H 0.7609 0.4326 0.1756 0.023 Uiso 1 1 calc R . . . .
C8 C 0.48002(13) 0.36424(15) 0.25943(6) 0.0142(3) Uani 1 1 d . . . . .
C9 C 0.40871(13) 0.32066(15) 0.28365(7) 0.0172(3) Uani 1 1 d . . . . .
H9 H 0.3558 0.2834 0.2661 0.021 Uiso 1 1 calc R . . . .
C10 C 0.41482(15) 0.33167(18) 0.33341(7) 0.0226(4) Uani 1 1 d . . . . .
H10 H 0.3660 0.3021 0.3498 0.027 Uiso 1 1 calc R . . . .
C11 C 0.49230(16) 0.3859(2) 0.35916(7) 0.0255(4) Uani 1 1 d . . . . .
H11 H 0.4959 0.3943 0.3931 0.031 Uiso 1 1 calc R . . . .
C12 C 0.56449(15) 0.42782(19) 0.33551(8) 0.0243(4) Uani 1 1 d . . . . .
H12 H 0.6180 0.4637 0.3533 0.029 Uiso 1 1 calc R . . . .
C13 C 0.55837(13) 0.41720(16) 0.28594(7) 0.0183(4) Uani 1 1 d . . . . .
H13 H 0.6078 0.4461 0.2698 0.022 Uiso 1 1 calc R . . . .
C14 C 0.41489(13) 0.49232(15) 0.17907(6) 0.0139(3) Uani 1 1 d . . . . .
C15 C 0.31484(13) 0.50414(16) 0.17132(7) 0.0174(3) Uani 1 1 d . . . . .
H15 H 0.2749 0.4424 0.1724 0.021 Uiso 1 1 calc R . . . .
C16 C 0.27342(14) 0.60543(17) 0.16210(8) 0.0226(4) Uani 1 1 d . . . . .
H16 H 0.2054 0.6129 0.1575 0.027 Uiso 1 1 calc R . . . .
C17 C 0.33126(15) 0.69599(17) 0.15958(8) 0.0232(4) Uani 1 1 d . . . . .
H17 H 0.3029 0.7650 0.1525 0.028 Uiso 1 1 calc R . . . .
C18 C 0.43057(15) 0.68525(16) 0.16736(8) 0.0206(4) Uani 1 1 d . . . . .
H18 H 0.4703 0.7471 0.1659 0.025 Uiso 1 1 calc R . . . .
C19 C 0.47198(13) 0.58432(15) 0.17730(7) 0.0162(3) Uani 1 1 d . . . . .
H19 H 0.5400 0.5777 0.1830 0.019 Uiso 1 1 calc R . . . .
C20 C 0.43887(13) -0.02146(15) 0.20105(7) 0.0145(3) Uani 1 1 d . . . . .
H20A H 0.3895(17) -0.075(2) 0.2072(9) 0.017 Uiso 1 1 d R . . . .
H20B H 0.4893(17) -0.060(2) 0.1873(9) 0.017 Uiso 1 1 d R . . . .
C21 C 0.47895(12) 0.02850(14) 0.24842(6) 0.0133(3) Uani 1 1 d . . . . .
C22 C 0.55304(12) 0.10657(14) 0.25222(6) 0.0127(3) Uani 1 1 d . . . . .
C23 C 0.59451(13) 0.13974(16) 0.29863(7) 0.0165(3) Uani 1 1 d . . . . .
H23 H 0.6456 0.1908 0.3018 0.020 Uiso 1 1 calc R . . . .
C24 C 0.56237(14) 0.09929(17) 0.33989(7) 0.0203(4) Uani 1 1 d . . . . .
H24 H 0.5921 0.1219 0.3709 0.024 Uiso 1 1 calc R . . . .
C25 C 0.48676(15) 0.02588(17) 0.33574(7) 0.0208(4) Uani 1 1 d . . . . .
H25 H 0.4633 -0.0005 0.3637 0.025 Uiso 1 1 calc R . . . .
