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

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

data_PNP2ZrCl2
_database_code_depnum_ccdc_archive 'CCDC 2023865'
loop_
_audit_author_name
_audit_author_address
'F. Mark Chadwick'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2020-08-18 deposited with the CCDC.	2020-11-10 downloaded from the CCDC.
;
_oxford_structure_analysis_title 'lve\FMC2002\FMC2002.cif_od At 11:37 on 20/ 1'
_chemical_name_systematic        .
_chemical_melting_point          'not measured'


_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
_cell_length_a                   11.1053(7)
_cell_length_b                   13.1355(8)
_cell_length_c                   20.3905(10)
_cell_angle_alpha                85.224(4)
_cell_angle_beta                 86.838(4)
_cell_angle_gamma                66.436(6)
_cell_volume                     2716.2(3)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Zr -0.1862 2.2449 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627
2.0693 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C60 H48 Cl2 N2 P4 Zr1 
# Dc =      1.32 Fooo =   1112.00 Mu =     39.81 M =   1083.08
# Found Formula = C60 H52 Cl2 N2 P4 Zr1 
# Dc =      1.33 FOOO =   1120.00 Mu =     39.82 M =   1087.11

_chemical_formula_sum            'C60 H52 Cl2 N2 P4 Zr1'
_chemical_formula_moiety         'C60 H52 Cl2 N2 P4 Zr1'
_chemical_compound_source        .
_chemical_formula_weight         1087.11


_cell_measurement_reflns_used    6386
_cell_measurement_theta_min      4
_cell_measurement_theta_max      73
_cell_measurement_temperature    173

_exptl_crystal_description       shard
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1120
_exptl_absorpt_coefficient_mu    3.982

# Sheldrick geometric approximatio 0.45 0.67 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_T_max  0.67
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_reduction        
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      173
_diffrn_reflns_number            15595
_diffrn_reflns_av_unetI/netI     0.068
_reflns_number_total             10361
_diffrn_reflns_av_R_equivalents  0.039
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 10361 
# Theoretical number of reflections is about 21866 


_diffrn_reflns_theta_min         3.679
_diffrn_reflns_theta_max         73.426
_diffrn_measured_fraction_theta_max 0.947

_diffrn_reflns_theta_full        43.321
_diffrn_measured_fraction_theta_full 0.994


_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              -16
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              25

_oxford_diffrn_Wilson_B_factor   2.29
_oxford_diffrn_Wilson_scale      0.24

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

_refine_diff_density_min         -0.78
_refine_diff_density_max         0.58


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


# The values actually used during refinement 
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_restraints     0
_refine_ls_number_parameters     622
_refine_ls_number_reflns         10316
_oxford_refine_ls_R_factor_ref   0.0562
_refine_ls_wR_factor_ref         0.1274
_refine_ls_goodness_of_fit_ref   1.6170
_refine_ls_shift/su_max          0.0010450
_refine_ls_shift/su_mean         0.0000239


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        10316
_refine_ls_R_factor_all          0.0562
_refine_ls_wR_factor_all         0.1274

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8347
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_gt          0.1134