C26 C 0.44588(13) -0.00842(16) 0.29033(7) 0.0169(3) Uani 1 1 d . . . . .
H26 H 0.3940 -0.0584 0.2876 0.020 Uiso 1 1 calc R . . . .
C27 C 0.35144(13) -0.02679(15) 0.10488(6) 0.0145(3) Uani 1 1 d . . . . .
C28 C 0.42038(14) -0.08481(16) 0.08401(7) 0.0185(4) Uani 1 1 d . . . . .
H28 H 0.4866 -0.0691 0.0932 0.022 Uiso 1 1 calc R . . . .
C29 C 0.39344(15) -0.16506(18) 0.05014(7) 0.0222(4) Uani 1 1 d . . . . .
H29 H 0.4410 -0.2044 0.0365 0.027 Uiso 1 1 calc R . . . .
C30 C 0.29643(16) -0.18765(18) 0.03631(8) 0.0240(4) Uani 1 1 d . . . . .
H30 H 0.2775 -0.2426 0.0132 0.029 Uiso 1 1 calc R . . . .
C31 C 0.22747(15) -0.12983(19) 0.05637(8) 0.0241(4) Uani 1 1 d . . . . .
H31 H 0.1613 -0.1451 0.0467 0.029 Uiso 1 1 calc R . . . .
C32 C 0.25406(13) -0.04972(16) 0.09046(7) 0.0184(4) Uani 1 1 d . . . . .
H32 H 0.2062 -0.0105 0.1040 0.022 Uiso 1 1 calc R . . . .
C33 C 0.28193(12) 0.12819(14) 0.16622(7) 0.0137(3) Uani 1 1 d . . . . .
C34 C 0.23446(14) 0.08863(18) 0.20290(7) 0.0206(4) Uani 1 1 d . . . . .
H34 H 0.2634 0.0334 0.2237 0.025 Uiso 1 1 calc R . . . .
C35 C 0.14452(15) 0.12963(19) 0.20932(8) 0.0248(4) Uani 1 1 d . . . . .
H35 H 0.1127 0.1028 0.2346 0.030 Uiso 1 1 calc R . . . .
C36 C 0.10167(14) 0.20926(18) 0.17888(8) 0.0233(4) Uani 1 1 d . . . . .
H36 H 0.0402 0.2365 0.1831 0.028 Uiso 1 1 calc R . . . .
C37 C 0.14820(15) 0.24945(18) 0.14212(8) 0.0250(4) Uani 1 1 d . . . . .
H37 H 0.1185 0.3037 0.1210 0.030 Uiso 1 1 calc R . . . .
C38 C 0.23821(14) 0.20998(17) 0.13629(8) 0.0214(4) Uani 1 1 d . . . . .
H38 H 0.2707 0.2389 0.1116 0.026 Uiso 1 1 calc R . . . .
C39 C 0.67016(15) 0.10729(16) 0.10907(7) 0.0191(4) Uani 1 1 d . . . . .
H39A H 0.6761(18) 0.135(2) 0.0758(9) 0.023 Uiso 1 1 d R . . . .
H39B H 0.7239(19) 0.132(2) 0.1310(9) 0.023 Uiso 1 1 d R . . . .
C40 C 0.67137(12) -0.01305(16) 0.10992(7) 0.0161(3) Uani 1 1 d . . . . .
C41 C 0.67805(13) -0.07060(17) 0.15339(7) 0.0191(4) Uani 1 1 d . . . . .
H41 H 0.6807 -0.0317 0.1828 0.023 Uiso 1 1 calc R . . . .
C42 C 0.68082(15) -0.18252(18) 0.15453(8) 0.0235(4) Uani 1 1 d . . . . .
H42 H 0.6866 -0.2193 0.1846 0.028 Uiso 1 1 calc R . . . .
C43 C 0.67520(16) -0.24137(19) 0.11206(9) 0.0281(4) Uani 1 1 d . . . . .
H43 H 0.6777 -0.3182 0.1128 0.034 Uiso 1 1 calc R . . . .
C44 C 0.66592(17) -0.18651(18) 0.06853(8) 0.0271(4) Uani 1 1 d . . . . .
H44 H 0.6608 -0.2261 0.0392 0.033 Uiso 1 1 calc R . . . .
C45 C 0.66407(14) -0.07432(17) 0.06746(7) 0.0210(4) Uani 1 1 d . . . . .
H45 H 0.6577 -0.0382 0.0373 0.025 Uiso 1 1 calc R . . . .
C46 C 0.45114(16) 0.18984(17) 0.05978(7) 0.0216(4) Uani 1 1 d . . . . .
H46A H 0.4848(19) 0.137(2) 0.0414(10) 0.026 Uiso 1 1 d R . . . .
H46B H 0.383(2) 0.175(2) 0.0544(10) 0.026 Uiso 1 1 d R . . . .
C47 C 0.47509(15) 0.30390(17) 0.05588(6) 0.0195(4) Uani 1 1 d . . . . .
C48 C 0.57109(15) 0.33759(18) 0.05446(7) 0.0215(4) Uani 1 1 d . . . . .
H48 H 0.6194 0.2849 0.0519 0.026 Uiso 1 1 calc R . . . .
C49 C 0.59578(16) 0.44733(18) 0.05673(7) 0.0246(4) Uani 1 1 d . . . . .
H49 H 0.6603 0.4682 0.0551 0.030 Uiso 1 1 calc R . . . .
C50 C 0.52789(18) 0.52538(18) 0.06132(7) 0.0269(4) Uani 1 1 d . . . . .
H50 H 0.5453 0.5997 0.0631 0.032 Uiso 1 1 calc R . . . .
C51 C 0.43299(17) 0.49408(19) 0.06328(7) 0.0260(4) Uani 1 1 d . . . . .
H51 H 0.3857 0.5476 0.0662 0.031 Uiso 1 1 calc R . . . .
C52 C 0.40728(15) 0.38643(19) 0.06098(7) 0.0233(4) Uani 1 1 d . . . . .
H52 H 0.3425 0.3670 0.0629 0.028 Uiso 1 1 calc R . . . .


_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 P1 2.8342(5) . ?
Zr P2 2.7250(5) . ?
Zr N 2.1482(15) . ?
Zr C1 2.2961(18) . ?
Zr C2 2.6398(18) . ?
Zr C3 2.6301(17) . ?
Zr C39 2.3362(19) . ?
Zr C46 2.3542(19) . ?
Zr C47 2.6565(19) . ?
P1 C1 1.7956(18) . ?
P1 C8 1.8302(18) . ?
P1 C14 1.8345(19) . ?
P2 C20 1.8343(19) . ?
P2 C27 1.8293(18) . ?
P2 C33 1.8138(18) . ?
N C3 1.424(2) . ?
N C22 1.405(2) . ?
C1 H1 0.92(2) . ?
C1 C2 1.460(2) . ?
C2 C3 1.420(3) . ?
C2 C7 1.419(3) . ?
C3 C4 1.411(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.381(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.403(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.376(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.395(3) . ?
C8 C13 1.400(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.392(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.390(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.388(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.386(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.399(2) . ?
C14 C19 1.396(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.389(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.390(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.388(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.387(3) . ?
C19 H19 0.9500 . ?
C20 H20A 0.99(2) . ?
C20 H20B 0.98(2) . ?
C20 C21 1.500(3) . ?
C21 C22 1.412(2) . ?
C21 C26 1.399(2) . ?
C22 C23 1.409(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.392(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.389(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.386(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.398(3) . ?
C27 C32 1.399(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.388(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.391(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.385(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.390(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.391(3) . ?
C33 C38 1.399(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.396(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.383(3) . ?
C36 H36 0.9500 . ?
C36 C37 1.388(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.386(3) . ?
C38 H38 0.9500 . ?
C39 H39A 1.01(3) . ?
C39 H39B 0.95(3) . ?
C39 C40 1.487(3) . ?