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 650. 0.101E+04 578. 210. 33.1 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C -0.2059(4) 0.7613(3) 0.2784(2) 0.0322 1.0000 Uani . . . . . .
C2 C -0.3233(4) 0.7769(4) 0.3097(2) 0.0375 1.0000 Uani . . . . . .
C3 C -0.2986(4) 0.6975(4) 0.3637(2) 0.0390 1.0000 Uani . . . . . .
C4 C -0.1659(4) 0.6368(3) 0.3645(2) 0.0337 1.0000 Uani . . . . . .
C5 C -0.1732(4) 0.8263(4) 0.2238(2) 0.0351 1.0000 Uani . . . . . .
C6 C -0.0861(4) 0.5407(4) 0.4091(2) 0.0369 1.0000 Uani . . . . . .
C7 C 0.0272(4) 0.9072(3) 0.1772(2) 0.0318 1.0000 Uani . . . . . .
C8 C 0.1204(5) 0.8452(4) 0.1320(2) 0.0427 1.0000 Uani . . . . . .
C9 C 0.1612(6) 0.8956(4) 0.0784(2) 0.0525 1.0000 Uani . . . . . .
C10 C 0.1091(7) 1.0108(5) 0.0687(3) 0.0631 1.0000 Uani . . . . . .
C11 C 0.0166(7) 1.0720(5) 0.1124(3) 0.0675 1.0000 Uani . . . . . .
C12 C -0.0261(6) 1.0229(4) 0.1653(2) 0.0481 1.0000 Uani . . . . . .
C13 C -0.0790(4) 0.9364(3) 0.3120(2) 0.0331 1.0000 Uani . . . . . .
C14 C 0.0124(4) 0.9408(4) 0.3548(2) 0.0393 1.0000 Uani . . . . . .
C15 C -0.0253(5) 1.0116(4) 0.4052(2) 0.0452 1.0000 Uani . . . . . .
C16 C -0.1562(5) 1.0792(4) 0.4148(2) 0.0489 1.0000 Uani . . . . . .
C17 C -0.2476(5) 1.0754(4) 0.3730(3) 0.0559 1.0000 Uani . . . . . .
C18 C -0.2108(4) 1.0057(4) 0.3218(3) 0.0445 1.0000 Uani . . . . . .
C19 C -0.0394(4) 0.3845(3) 0.3101(2) 0.0321 1.0000 Uani . . . . . .
C20 C -0.1448(4) 0.4525(4) 0.2693(2) 0.0352 1.0000 Uani . . . . . .
C21 C -0.2060(4) 0.4042(4) 0.2330(2) 0.0398 1.0000 Uani . . . . . .
C22 C -0.1637(5) 0.2898(4) 0.2343(3) 0.0480 1.0000 Uani . . . . . .
C23 C -0.0584(5) 0.2234(4) 0.2722(3) 0.0494 1.0000 Uani . . . . . .
C24 C 0.0027(5) 0.2703(4) 0.3097(2) 0.0431 1.0000 Uani . . . . . .
C25 C 0.1480(4) 0.3366(4) 0.4134(2) 0.0346 1.0000 Uani . . . . . .
C26 C 0.0923(5) 0.2815(4) 0.4599(2) 0.0456 1.0000 Uani . . . . . .
C27 C 0.1691(5) 0.1977(4) 0.5028(3) 0.0496 1.0000 Uani . . . . . .
C28 C 0.3038(5) 0.1665(4) 0.5009(3) 0.0497 1.0000 Uani . . . . . .
C29 C 0.3602(5) 0.2202(4) 0.4560(2) 0.0477 1.0000 Uani . . . . . .
C30 C 0.2837(4) 0.3051(4) 0.4120(2) 0.0396 1.0000 Uani . . . . . .
C31 C 0.4215(4) 0.4501(3) 0.2968(2) 0.0312 1.0000 Uani . . . . . .
C32 C 0.5135(4) 0.3450(4) 0.2906(2) 0.0396 1.0000 Uani . . . . . .
C33 C 0.4549(5) 0.2847(4) 0.2609(2) 0.0414 1.0000 Uani . . . . . .
C34 C 0.3267(4) 0.3562(3) 0.2479(2) 0.0320 1.0000 Uani . . . . . .
C35 C 0.4372(4) 0.5498(4) 0.3185(2) 0.0352 1.0000 Uani . . . . . .
C36 C 0.2346(4) 0.3314(4) 0.2072(2) 0.0368 1.0000 Uani . . . . . .
C37 C 0.4266(4) 0.6487(3) 0.1886(2) 0.0324 1.0000 Uani . . . . . .
C38 C 0.4006(5) 0.5915(4) 0.1401(2) 0.0436 1.0000 Uani . . . . . .
C39 C 0.4721(6) 0.5743(5) 0.0814(3) 0.0539 1.0000 Uani . . . . . .
C40 C 0.5723(5) 0.6117(4) 0.0703(3) 0.0519 1.0000 Uani . . . . . .
C41 C 0.6009(5) 0.6659(4) 0.1189(2) 0.0482 1.0000 Uani . . . . . .
C42 C 0.5291(4) 0.6847(4) 0.1771(2) 0.0384 1.0000 Uani . . . . . .
C43 C 0.3384(4) 0.7933(3) 0.2964(2) 0.0319 1.0000 Uani . . . . . .
C44 C 0.3106(4) 0.8899(4) 0.2546(2) 0.0388 1.0000 Uani . . . . . .
C45 C 0.3048(5) 0.9877(4) 0.2788(3) 0.0446 1.0000 Uani . . . . . .
C46 C 0.3253(5) 0.9907(4) 0.3448(3) 0.0464 1.0000 Uani . . . . . .
C47 C 0.3525(4) 0.8966(4) 0.3862(3) 0.0466 1.0000 Uani . . . . . .
C48 C 0.3599(4) 0.7978(4) 0.3629(2) 0.0379 1.0000 Uani . . . . . .
C49 C 0.4127(5) 0.2088(5) 0.1077(2) 0.0562 1.0000 Uani . . . . . .
C50 C 0.5378(6) 0.2036(7) 0.0943(3) 0.0792 1.0000 Uani . . . . . .
C51 C 0.6430(7) 0.1001(10) 0.0851(4) 0.1080 1.0000 Uani . . . . . .
C52 C 0.6159(10) 0.0054(9) 0.0898(4) 0.1162 1.0000 Uani . . . . . .
C53 C 0.4938(9) 0.0075(6) 0.1039(4) 0.1018 1.0000 Uani . . . . . .
C54 C 0.3932(7) 0.1104(5) 0.1123(3) 0.0687 1.0000 Uani . . . . . .
C55 C 0.1461(5) 0.3328(4) 0.0750(2) 0.0372 1.0000 Uani . . . . . .
C56 C 0.1700(5) 0.2818(4) 0.0163(2) 0.0482 1.0000 Uani . . . . . .
C57 C 0.0682(6) 0.2829(5) -0.0205(2) 0.0544 1.0000 Uani . . . . . .
C58 C -0.0601(6) 0.3370(5) 0.0003(3) 0.0568 1.0000 Uani . . . . . .
C59 C -0.0855(5) 0.3865(5) 0.0591(3) 0.0519 1.0000 Uani . . . . . .
C60 C 0.0155(5) 0.3862(4) 0.0957(3) 0.0478 1.0000 Uani . . . . . .
N1 N -0.1040(3) 0.6741(3) 0.31216(16) 0.0293 1.0000 Uani . . . . . .
N2 N 0.3024(3) 0.4596(3) 0.27089(17) 0.0306 1.0000 Uani . . . . . .
P1 P -0.02206(10) 0.83752(8) 0.24790(5) 0.0293 1.0000 Uani . . . . . .
P2 P 0.04457(10) 0.44811(8) 0.35720(5) 0.0302 1.0000 Uani . . . . . .
P3 P 0.33251(10) 0.66886(8) 0.26586(5) 0.0280 1.0000 Uani . . . . . .
P4 P 0.27968(12) 0.34753(10) 0.11756(6) 0.0393 1.0000 Uani . . . . . .
Cl1 Cl 0.06339(10) 0.60113(9) 0.17406(5) 0.0372 1.0000 Uani . . . . . .
Cl2 Cl 0.14912(10) 0.65159(9) 0.39683(5) 0.0342 1.0000 Uani . . . . . .
Zr1 Zr 0.11328(3) 0.60966(3) 0.286967(16) 0.0260 1.0000 Uani . . . . . .
H21 H -0.4057 0.8313 0.2970 0.0450 1.0000 Uiso R . . . . .
H31 H -0.3619 0.6885 0.3935 0.0466 1.0000 Uiso R . . . . .
H51 H -0.2436 0.9003 0.2162 0.0430 1.0000 Uiso R . . . . .
H52 H -0.1564 0.7903 0.1820 0.0433 1.0000 Uiso R . . . . .
H62 H -0.0484 0.5649 0.4444 0.0447 1.0000 Uiso R . . . . .
H61 H -0.1399 0.5036 0.4297 0.0451 1.0000 Uiso R . . . . .
H81 H 0.1554 0.7664 0.1384 0.0511 1.0000 Uiso R . . . . .
H91 H 0.2267 0.8516 0.0481 0.0634 1.0000 Uiso R . . . . .
H101 H 0.1385 1.0467 0.0328 0.0739 1.0000 Uiso R . . . . .
H111 H -0.0187 1.1512 0.1051 0.0812 1.0000 Uiso R . . . . .
H121 H -0.0929 1.0666 0.1947 0.0596 1.0000 Uiso R . . . . .
H141 H 0.1023 0.8933 0.3492 0.0484 1.0000 Uiso R . . . . .
H151 H 0.0391 1.0146 0.4338 0.0542 1.0000 Uiso R . . . . .
H161 H -0.1829 1.1286 0.4496 0.0582 1.0000 Uiso R . . . . .
H171 H -0.3371 1.1214 0.3794 0.0682 1.0000 Uiso R . . . . .
H181 H -0.2748 1.0054 0.2926 0.0531 1.0000 Uiso R . . . . .
H201 H -0.1724 0.5310 0.2677 0.0426 1.0000 Uiso R . . . . .
H211 H -0.2776 0.4509 0.2063 0.0485 1.0000 Uiso R . . . . .
H221 H -0.2066 0.2574 0.2086 0.0590 1.0000 Uiso R . . . . .
H231 H -0.0299 0.1450 0.2725 0.0588 1.0000 Uiso R . . . . .
H241 H 0.0736 0.2236 0.3363 0.0539 1.0000 Uiso R . . . . .
H261 H -0.0005 0.3031 0.4617 0.0560 1.0000 Uiso R . . . . .
H271 H 0.1291 0.1607 0.5338 0.0604 1.0000 Uiso R . . . . .
H281 H 0.3581 0.1090 0.5301 0.0599 1.0000 Uiso R . . . . .
H291 H 0.4530 0.1970 0.4547 0.0572 1.0000 Uiso R . . . . .
H301 H 0.3235 0.3425 0.3809 0.0470 1.0000 Uiso R . . . . .
H321 H 0.6020 0.3176 0.3039 0.0484 1.0000 Uiso R . . . . .
H331 H 0.4941 0.2088 0.2512 0.0501 1.0000 Uiso R . . . . .
H351 H 0.5291 0.5414 0.3123 0.0430 1.0000 Uiso R . . . . .
H352 H 0.4095 0.5642 0.3641 0.0429 1.0000 Uiso R . . . . .
H362 H 0.1435 0.3828 0.2160 0.0449 1.0000 Uiso R . . . . .
H361 H 0.2408 0.2548 0.2176 0.0453 1.0000 Uiso R . . . . .
H381 H 0.3324 0.5641 0.1477 0.0539 1.0000 Uiso R . . . . .
H391 H 0.4526 0.5357 0.0485 0.0650 1.0000 Uiso R . . . . .
H401 H 0.6199 0.6007 0.0300 0.0620 1.0000 Uiso R . . . . .
H411 H 0.6698 0.6912 0.1111 0.0574 1.0000 Uiso R . . . . .
H421 H 0.5494 0.7232 0.2103 0.0485 1.0000 Uiso R . . . . .
H441 H 0.2967 0.8869 0.2096 0.0481 1.0000 Uiso R . . . . .
H451 H 0.2882 1.0521 0.2495 0.0539 1.0000 Uiso R . . . . .
H461 H 0.3211 1.0576 0.3623 0.0549 1.0000 Uiso R . . . . .
H471 H 0.3663 0.8995 0.4314 0.0567 1.0000 Uiso R . . . . .
H481 H 0.3791 0.7323 0.3921 0.0473 1.0000 Uiso R . . . . .
H501 H 0.5533 0.2733 0.0908 0.0990 1.0000 Uiso R . . . . .
H511 H 0.7307 0.0958 0.0772 0.1270 1.0000 Uiso R . . . . .
H521 H 0.6856 -0.0638 0.0823 0.1352 1.0000 Uiso R . . . . .
H531 H 0.4774 -0.0607 0.1078 0.1254 1.0000 Uiso R . . . . .
H541 H 0.3039 0.1145 0.1220 0.0883 1.0000 Uiso R . . . . .
H561 H 0.2593 0.2453 0.0006 0.0590 1.0000 Uiso R . . . . .
H571 H 0.0871 0.2471 -0.0604 0.0664 1.0000 Uiso R . . . . .
H581 H -0.1309 0.3405 -0.0258 0.0690 1.0000 Uiso R . . . . .
H591 H -0.1732 0.4197 0.0759 0.0624 1.0000 Uiso R . . . . .
H601 H -0.0037 0.4238 0.1351 0.0571 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.074(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C2 . 1.366(6) yes
C1 . C5 . 1.465(6) yes
C1 . N1 . 1.409(5) yes
C2 . C3 . 1.411(6) yes
C2 . H21 . 0.942 no
C3 . C4 . 1.367(6) yes
C3 . H31 . 0.941 no
C4 . C6 . 1.486(6) yes
C4 . N1 . 1.398(5) yes
C5 . P1 . 1.839(4) yes
C5 . H51 . 0.981 no
C5 . H52 . 0.982 no
C6 . P2 . 1.828(4) yes
C6 . H62 . 0.985 no
C6 . H61 . 0.971 no
C7 . C8 . 1.388(6) yes
C7 . C12 . 1.398(6) yes
C7 . P1 . 1.819(4) yes
C8 . C9 . 1.380(6) yes
C8 . H81 . 0.949 no
C9 . C10 . 1.387(8) yes
C9 . H91 . 0.958 no
C10 . C11 . 1.362(8) yes
C10 . H101 . 0.951 no
C11 . C12 . 1.369(7) yes
C11 . H111 . 0.955 no
C12 . H121 . 0.953 no
C13 . C14 . 1.396(6) yes
C13 . C18 . 1.394(6) yes
C13 . P1 . 1.825(5) yes
C14 . C15 . 1.377(7) yes
C14 . H141 . 0.949 no
C15 . C16 . 1.381(7) yes
C15 . H151 . 0.962 no
C16 . C17 . 1.379(8) yes
C16 . H161 . 0.954 no
C17 . C18 . 1.383(7) yes
C17 . H171 . 0.943 no
C18 . H181 . 0.953 no
C19 . C20 . 1.417(6) yes
C19 . C24 . 1.382(6) yes
C19 . P2 . 1.829(5) yes
C20 . C21 . 1.375(6) yes
C20 . H201 . 0.949 no
C21 . C22 . 1.382(7) yes
C21 . H211 . 0.953 no
C22 . C23 . 1.378(7) yes
C22 . H221 . 0.953 no
C23 . C24 . 1.376(7) yes
C23 . H231 . 0.948 no
C24 . H241 . 0.947 no
C25 . C26 . 1.410(6) yes
C25 . C30 . 1.394(6) yes
C25 . P2 . 1.816(4) yes
C26 . C27 . 1.369(7) yes
C26 . H261 . 0.952 no
C27 . C28 . 1.383(7) yes
C27 . H271 . 0.961 no
C28 . C29 . 1.382(7) yes
C28 . H281 . 0.944 no
C29 . C30 . 1.389(6) yes
C29 . H291 . 0.950 no
C30 . H301 . 0.963 no
C31 . C32 . 1.361(6) yes
C31 . C35 . 1.494(6) yes
C31 . N2 . 1.407(5) yes
C32 . C33 . 1.399(7) yes
C32 . H321 . 0.948 no
C33 . C34 . 1.381(6) yes
C33 . H331 . 0.948 no
C34 . C36 . 1.499(6) yes
C34 . N2 . 1.391(5) yes
C35 . P3 . 1.831(4) yes
C35 . H351 . 0.984 no
C35 . H352 . 0.974 no
C36 . P4 . 1.886(4) yes
C36 . H362 . 0.983 no
C36 . H361 . 0.986 no
C37 . C38 . 1.398(6) yes
C37 . C42 . 1.399(6) yes
C37 . P3 . 1.819(4) yes
C38 . C39 . 1.382(7) yes
C38 . H381 . 0.961 no
C39 . C40 . 1.386(8) yes
C39 . H391 . 0.957 no
C40 . C41 . 1.386(8) yes
C40 . H401 . 0.942 no
C41 . C42 . 1.376(6) yes
C41 . H411 . 0.949 no
C42 . H421 . 0.965 no
C43 . C44 . 1.404(6) yes
C43 . C48 . 1.400(6) yes
C43 . P3 . 1.823(4) yes
C44 . C45 . 1.391(6) yes
C44 . H441 . 0.946 no
C45 . C46 . 1.384(7) yes
C45 . H451 . 0.955 no
C46 . C47 . 1.374(7) yes
C46 . H461 . 0.958 no
C47 . C48 . 1.389(7) yes
C47 . H471 . 0.949 no
C48 . H481 . 0.959 no
C49 . C50 . 1.377(8) yes
C49 . C54 . 1.389(9) yes
C49 . P4 . 1.850(6) yes
C50 . C51 . 1.413(11) yes
C50 . H501 . 0.994 no
C51 . C52 . 1.386(14) yes
C51 . H511 . 0.959 no
C52 . C53 . 1.361(14) yes
C52 . H521 . 0.947 no
C53 . C54 . 1.384(8) yes
C53 . H531 . 0.979 no
C54 . H541 . 0.980 no
C55 . C56 . 1.382(7) yes
C55 . C60 . 1.392(7) yes
C55 . P4 . 1.841(5) yes
C56 . C57 . 1.385(8) yes
C56 . H561 . 0.962 no
C57 . C58 . 1.374(8) yes
C57 . H571 . 0.946 no
C58 . C59 . 1.373(8) yes
C58 . H581 . 0.957 no
C59 . C60 . 1.380(7) yes
C59 . H591 . 0.950 no
C60 . H601 . 0.948 no
N1 . Zr1 . 2.260(3) yes
N2 . Zr1 . 2.264(3) yes
P1 . Zr1 . 2.8267(10) yes
P2 . Zr1 . 2.7935(10) yes
P3 . Zr1 . 2.8390(11) yes
Cl1 . Zr1 . 2.4193(11) yes
Cl2 . Zr1 . 2.4412(10) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . C5 . 130.7(4) yes
C2 . C1 . N1 . 109.4(4) yes
C5 . C1 . N1 . 119.4(4) yes
C1 . C2 . C3 . 107.9(4) yes
C1 . C2 . H21 . 125.5 no
C3 . C2 . H21 . 126.6 no
C2 . C3 . C4 . 107.1(4) yes
C2 . C3 . H31 . 126.2 no
C4 . C3 . H31 . 126.7 no
C3 . C4 . C6 . 130.3(4) yes
C3 . C4 . N1 . 110.2(4) yes
C6 . C4 . N1 . 119.5(4) yes
C1 . C5 . P1 . 105.3(3) yes
C1 . C5 . H51 . 111.9 no
P1 . C5 . H51 . 110.6 no
C1 . C5 . H52 . 113.0 no
P1 . C5 . H52 . 108.9 no
H51 . C5 . H52 . 107.0 no
C4 . C6 . P2 . 105.7(3) yes
C4 . C6 . H62 . 111.3 no
P2 . C6 . H62 . 110.4 no
C4 . C6 . H61 . 110.5 no
P2 . C6 . H61 . 111.2 no
H62 . C6 . H61 . 107.8 no
C8 . C7 . C12 . 117.3(4) yes
C8 . C7 . P1 . 120.1(3) yes
C12 . C7 . P1 . 122.6(4) yes
C7 . C8 . C9 . 121.5(5) yes
C7 . C8 . H81 . 118.5 no
C9 . C8 . H81 . 120.0 no
C8 . C9 . C10 . 120.1(5) yes
C8 . C9 . H91 . 120.4 no
C10 . C9 . H91 . 119.6 no
C9 . C10 . C11 . 118.8(5) yes
C9 . C10 . H101 . 121.0 no
C11 . C10 . H101 . 120.3 no
C10 . C11 . C12 . 121.7(5) yes
C10 . C11 . H111 . 118.0 no
C12 . C11 . H111 . 120.3 no
C7 . C12 . C11 . 120.7(5) yes
C7 . C12 . H121 . 118.4 no
C11 . C12 . H121 . 120.9 no