C40 C41 1.402(3) . ?
C40 C45 1.402(3) . ?
C41 H41 0.9500 . ?
C41 C42 1.384(3) . ?
C42 H42 0.9500 . ?
C42 C43 1.387(3) . ?
C43 H43 0.9500 . ?
C43 C44 1.385(3) . ?
C44 H44 0.9500 . ?
C44 C45 1.386(3) . ?
C45 H45 0.9500 . ?
C46 H46A 0.99(3) . ?
C46 H46B 0.96(3) . ?
C46 C47 1.456(3) . ?
C47 C48 1.417(3) . ?
C47 C52 1.416(3) . ?
C48 H48 0.9500 . ?
C48 C49 1.399(3) . ?
C49 H49 0.9500 . ?
C49 C50 1.375(3) . ?
C50 H50 0.9500 . ?
C50 C51 1.396(3) . ?
C51 H51 0.9500 . ?
C51 C52 1.377(3) . ?
C52 H52 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P2 Zr P1 86.362(14) . . ?
N Zr P1 72.49(4) . . ?
N Zr P2 77.08(4) . . ?
N Zr C1 78.62(6) . . ?
N Zr C2 59.88(6) . . ?
N Zr C3 32.75(5) . . ?
N Zr C39 95.42(6) . . ?
N Zr C46 153.60(6) . . ?
N Zr C47 164.05(6) . . ?
C1 Zr P1 39.24(4) . . ?
C1 Zr P2 125.05(4) . . ?
C1 Zr C2 33.50(6) . . ?
C1 Zr C3 60.64(6) . . ?
C1 Zr C39 116.81(7) . . ?
C1 Zr C46 120.76(7) . . ?
C1 Zr C47 88.89(6) . . ?
C2 Zr P1 64.36(4) . . ?
C2 Zr P2 132.95(4) . . ?
C2 Zr C47 113.40(6) . . ?
C3 Zr P1 76.62(4) . . ?
C3 Zr P2 109.79(4) . . ?
C3 Zr C2 31.27(6) . . ?
C3 Zr C47 144.31(6) . . ?
C39 Zr P1 153.95(5) . . ?
C39 Zr P2 113.96(5) . . ?
C39 Zr C2 89.59(6) . . ?
C39 Zr C3 80.99(6) . . ?
C39 Zr C46 91.10(8) . . ?
C39 Zr C47 99.08(7) . . ?
C46 Zr P1 110.08(6) . . ?
C46 Zr P2 76.89(5) . . ?
C46 Zr C2 145.92(6) . . ?
C46 Zr C3 171.20(7) . . ?
C46 Zr C47 33.10(6) . . ?
C47 Zr P1 91.56(5) . . ?
C47 Zr P2 102.77(4) . . ?
C1 P1 Zr 53.98(6) . . ?
C1 P1 C8 110.05(8) . . ?
C1 P1 C14 102.24(8) . . ?
C8 P1 Zr 127.04(6) . . ?
C8 P1 C14 99.56(8) . . ?
C14 P1 Zr 131.67(6) . . ?
C20 P2 Zr 106.93(6) . . ?
C27 P2 Zr 116.88(6) . . ?
C27 P2 C20 99.68(8) . . ?
C33 P2 Zr 121.46(6) . . ?
C33 P2 C20 107.20(8) . . ?
C33 P2 C27 102.30(8) . . ?
C3 N Zr 92.57(10) . . ?
C22 N Zr 148.75(12) . . ?
C22 N C3 118.19(14) . . ?
Zr C1 H1 118.4(15) . . ?
P1 C1 Zr 86.78(7) . . ?
P1 C1 H1 113.0(15) . . ?
C2 C1 Zr 86.28(11) . . ?
C2 C1 P1 127.22(14) . . ?
C2 C1 H1 116.1(15) . . ?
C1 C2 Zr 60.22(9) . . ?
C3 C2 Zr 73.99(10) . . ?
C3 C2 C1 120.72(16) . . ?