C14 . C13 . C18 . 118.1(4) yes
C14 . C13 . P1 . 118.8(3) yes
C18 . C13 . P1 . 123.0(4) yes
C13 . C14 . C15 . 121.4(4) yes
C13 . C14 . H141 . 119.0 no
C15 . C14 . H141 . 119.5 no
C14 . C15 . C16 . 120.0(5) yes
C14 . C15 . H151 . 120.5 no
C16 . C15 . H151 . 119.5 no
C15 . C16 . C17 . 119.1(5) yes
C15 . C16 . H161 . 120.4 no
C17 . C16 . H161 . 120.5 no
C16 . C17 . C18 . 121.4(5) yes
C16 . C17 . H171 . 119.5 no
C18 . C17 . H171 . 119.1 no
C13 . C18 . C17 . 119.9(5) yes
C13 . C18 . H181 . 119.7 no
C17 . C18 . H181 . 120.4 no
C20 . C19 . C24 . 118.3(4) yes
C20 . C19 . P2 . 119.9(3) yes
C24 . C19 . P2 . 121.6(3) yes
C19 . C20 . C21 . 119.7(4) yes
C19 . C20 . H201 . 119.3 no
C21 . C20 . H201 . 121.0 no
C20 . C21 . C22 . 121.0(4) yes
C20 . C21 . H211 . 118.9 no
C22 . C21 . H211 . 120.1 no
C21 . C22 . C23 . 119.4(5) yes
C21 . C22 . H221 . 120.0 no
C23 . C22 . H221 . 120.6 no
C22 . C23 . C24 . 120.5(5) yes
C22 . C23 . H231 . 118.8 no
C24 . C23 . H231 . 120.8 no
C19 . C24 . C23 . 121.1(5) yes
C19 . C24 . H241 . 119.5 no
C23 . C24 . H241 . 119.4 no
C26 . C25 . C30 . 118.7(4) yes
C26 . C25 . P2 . 120.6(3) yes
C30 . C25 . P2 . 120.6(3) yes
C25 . C26 . C27 . 121.2(5) yes
C25 . C26 . H261 . 119.3 no
C27 . C26 . H261 . 119.5 no
C26 . C27 . C28 . 119.7(5) yes
C26 . C27 . H271 . 119.8 no
C28 . C27 . H271 . 120.5 no
C27 . C28 . C29 . 120.0(5) yes
C27 . C28 . H281 . 120.7 no
C29 . C28 . H281 . 119.3 no
C28 . C29 . C30 . 121.0(5) yes
C28 . C29 . H291 . 119.0 no
C30 . C29 . H291 . 119.9 no
C25 . C30 . C29 . 119.3(4) yes
C25 . C30 . H301 . 120.0 no
C29 . C30 . H301 . 120.7 no
C32 . C31 . C35 . 129.3(4) yes
C32 . C31 . N2 . 109.5(4) yes
C35 . C31 . N2 . 120.8(3) yes
C31 . C32 . C33 . 108.0(4) yes
C31 . C32 . H321 . 126.0 no
C33 . C32 . H321 . 126.0 no
C32 . C33 . C34 . 107.3(4) yes
C32 . C33 . H331 . 127.3 no
C34 . C33 . H331 . 125.4 no
C33 . C34 . C36 . 125.2(4) yes
C33 . C34 . N2 . 109.4(4) yes
C36 . C34 . N2 . 125.0(4) yes
C31 . C35 . P3 . 106.4(3) yes
C31 . C35 . H351 . 110.3 no
P3 . C35 . H351 . 109.3 no
C31 . C35 . H352 . 113.0 no
P3 . C35 . H352 . 108.4 no
H351 . C35 . H352 . 109.3 no
C34 . C36 . P4 . 108.6(3) yes
C34 . C36 . H362 . 110.1 no
P4 . C36 . H362 . 110.0 no
C34 . C36 . H361 . 111.1 no
P4 . C36 . H361 . 109.0 no
H362 . C36 . H361 . 108.0 no
C38 . C37 . C42 . 118.4(4) yes
C38 . C37 . P3 . 119.7(3) yes
C42 . C37 . P3 . 121.8(3) yes
C37 . C38 . C39 . 120.5(5) yes
C37 . C38 . H381 . 119.6 no
C39 . C38 . H381 . 119.9 no
C38 . C39 . C40 . 120.4(5) yes
C38 . C39 . H391 . 119.6 no
C40 . C39 . H391 . 120.0 no
C39 . C40 . C41 . 119.4(4) yes
C39 . C40 . H401 . 120.1 no
C41 . C40 . H401 . 120.5 no
C40 . C41 . C42 . 120.5(5) yes
C40 . C41 . H411 . 119.1 no
C42 . C41 . H411 . 120.3 no
C37 . C42 . C41 . 120.7(5) yes
C37 . C42 . H421 . 119.5 no
C41 . C42 . H421 . 119.8 no
C44 . C43 . C48 . 118.5(4) yes
C44 . C43 . P3 . 120.3(3) yes
C48 . C43 . P3 . 121.0(3) yes
C43 . C44 . C45 . 120.6(4) yes
C43 . C44 . H441 . 118.6 no
C45 . C44 . H441 . 120.8 no
C44 . C45 . C46 . 120.1(5) yes
C44 . C45 . H451 . 119.6 no
C46 . C45 . H451 . 120.3 no
C45 . C46 . C47 . 119.8(5) yes
C45 . C46 . H461 . 121.1 no
C47 . C46 . H461 . 119.1 no
C46 . C47 . C48 . 121.1(5) yes
C46 . C47 . H471 . 119.2 no
C48 . C47 . H471 . 119.7 no
C43 . C48 . C47 . 119.9(5) yes
C43 . C48 . H481 . 119.4 no
C47 . C48 . H481 . 120.7 no
C50 . C49 . C54 . 118.5(6) yes
C50 . C49 . P4 . 117.7(6) yes
C54 . C49 . P4 . 123.8(4) yes
C49 . C50 . C51 . 120.2(9) yes
C49 . C50 . H501 . 119.4 no
C51 . C50 . H501 . 120.4 no
C50 . C51 . C52 . 118.1(8) yes
C50 . C51 . H511 . 120.5 no
C52 . C51 . H511 . 121.4 no
C51 . C52 . C53 . 123.1(8) yes
C51 . C52 . H521 . 118.3 no
C53 . C52 . H521 . 118.6 no
C52 . C53 . C54 . 117.2(9) yes
C52 . C53 . H531 . 121.6 no
C54 . C53 . H531 . 121.2 no
C49 . C54 . C53 . 122.9(8) yes
C49 . C54 . H541 . 118.2 no
C53 . C54 . H541 . 118.9 no
C56 . C55 . C60 . 117.5(5) yes
C56 . C55 . P4 . 120.8(4) yes
C60 . C55 . P4 . 121.1(4) yes
C55 . C56 . C57 . 121.4(5) yes
C55 . C56 . H561 . 119.1 no
C57 . C56 . H561 . 119.5 no
C56 . C57 . C58 . 120.3(5) yes
C56 . C57 . H571 . 119.8 no
C58 . C57 . H571 . 119.9 no
C57 . C58 . C59 . 119.0(5) yes
C57 . C58 . H581 . 120.7 no
C59 . C58 . H581 . 120.3 no
C58 . C59 . C60 . 120.8(5) yes
C58 . C59 . H591 . 120.3 no
C60 . C59 . H591 . 118.9 no
C55 . C60 . C59 . 121.0(5) yes
C55 . C60 . H601 . 119.2 no
C59 . C60 . H601 . 119.9 no
C1 . N1 . C4 . 105.4(3) yes
C1 . N1 . Zr1 . 127.0(3) yes
C4 . N1 . Zr1 . 127.6(3) yes
C31 . N2 . C34 . 105.8(3) yes
C31 . N2 . Zr1 . 121.4(3) yes
C34 . N2 . Zr1 . 131.8(3) yes
C5 . P1 . C13 . 103.4(2) yes
C5 . P1 . C7 . 105.46(19) yes
C13 . P1 . C7 . 106.73(19) yes
C5 . P1 . Zr1 . 96.12(14) yes
C13 . P1 . Zr1 . 117.98(13) yes
C7 . P1 . Zr1 . 123.59(14) yes
C19 . P2 . C6 . 103.8(2) yes
C19 . P2 . C25 . 105.13(19) yes
C6 . P2 . C25 . 105.1(2) yes
C19 . P2 . Zr1 . 115.41(13) yes
C6 . P2 . Zr1 . 97.88(14) yes
C25 . P2 . Zr1 . 126.41(14) yes
C35 . P3 . C43 . 107.1(2) yes
C35 . P3 . C37 . 102.06(19) yes
C43 . P3 . C37 . 105.18(19) yes
C35 . P3 . Zr1 . 92.59(14) yes
C43 . P3 . Zr1 . 123.24(13) yes
C37 . P3 . Zr1 . 122.22(15) yes
C36 . P4 . C49 . 99.9(2) yes
C36 . P4 . C55 . 102.9(2) yes
C49 . P4 . C55 . 100.5(2) yes
P2 . Zr1 . P1 . 134.87(3) yes
P2 . Zr1 . P3 . 139.69(3) yes
P1 . Zr1 . P3 . 81.20(3) yes
P2 . Zr1 . N2 . 81.51(9) yes
P1 . Zr1 . N2 . 143.05(9) yes
P3 . Zr1 . N2 . 67.97(9) yes
P2 . Zr1 . N1 . 67.96(9) yes
P1 . Zr1 . N1 . 67.06(9) yes
P3 . Zr1 . N1 . 144.70(9) yes
N2 . Zr1 . N1 . 147.12(12) yes
P2 . Zr1 . Cl2 . 82.95(3) yes
P1 . Zr1 . Cl2 . 92.24(3) yes
P3 . Zr1 . Cl2 . 77.42(3) yes
N2 . Zr1 . Cl2 . 100.07(9) yes
N1 . Zr1 . Cl2 . 88.40(9) yes
P2 . Zr1 . Cl1 . 104.44(4) yes
P1 . Zr1 . Cl1 . 78.32(3) yes
P3 . Zr1 . Cl1 . 99.79(4) yes
N2 . Zr1 . Cl1 . 87.08(9) yes
N1 . Zr1 . Cl1 . 88.91(9) yes
Cl2 . Zr1 . Cl1 . 170.50(4) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C20 . H201 . C4 . 124 0.95 2.53 3.156(8) yes
C20 . H201 . N1 . 139 0.95 2.54 3.310(8) yes
C30 . H301 . C31 . 178 0.96 2.60 3.560(8) yes
C30 . H301 . N2 . 147 0.96 2.58 3.426(8) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
# looking for PLATON_SQD.SQF 

# SQUEEZE RESULTS (Version = 291119) 
# 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 0.500 0.500 0.500 142 39 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
####################################################################### 
# 
# 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_LiPNPPh
_database_code_depnum_ccdc_archive 'CCDC 2023867'
loop_
_audit_author_name
_audit_author_address
'F. Mark Chadwick'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2020-08-18 deposited with the CCDC.	2020-11-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-06
_audit_creation_method           CRYSTALS_ver_14.61_build_6999

_oxford_structure_analysis_title C:\Users\fchadwic\Desktop\solve\FMC2004.cif_
_chemical_name_systematic        .
_chemical_melting_point          'not measured'


_cell_length_a                   10.70733(3)
_cell_length_b                   10.84431(3)
_cell_length_c                   14.74442(3)
_cell_angle_alpha                94.396(4)
_cell_angle_beta                 105.416(4)
_cell_angle_gamma                114.647(4)
_cell_volume                     1465.32(8)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Li 0.0008 0.0003 1.1282 3.9546 0.7508 1.0524 0.6175 85.3905 0.4653 168.2610
0.0377 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C17 H17 Li0.50 N0.50 O0.50 P1 
# Dc =      0.61 Fooo =    286.00 Mu =      7.73 M =    270.77
# Found Formula = C34 H34 Li1 N1 O1 P2 
# Dc =      1.23 FOOO =    572.00 Mu =     15.45 M =    541.54

_chemical_formula_sum            'C34 H34 Li1 N1 O1 P2'
_chemical_formula_moiety         'C34 H34 Li1 N1 O1 P2'
_chemical_compound_source        .
_chemical_formula_weight         541.54


_cell_measurement_reflns_used    3783
_cell_measurement_theta_min      5
_cell_measurement_theta_max      73
_cell_measurement_temperature    173

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_max          0.100

_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             572
_exptl_absorpt_coefficient_mu    1.545

# Sheldrick geometric approximatio 0.86 0.86 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_T_max  0.86
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_reduction        
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      173
_diffrn_reflns_number            8327
_diffrn_reflns_av_unetI/netI     0.050
_reflns_number_total             5524
_diffrn_reflns_av_R_equivalents  0.027
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 5524 
# Theoretical number of reflections is about 11786 


_diffrn_reflns_theta_min         4.593
_diffrn_reflns_theta_max         73.368
_diffrn_measured_fraction_theta_max 0.935

_diffrn_reflns_theta_full        41.086
_diffrn_measured_fraction_theta_full 0.993


_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              -13
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_oxford_diffrn_Wilson_B_factor   2.63
_oxford_diffrn_Wilson_scale      0.02

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

_refine_diff_density_min         -0.47
_refine_diff_density_max         0.50


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


# The values actually used during refinement 
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_restraints     0
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5524
_oxford_refine_ls_R_factor_ref   0.0566
_refine_ls_wR_factor_ref         0.1005
_refine_ls_goodness_of_fit_ref   1.4590
_refine_ls_shift/su_max          0.0004157
_refine_ls_shift/su_mean         0.0000385


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        5524
_refine_ls_R_factor_all          0.0566
_refine_ls_wR_factor_all         0.1005

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4372
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_gt          0.0850