C7 C2 Zr 134.32(13) . . ?
C7 C2 C1 120.86(17) . . ?
C7 C2 C3 117.88(17) . . ?
N C3 Zr 54.68(8) . . ?
C2 C3 Zr 74.74(10) . . ?
C2 C3 N 117.17(15) . . ?
C4 C3 Zr 136.24(13) . . ?
C4 C3 N 122.36(16) . . ?
C4 C3 C2 119.75(16) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.75(18) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 H5 120.1 . . ?
C4 C5 C6 119.86(18) . . ?
C6 C5 H5 120.1 . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.30(18) . . ?
C7 C6 H6 119.8 . . ?
C2 C7 H7 119.3 . . ?
C6 C7 C2 121.40(19) . . ?
C6 C7 H7 119.3 . . ?
C9 C8 P1 118.85(14) . . ?
C9 C8 C13 119.15(17) . . ?
C13 C8 P1 121.91(14) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.20(18) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.00(18) . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 119.9 . . ?
C12 C11 C10 120.23(19) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.83(19) . . ?
C13 C12 H12 120.1 . . ?
C8 C13 H13 119.7 . . ?
C12 C13 C8 120.57(18) . . ?
C12 C13 H13 119.7 . . ?
C15 C14 P1 118.25(14) . . ?
C19 C14 P1 123.08(14) . . ?
C19 C14 C15 118.63(17) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.54(18) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.14(18) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 120.1 . . ?
C18 C17 C16 119.79(19) . . ?
C18 C17 H17 120.1 . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 120.08(18) . . ?
C19 C18 H18 120.0 . . ?
C14 C19 H19 119.6 . . ?
C18 C19 C14 120.81(17) . . ?
C18 C19 H19 119.6 . . ?
P2 C20 H20A 111.7(14) . . ?
P2 C20 H20B 101.9(14) . . ?
H20A C20 H20B 108(2) . . ?
C21 C20 P2 116.92(13) . . ?
C21 C20 H20A 107.8(14) . . ?
C21 C20 H20B 110.4(14) . . ?
C22 C21 C20 121.89(15) . . ?
C26 C21 C20 118.76(16) . . ?
C26 C21 C22 119.23(17) . . ?
N C22 C21 120.55(15) . . ?
N C22 C23 121.19(16) . . ?
C23 C22 C21 118.19(16) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 C22 121.47(18) . . ?
C24 C23 H23 119.3 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 119.92(18) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 120.4 . . ?
C26 C25 C24 119.28(17) . . ?
C26 C25 H25 120.4 . . ?
C21 C26 H26 119.1 . . ?
C25 C26 C21 121.82(18) . . ?
C25 C26 H26 119.1 . . ?
C28 C27 P2 117.98(14) . . ?
C28 C27 C32 118.84(17) . . ?
C32 C27 P2 123.12(14) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 C27 120.97(18) . . ?
C29 C28 H28 119.5 . . ?
C28 C29 H29 120.1 . . ?
C28 C29 C30 119.70(19) . . ?
C30 C29 H29 120.1 . . ?
C29 C30 H30 120.1 . . ?
C31 C30 C29 119.81(19) . . ?
C31 C30 H30 120.1 . . ?
C30 C31 H31 119.6 . . ?
C30 C31 C32 120.73(18) . . ?
C32 C31 H31 119.6 . . ?
C27 C32 H32 120.0 . . ?
C31 C32 C27 119.95(18) . . ?
C31 C32 H32 120.0 . . ?
C34 C33 P2 123.16(14) . . ?
C34 C33 C38 118.79(17) . . ?
C38 C33 P2 117.86(14) . . ?
C33 C34 H34 119.8 . . ?
C33 C34 C35 120.32(19) . . ?
C35 C34 H34 119.8 . . ?
C34 C35 H35 120.0 . . ?
C36 C35 C34 120.10(19) . . ?
C36 C35 H35 120.0 . . ?
C35 C36 H36 119.9 . . ?
C35 C36 C37 120.18(18) . . ?