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 836. 0.130E+04 722. 245. 34.8 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
P1 P 1.21935(7) 0.86108(6) 1.04753(4) 0.0312 1.0000 Uani . . . . . .
C2 C 1.0282(3) 0.7952(2) 1.04466(16) 0.0323 1.0000 Uani . . . . . .
C3 C 0.9258(2) 0.6632(2) 0.97053(16) 0.0297 1.0000 Uani . . . . . .
N4 N 0.9770(2) 0.59053(19) 0.92297(13) 0.0280 1.0000 Uani . . . . . .
C5 C 0.8553(2) 0.4823(2) 0.85699(15) 0.0292 1.0000 Uani . . . . . .
C6 C 0.8710(3) 0.3896(2) 0.78457(15) 0.0315 1.0000 Uani . . . . . .
P7 P 0.83893(7) 0.43998(6) 0.66585(4) 0.0337 1.0000 Uani . . . . . .
C8 C 0.6394(3) 0.3527(3) 0.61935(16) 0.0366 1.0000 Uani . . . . . .
C9 C 0.5578(3) 0.2089(3) 0.5972(2) 0.0465 1.0000 Uani . . . . . .
C10 C 0.4067(3) 0.1464(4) 0.5663(2) 0.0647 1.0000 Uani . . . . . .
C11 C 0.3360(4) 0.2281(5) 0.5571(2) 0.0711 1.0000 Uani . . . . . .
C12 C 0.4145(4) 0.3713(5) 0.5775(2) 0.0720 1.0000 Uani . . . . . .
C13 C 0.5663(4) 0.4334(3) 0.6078(2) 0.0545 1.0000 Uani . . . . . .
C14 C 0.8751(2) 0.3212(2) 0.59344(16) 0.0329 1.0000 Uani . . . . . .
C15 C 0.9168(3) 0.2236(3) 0.62627(19) 0.0483 1.0000 Uani . . . . . .
C16 C 0.9501(4) 0.1445(4) 0.5673(2) 0.0611 1.0000 Uani . . . . . .
C17 C 0.9397(3) 0.1593(3) 0.4742(2) 0.0536 1.0000 Uani . . . . . .
C18 C 0.8977(3) 0.2549(3) 0.4405(2) 0.0533 1.0000 Uani . . . . . .
C19 C 0.8662(3) 0.3352(3) 0.49930(19) 0.0464 1.0000 Uani . . . . . .
C20 C 0.7294(2) 0.4845(3) 0.86386(17) 0.0347 1.0000 Uani . . . . . .
C21 C 0.7746(3) 0.6014(2) 0.93676(17) 0.0351 1.0000 Uani . . . . . .
C22 C 1.3043(3) 1.0038(2) 1.15388(17) 0.0341 1.0000 Uani . . . . . .
C23 C 1.2604(3) 1.1067(3) 1.1599(2) 0.0496 1.0000 Uani . . . . . .
C24 C 1.3158(3) 1.2053(3) 1.2450(2) 0.0548 1.0000 Uani . . . . . .
C25 C 1.4164(3) 1.2019(3) 1.3248(2) 0.0484 1.0000 Uani . . . . . .
C26 C 1.4649(3) 1.1036(3) 1.31806(19) 0.0480 1.0000 Uani . . . . . .
C27 C 1.4095(3) 1.0043(3) 1.23310(18) 0.0388 1.0000 Uani . . . . . .
C28 C 1.2246(3) 0.9569(2) 0.95034(17) 0.0340 1.0000 Uani . . . . . .
C29 C 1.1040(3) 0.9179(3) 0.86904(18) 0.0417 1.0000 Uani . . . . . .
C30 C 1.1139(4) 0.9893(3) 0.7948(2) 0.0553 1.0000 Uani . . . . . .
C31 C 1.2441(4) 1.0982(3) 0.8000(2) 0.0615 1.0000 Uani . . . . . .
C32 C 1.3648(4) 1.1362(3) 0.8792(2) 0.0619 1.0000 Uani . . . . . .
C33 C 1.3552(3) 1.0660(3) 0.9537(2) 0.0511 1.0000 Uani . . . . . .
O34 O 1.2791(2) 0.6059(3) 0.90312(14) 0.0595 1.0000 Uani . . . . . .
C35 C 1.2561(3) 0.6664(3) 0.82091(19) 0.0425 1.0000 Uani . . . . . .
C36 C 1.2659(3) 0.5781(3) 0.74162(19) 0.0489 1.0000 Uani . . . . . .
C37 C 1.3516(5) 0.5097(5) 0.7947(3) 0.0832 1.0000 Uani . . . . . .
C38 C 1.3738(5) 0.5482(6) 0.8933(3) 0.1089 1.0000 Uani . . . . . .
Li39 Li 1.1642(4) 0.5796(5) 0.9899(3) 0.0366 1.0000 Uani . . . . . .
H21 H 1.0250 0.7782 1.1091 0.0406 1.0000 Uiso R . . . . .
H22 H 0.9979 0.8677 1.0314 0.0409 1.0000 Uiso R . . . . .
H61 H 0.9709 0.4004 0.8083 0.0399 1.0000 Uiso R . . . . .
H62 H 0.8016 0.2910 0.7768 0.0408 1.0000 Uiso R . . . . .
H91 H 0.6097 0.1518 0.6038 0.0577 1.0000 Uiso R . . . . .
H101 H 0.3496 0.0447 0.5514 0.0803 1.0000 Uiso R . . . . .
H111 H 0.2327 0.1837 0.5371 0.0834 1.0000 Uiso R . . . . .
H121 H 0.3665 0.4290 0.5710 0.0858 1.0000 Uiso R . . . . .
H131 H 0.6216 0.5340 0.6211 0.0679 1.0000 Uiso R . . . . .
H151 H 0.9223 0.2086 0.6903 0.0582 1.0000 Uiso R . . . . .
H161 H 0.9774 0.0775 0.5912 0.0732 1.0000 Uiso R . . . . .
H171 H 0.9588 0.0999 0.4336 0.0651 1.0000 Uiso R . . . . .
H181 H 0.8904 0.2654 0.3751 0.0665 1.0000 Uiso R . . . . .
H191 H 0.8392 0.4045 0.4756 0.0586 1.0000 Uiso R . . . . .
H201 H 0.6317 0.4215 0.8255 0.0439 1.0000 Uiso R . . . . .
H211 H 0.7162 0.6363 0.9592 0.0433 1.0000 Uiso R . . . . .
H231 H 1.1899 1.1091 1.1049 0.0613 1.0000 Uiso R . . . . .
H241 H 1.2854 1.2760 1.2484 0.0663 1.0000 Uiso R . . . . .
H251 H 1.4505 1.2686 1.3850 0.0597 1.0000 Uiso R . . . . .
H261 H 1.5385 1.1037 1.3744 0.0589 1.0000 Uiso R . . . . .
H271 H 1.4453 0.9368 1.2282 0.0489 1.0000 Uiso R . . . . .
H291 H 1.0108 0.8400 0.8634 0.0510 1.0000 Uiso R . . . . .
H301 H 1.0305 0.9617 0.7400 0.0689 1.0000 Uiso R . . . . .
H311 H 1.2528 1.1487 0.7495 0.0743 1.0000 Uiso R . . . . .
H321 H 1.4549 1.2128 0.8831 0.0756 1.0000 Uiso R . . . . .
H331 H 1.4388 1.0929 1.0096 0.0644 1.0000 Uiso R . . . . .
H351 H 1.3340 0.7631 0.8364 0.0540 1.0000 Uiso R . . . . .
H352 H 1.1589 0.6653 0.8068 0.0545 1.0000 Uiso R . . . . .
H361 H 1.3172 0.6366 0.7020 0.0606 1.0000 Uiso R . . . . .
H362 H 1.1690 0.5061 0.7007 0.0606 1.0000 Uiso R . . . . .
H371 H 1.4438 0.5396 0.7822 0.1012 1.0000 Uiso R . . . . .
H372 H 1.2948 0.4078 0.7738 0.1023 1.0000 Uiso R . . . . .
H381 H 1.4742 0.6202 0.9226 0.1248 1.0000 Uiso R . . . . .
H382 H 1.3543 0.4672 0.9233 0.1236 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          5.19(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
P1 . C2 . 1.852(2) yes
P1 . C22 . 1.838(2) yes
P1 . C28 . 1.833(2) yes
C2 . C3 . 1.503(3) yes
C2 . H21 . 0.988 no
C2 . H22 . 0.982 no
C3 . N4 . 1.376(3) yes
C3 . C21 . 1.390(3) yes
N4 . C5 . 1.378(3) yes
C5 . C6 . 1.500(3) yes
C5 . C20 . 1.388(3) yes
C6 . P7 . 1.861(2) yes
C6 . H61 . 0.985 no
C6 . H62 . 0.991 no
P7 . C8 . 1.834(3) yes
P7 . C14 . 1.837(2) yes
C8 . C9 . 1.391(4) yes
C8 . C13 . 1.390(4) yes
C9 . C10 . 1.390(4) yes
C9 . H91 . 0.984 no
C10 . C11 . 1.378(5) yes
C10 . H101 . 0.983 no
C11 . C12 . 1.384(5) yes
C11 . H111 . 0.950 no
C12 . C13 . 1.396(5) yes
C12 . H121 . 0.956 no
C13 . H131 . 0.973 no
C14 . C15 . 1.383(4) yes
C14 . C19 . 1.390(3) yes
C15 . C16 . 1.387(4) yes
C15 . H151 . 0.961 no
C16 . C17 . 1.375(4) yes
C16 . H161 . 0.949 no
C17 . C18 . 1.369(4) yes
C17 . H171 . 0.964 no
C18 . C19 . 1.382(4) yes
C18 . H181 . 0.965 no
C19 . H191 . 0.968 no
C20 . C21 . 1.413(3) yes
C20 . H201 . 0.955 no
C21 . H211 . 0.965 no
C22 . C23 . 1.385(4) yes
C22 . C27 . 1.388(3) yes
C23 . C24 . 1.393(4) yes
C23 . H231 . 0.960 no
C24 . C25 . 1.383(4) yes
C24 . H241 . 0.952 no
C25 . C26 . 1.375(4) yes
C25 . H251 . 0.977 no
C26 . C27 . 1.395(4) yes
C26 . H261 . 0.980 no
C27 . H271 . 0.963 no
C28 . C29 . 1.388(3) yes
C28 . C33 . 1.390(4) yes
C29 . C30 . 1.390(4) yes
C29 . H291 . 0.978 no
C30 . C31 . 1.379(4) yes
C30 . H301 . 0.946 no
C31 . C32 . 1.372(5) yes
C31 . H311 . 0.958 no
C32 . C33 . 1.385(4) yes
C32 . H321 . 0.959 no
C33 . H331 . 0.958 no
O34 . C35 . 1.434(3) yes
O34 . C38 . 1.427(4) yes
C35 . C36 . 1.507(4) yes
C35 . H351 . 0.990 no
C35 . H352 . 1.001 no
C36 . C37 . 1.510(4) yes
C36 . H361 . 0.991 no
C36 . H362 . 0.985 no
C37 . C38 . 1.409(5) yes
C37 . H371 . 0.976 no
C37 . H372 . 0.987 no
C38 . H381 . 0.976 no
C38 . H382 . 0.983 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . P1 . C22 . 98.24(11) yes
C2 . P1 . C28 . 102.72(11) yes
C22 . P1 . C28 . 101.12(11) yes
P1 . C2 . C3 . 113.13(16) yes
P1 . C2 . H21 . 107.9 no
C3 . C2 . H21 . 109.1 no
P1 . C2 . H22 . 108.1 no
C3 . C2 . H22 . 109.7 no
H21 . C2 . H22 . 108.8 no
C2 . C3 . N4 . 121.2(2) yes
C2 . C3 . C21 . 127.8(2) yes
N4 . C3 . C21 . 111.0(2) yes
C3 . N4 . C5 . 105.57(18) yes
N4 . C5 . C6 . 120.1(2) yes
N4 . C5 . C20 . 110.9(2) yes
C6 . C5 . C20 . 128.8(2) yes
C5 . C6 . P7 . 110.35(15) yes
C5 . C6 . H61 . 107.9 no
P7 . C6 . H61 . 109.5 no
C5 . C6 . H62 . 111.0 no
P7 . C6 . H62 . 109.2 no
H61 . C6 . H62 . 108.9 no
C6 . P7 . C8 . 100.34(11) yes
C6 . P7 . C14 . 102.06(11) yes
C8 . P7 . C14 . 99.43(11) yes
P7 . C8 . C9 . 122.8(2) yes
P7 . C8 . C13 . 118.8(2) yes
C9 . C8 . C13 . 118.4(3) yes
C8 . C9 . C10 . 121.2(3) yes
C8 . C9 . H91 . 118.4 no
C10 . C9 . H91 . 120.3 no
C9 . C10 . C11 . 119.5(3) yes
C9 . C10 . H101 . 120.9 no
C11 . C10 . H101 . 119.6 no
C10 . C11 . C12 . 120.5(3) yes
C10 . C11 . H111 . 118.4 no
C12 . C11 . H111 . 121.1 no
C11 . C12 . C13 . 119.7(3) yes
C11 . C12 . H121 . 121.1 no
C13 . C12 . H121 . 119.2 no
C12 . C13 . C8 . 120.6(3) yes
C12 . C13 . H131 . 119.9 no
C8 . C13 . H131 . 119.5 no
P7 . C14 . C15 . 125.31(19) yes
P7 . C14 . C19 . 117.14(19) yes
C15 . C14 . C19 . 117.5(2) yes
C14 . C15 . C16 . 120.8(3) yes
C14 . C15 . H151 . 120.5 no
C16 . C15 . H151 . 118.7 no
C15 . C16 . C17 . 120.9(3) yes
C15 . C16 . H161 . 119.2 no
C17 . C16 . H161 . 119.9 no
C16 . C17 . C18 . 119.0(3) yes
C16 . C17 . H171 . 119.3 no
C18 . C17 . H171 . 121.7 no
C17 . C18 . C19 . 120.3(3) yes
C17 . C18 . H181 . 119.1 no
C19 . C18 . H181 . 120.6 no
C14 . C19 . C18 . 121.5(3) yes
C14 . C19 . H191 . 118.5 no
C18 . C19 . H191 . 119.9 no
C5 . C20 . C21 . 106.4(2) yes
C5 . C20 . H201 . 126.8 no
C21 . C20 . H201 . 126.7 no
C20 . C21 . C3 . 106.2(2) yes
C20 . C21 . H211 . 129.1 no
C3 . C21 . H211 . 124.7 no
P1 . C22 . C23 . 121.98(19) yes
P1 . C22 . C27 . 119.19(19) yes
C23 . C22 . C27 . 118.7(2) yes
C22 . C23 . C24 . 120.8(3) yes
C22 . C23 . H231 . 119.4 no
C24 . C23 . H231 . 119.8 no
C23 . C24 . C25 . 120.1(3) yes
C23 . C24 . H241 . 120.3 no
C25 . C24 . H241 . 119.6 no
C24 . C25 . C26 . 119.4(3) yes
C24 . C25 . H251 . 119.3 no
C26 . C25 . H251 . 121.3 no
C25 . C26 . C27 . 120.7(2) yes
C25 . C26 . H261 . 118.8 no
C27 . C26 . H261 . 120.5 no
C26 . C27 . C22 . 120.2(2) yes
C26 . C27 . H271 . 120.5 no
C22 . C27 . H271 . 119.3 no
P1 . C28 . C29 . 122.05(19) yes
P1 . C28 . C33 . 119.7(2) yes
C29 . C28 . C33 . 118.1(2) yes
C28 . C29 . C30 . 120.4(3) yes
C28 . C29 . H291 . 120.4 no
C30 . C29 . H291 . 119.2 no
C29 . C30 . C31 . 120.5(3) yes
C29 . C30 . H301 . 119.3 no
C31 . C30 . H301 . 120.1 no
C30 . C31 . C32 . 119.6(3) yes
C30 . C31 . H311 . 121.6 no
C32 . C31 . H311 . 118.8 no
C31 . C32 . C33 . 120.1(3) yes
C31 . C32 . H321 . 119.4 no
C33 . C32 . H321 . 120.4 no
C28 . C33 . C32 . 121.2(3) yes
C28 . C33 . H331 . 118.3 no
C32 . C33 . H331 . 120.5 no
C35 . O34 . C38 . 105.8(2) yes
O34 . C35 . C36 . 105.1(2) yes
O34 . C35 . H351 . 108.7 no
C36 . C35 . H351 . 110.9 no
O34 . C35 . H352 . 108.0 no
C36 . C35 . H352 . 113.6 no
H351 . C35 . H352 . 110.2 no
C35 . C36 . C37 . 103.8(2) yes
C35 . C36 . H361 . 110.6 no
C37 . C36 . H361 . 111.1 no
C35 . C36 . H362 . 111.5 no
C37 . C36 . H362 . 109.3 no
H361 . C36 . H362 . 110.3 no
C36 . C37 . C38 . 106.7(3) yes
C36 . C37 . H371 . 110.3 no
C38 . C37 . H371 . 111.4 no
C36 . C37 . H372 . 109.8 no
C38 . C37 . H372 . 108.9 no
H371 . C37 . H372 . 109.6 no
O34 . C38 . C37 . 109.0(3) yes
O34 . C38 . H381 . 108.6 no
C37 . C38 . H381 . 107.0 no
O34 . C38 . H382 . 109.8 no
C37 . C38 . H382 . 110.5 no
H381 . C38 . H382 . 111.8 no