C37 C36 H36 119.9 . . ?
C36 C37 H37 120.2 . . ?
C38 C37 C36 119.67(19) . . ?
C38 C37 H37 120.2 . . ?
C33 C38 H38 119.5 . . ?
C37 C38 C33 120.92(18) . . ?
C37 C38 H38 119.5 . . ?
Zr C39 H39A 107.8(15) . . ?
Zr C39 H39B 101.5(16) . . ?
H39A C39 H39B 109(2) . . ?
C40 C39 Zr 119.63(13) . . ?
C40 C39 H39A 110.4(15) . . ?
C40 C39 H39B 107.7(16) . . ?
C41 C40 C39 121.33(18) . . ?
C45 C40 C39 121.81(18) . . ?
C45 C40 C41 116.85(18) . . ?
C40 C41 H41 119.2 . . ?
C42 C41 C40 121.65(19) . . ?
C42 C41 H41 119.2 . . ?
C41 C42 H42 119.8 . . ?
C41 C42 C43 120.4(2) . . ?
C43 C42 H42 119.8 . . ?
C42 C43 H43 120.5 . . ?
C44 C43 C42 119.1(2) . . ?
C44 C43 H43 120.5 . . ?
C43 C44 H44 119.8 . . ?
C43 C44 C45 120.5(2) . . ?
C45 C44 H44 119.8 . . ?
C40 C45 H45 119.2 . . ?
C44 C45 C40 121.5(2) . . ?
C44 C45 H45 119.2 . . ?
Zr C46 H46A 105.6(15) . . ?
Zr C46 H46B 124.2(16) . . ?
H46A C46 H46B 109(2) . . ?
C47 C46 Zr 84.93(11) . . ?
C47 C46 H46A 117.6(16) . . ?
C47 C46 H46B 113.9(16) . . ?
C46 C47 Zr 61.97(10) . . ?
C48 C47 Zr 86.17(12) . . ?
C48 C47 C46 121.1(2) . . ?
C52 C47 Zr 115.39(13) . . ?
C52 C47 C46 121.53(19) . . ?
C52 C47 C48 116.60(19) . . ?
C47 C48 H48 119.5 . . ?
C49 C48 C47 120.9(2) . . ?
C49 C48 H48 119.5 . . ?
C48 C49 H49 119.6 . . ?
C50 C49 C48 120.9(2) . . ?
C50 C49 H49 119.6 . . ?
C49 C50 H50 120.4 . . ?
C49 C50 C51 119.2(2) . . ?
C51 C50 H50 120.4 . . ?
C50 C51 H51 119.6 . . ?
C52 C51 C50 120.7(2) . . ?
C52 C51 H51 119.6 . . ?
C47 C52 H52 119.2 . . ?
C51 C52 C47 121.6(2) . . ?
C51 C52 H52 119.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr P1 C1 C2 -82.85(16) . . . . ?
Zr P1 C8 C9 -96.99(15) . . . . ?
Zr P1 C8 C13 86.54(17) . . . . ?
Zr P1 C14 C15 101.73(15) . . . . ?
Zr P1 C14 C19 -80.89(17) . . . . ?
Zr P2 C20 C21 59.44(14) . . . . ?
Zr P2 C27 C28 42.99(17) . . . . ?
Zr P2 C27 C32 -139.96(14) . . . . ?
Zr P2 C33 C34 -134.44(15) . . . . ?
Zr P2 C33 C38 50.70(17) . . . . ?
Zr N C3 C2 43.43(15) . . . . ?
Zr N C3 C4 -126.79(16) . . . . ?
Zr N C22 C21 26.8(3) . . . . ?
Zr N C22 C23 -149.90(18) . . . . ?
Zr C1 C2 C3 -44.79(16) . . . . ?
Zr C1 C2 C7 126.57(16) . . . . ?
Zr C2 C3 N -35.55(13) . . . . ?
Zr C2 C3 C4 134.94(16) . . . . ?
Zr C2 C7 C6 -96.6(2) . . . . ?
Zr C3 C4 C5 96.5(2) . . . . ?
Zr C39 C40 C41 -63.3(2) . . . . ?
Zr C39 C40 C45 115.42(18) . . . . ?
Zr C46 C47 C48 65.79(18) . . . . ?
Zr C46 C47 C52 -104.08(17) . . . . ?
Zr C47 C48 C49 -118.22(18) . . . . ?
Zr C47 C52 C51 100.4(2) . . . . ?
P1 C1 C2 Zr 83.10(14) . . . . ?
P1 C1 C2 C3 38.3(2) . . . . ?
P1 C1 C2 C7 -150.34(15) . . . . ?
P1 C8 C9 C10 -175.39(15) . . . . ?
P1 C8 C13 C12 175.46(16) . . . . ?
P1 C14 C15 C16 177.48(16) . . . . ?
P1 C14 C19 C18 -178.34(15) . . . . ?
P2 C20 C21 C22 -54.8(2) . . . . ?
P2 C20 C21 C26 129.24(15) . . . . ?
P2 C27 C28 C29 176.17(16) . . . . ?
P2 C27 C32 C31 -176.31(16) . . . . ?
P2 C33 C34 C35 -174.37(16) . . . . ?
P2 C33 C38 C37 173.54(17) . . . . ?
N C3 C4 C5 167.35(17) . . . . ?
N C22 C23 C24 175.17(17) . . . . ?
C1 P1 C8 C9 -156.42(15) . . . . ?
C1 P1 C8 C13 27.12(18) . . . . ?
C1 P1 C14 C15 153.97(15) . . . . ?
C1 P1 C14 C19 -28.65(17) . . . . ?
C1 C2 C3 Zr 39.51(15) . . . . ?
C1 C2 C3 N 4.0(2) . . . . ?
C1 C2 C3 C4 174.45(16) . . . . ?
C1 C2 C7 C6 -173.60(18) . . . . ?
C2 C3 C4 C5 -2.6(3) . . . . ?
C3 N C22 C21 -164.30(16) . . . . ?
C3 N C22 C23 19.0(2) . . . . ?
C3 C2 C7 C6 -2.0(3) . . . . ?
C3 C4 C5 C6 1.5(3) . . . . ?
C4 C5 C6 C7 -0.6(3) . . . . ?
C5 C6 C7 C2 0.9(3) . . . . ?
C7 C2 C3 Zr -132.10(16) . . . . ?
C7 C2 C3 N -167.65(16) . . . . ?
C7 C2 C3 C4 2.8(3) . . . . ?
C8 P1 C1 Zr 121.83(7) . . . . ?
C8 P1 C1 C2 38.97(18) . . . . ?
C8 P1 C14 C15 -92.93(15) . . . . ?
C8 P1 C14 C19 84.45(16) . . . . ?
C8 C9 C10 C11 -0.2(3) . . . . ?
C9 C8 C13 C12 -1.0(3) . . . . ?
C9 C10 C11 C12 -1.0(3) . . . . ?
C10 C11 C12 C13 1.2(3) . . . . ?
C11 C12 C13 C8 -0.2(3) . . . . ?
C13 C8 C9 C10 1.2(3) . . . . ?
C14 P1 C1 Zr -133.10(7) . . . . ?
C14 P1 C1 C2 144.04(16) . . . . ?
C14 P1 C8 C9 96.70(16) . . . . ?
C14 P1 C8 C13 -79.76(17) . . . . ?
C14 C15 C16 C17 1.2(3) . . . . ?
C15 C14 C19 C18 -1.0(3) . . . . ?
C15 C16 C17 C18 -1.4(3) . . . . ?
C16 C17 C18 C19 0.4(3) . . . . ?
C17 C18 C19 C14 0.8(3) . . . . ?
C19 C14 C15 C16 0.0(3) . . . . ?
C20 P2 C27 C28 -71.70(16) . . . . ?
C20 P2 C27 C32 105.35(17) . . . . ?
C20 P2 C33 C34 -11.30(19) . . . . ?
C20 P2 C33 C38 173.85(15) . . . . ?
C20 C21 C22 N 10.8(3) . . . . ?
C20 C21 C22 C23 -172.48(16) . . . . ?
C20 C21 C26 C25 173.17(17) . . . . ?
C21 C22 C23 C24 -1.6(3) . . . . ?
C22 N C3 Zr -174.28(17) . . . . ?
C22 N C3 C2 -130.85(17) . . . . ?
C22 N C3 C4 58.9(2) . . . . ?
C22 C21 C26 C25 -2.9(3) . . . . ?
C22 C23 C24 C25 -1.1(3) . . . . ?
C23 C24 C25 C26 1.7(3) . . . . ?
C24 C25 C26 C21 0.3(3) . . . . ?
C26 C21 C22 N -173.26(16) . . . . ?
C26 C21 C22 C23 3.5(3) . . . . ?
C27 P2 C20 C21 -178.47(13) . . . . ?
C27 P2 C33 C34 93.04(17) . . . . ?
C27 P2 C33 C38 -81.82(16) . . . . ?
C27 C28 C29 C30 0.6(3) . . . . ?
C28 C27 C32 C31 0.7(3) . . . . ?
C28 C29 C30 C31 0.1(3) . . . . ?
C29 C30 C31 C32 -0.4(3) . . . . ?
C30 C31 C32 C27 0.0(3) . . . . ?
C32 C27 C28 C29 -1.0(3) . . . . ?
C33 P2 C20 C21 -72.27(15) . . . . ?
C33 P2 C27 C28 178.17(15) . . . . ?
C33 P2 C27 C32 -4.78(18) . . . . ?
C33 C34 C35 C36 0.6(3) . . . . ?
C34 C33 C38 C37 -1.5(3) . . . . ?
C34 C35 C36 C37 -0.6(3) . . . . ?
C35 C36 C37 C38 -0.5(3) . . . . ?
C36 C37 C38 C33 1.6(3) . . . . ?
C38 C33 C34 C35 0.4(3) . . . . ?
C39 C40 C41 C42 -178.91(19) . . . . ?
C39 C40 C45 C44 179.55(19) . . . . ?
C40 C41 C42 C43 -1.2(3) . . . . ?
C41 C40 C45 C44 -1.7(3) . . . . ?
C41 C42 C43 C44 -0.6(3) . . . . ?
C42 C43 C44 C45 1.2(3) . . . . ?
C43 C44 C45 C40 0.0(3) . . . . ?
C45 C40 C41 C42 2.3(3) . . . . ?
C46 C47 C48 C49 -172.01(18) . . . . ?
C46 C47 C52 C51 171.82(19) . . . . ?
C47 C48 C49 C50 1.3(3) . . . . ?
C48 C47 C52 C51 1.5(3) . . . . ?
C48 C49 C50 C51 -0.6(3) . . . . ?
C49 C50 C51 C52 0.4(3) . . . . ?
C50 C51 C52 C47 -0.9(3) . . . . ?
C52 C47 C48 C49 -1.7(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.184
_oxdiff_exptl_absorpt_empirical_full_min 0.788
_cell_oxdiff_length_a            14.05010(18)
_cell_oxdiff_length_b            12.35356(14)
_cell_oxdiff_length_c            28.0193(4)
_cell_oxdiff_angle_alpha         89.9704(10)
_cell_oxdiff_angle_beta          98.1485(11)
_cell_oxdiff_angle_gamma         90.0007(10)
_cell_oxdiff_volume              4814.18(11)
_cell_oxdiff_measurement_reflns_used 43081
_diffrn_measurement_specimen_support 'polyimid foil'

# SQUEEZE RESULTS (Version = 120716)
# Ref.: P. v. d. Sluis, A. L. Spek,  Acta Cryst. 1990, A46, 194.
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 -0.000 -0.014 -0.000 518 147 'disordered ether or toluene'
2 0.500 -0.019 0.500 518 147 'disordered ether or toluene'
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