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 

# start Validation Reply Form
_vrf_PLAT010_PNP2ZrCl2           
;
PROBLEM: No Suitable  (Embedded) Reflection Data Supplied     Please Do !  
RESPONSE: Reflection data embedded in CIF.
;
_vrf_PLAT027_PNP2ZrCl2           
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      43.32 Degree
RESPONSE: All crystals were found to be weakly diffracting, leading to low theta full values.
;
_vrf_PLAT010_PNP2HfCl2           
;
PROBLEM: No Suitable  (Embedded) Reflection Data Supplied     Please Do !  
RESPONSE: Reflection data embedded in CIF.
;
_vrf_PLAT027_PNP2HfCl2           
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      25.07 Degree
RESPONSE: All crystals were found to be weakly diffracting, leading to low theta full values.
;
_vrf_PLAT602_PNP2HfCl2           
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info  
RESPONSE: This is noted, and probably related to the low theta full values. No evidence of solvent occupancy was found.
;
_vrf_PLAT010_LiPNPPh             
;
PROBLEM: No Suitable  (Embedded) Reflection Data Supplied     Please Do !  
RESPONSE: Reflection data embedded in CIF.
;
_vrf_PLAT027_LiPNPPh             
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      41.09 Degree
RESPONSE: All crystals were found to be weakly diffracting, leading to low theta full values.
;
# end Validation Reply Form

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

data_PNP2HfCl2
_database_code_depnum_ccdc_archive 'CCDC 2023866'
loop_
_audit_author_name
_audit_author_address
'F. Mark Chadwick'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2020-08-18 deposited with the CCDC.	2020-11-10 downloaded from the CCDC.
;
_audit_creation_date             2020-03-06
_audit_creation_method           CRYSTALS_ver_14.61_build_6999
_oxford_structure_analysis_title 'lve\FMC2003\FMC2003.cif_od At 10: 4 on 5/ 3'
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   11.07535(3)
_cell_length_b                   13.14605(3)
_cell_length_c                   20.39291(4)
_cell_angle_alpha                84.873(4)
_cell_angle_beta                 86.804(5)
_cell_angle_gamma                66.482(5)
_cell_volume                     2710.96(10)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Hf -6.1794 4.9776 29.1440 1.8326 15.1726 9.5999 14.7586 0.2751 4.3001 72.0290
8.5815 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C60 H52 Cl8 Hf2 N4 P8 
# Dc =      2.10 Fooo =   1680.00 Mu =    132.12 M =   1717.49
# Found Formula = C60 H52 Cl2 Hf1 N2 P4 
# Dc =      1.44 FOOO =   1184.00 Mu =     58.85 M =   1174.38

_chemical_formula_sum            'C60 H52 Cl2 Hf1 N2 P4'
_chemical_formula_moiety         'C60 H52 Cl2 Hf1 N2 P4'
_chemical_compound_source        .
_chemical_formula_weight         1174.38


_cell_measurement_reflns_used    3904
_cell_measurement_theta_min      4
_cell_measurement_theta_max      71
_cell_measurement_temperature    173

_exptl_crystal_description       block
_exptl_crystal_colour            yello
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1184
_exptl_absorpt_coefficient_mu    5.885

# Sheldrick geometric approximatio 0.31 0.56 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_T_max  0.56
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_reduction        
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      173
_diffrn_reflns_number            15997
_diffrn_reflns_av_unetI/netI     0.112
_reflns_number_total             11605
_diffrn_reflns_av_R_equivalents  0.069
# Number of reflections without Friedels Law is 11605 
# Number of reflections with Friedels Law is 10317 
# Theoretical number of reflections is about 10966 


_diffrn_reflns_theta_min         3.677
_diffrn_reflns_theta_max         73.742
_diffrn_measured_fraction_theta_max 0.940

_diffrn_reflns_theta_full        25.072
_diffrn_measured_fraction_theta_full 0.993


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       20
_reflns_limit_h_min              -13
_reflns_limit_h_max              12
_reflns_limit_k_min              -15
_reflns_limit_k_max              16
_reflns_limit_l_min              -25
_reflns_limit_l_max              20

_oxford_diffrn_Wilson_B_factor   2.90
_oxford_diffrn_Wilson_scale      1.49

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

_refine_diff_density_min         -1.78
_refine_diff_density_max         3.36


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


# The values actually used during refinement 
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_restraints     140
_refine_ls_number_parameters     677
_refine_ls_number_reflns         11601
_oxford_refine_ls_R_factor_ref   0.1028
_refine_ls_wR_factor_ref         0.2571
_refine_ls_goodness_of_fit_ref   1.5867
_refine_ls_shift/su_max          0.0102888
_refine_ls_shift/su_mean         0.0002721


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        11601
_refine_ls_R_factor_all          0.1028
_refine_ls_wR_factor_all         0.2571

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8407
_refine_ls_R_factor_gt           0.0759
_refine_ls_wR_factor_gt          0.2129


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 914. 0.140E+04 852. 336. 55.5 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.2944(10) 0.2606(9) 0.2791(5) 0.0401 1.0000 Uani . . . . . .
C2 C 0.1763(11) 0.2749(10) 0.3091(6) 0.0499 1.0000 Uani . . . . . .
C3 C 0.2009(10) 0.1947(10) 0.3629(5) 0.0437 1.0000 Uani . . . . . .
C4 C 0.3362(12) 0.1356(9) 0.3635(6) 0.0454 1.0000 Uani . . . . . .
C5 C 0.3282(11) 0.3254(10) 0.2230(6) 0.0475 1.0000 Uani . . . . . .
C6 C 0.4155(11) 0.0403(9) 0.4091(6) 0.0432 1.0000 Uani . . . . . .
C7 C 0.4204(11) 0.4345(9) 0.3126(5) 0.0409 1.0000 Uani . . . . . .
C8 C 0.2875(12) 0.5025(11) 0.3224(7) 0.0560 1.0000 Uani . . . . . .
C9 C 0.2487(14) 0.5741(12) 0.3717(8) 0.0680 1.0000 Uani . . . . . .
C10 C 0.3421(14) 0.5775(12) 0.4128(7) 0.0643 1.0000 Uani . . . . . .
C11 C 0.4722(14) 0.5099(11) 0.4047(6) 0.0553 1.0000 Uani . . . . . .
C12 C 0.5108(12) 0.4395(10) 0.3555(5) 0.0471 1.0000 Uani . . . . . .
C13 C 0.5276(11) 0.4066(10) 0.1762(6) 0.0434 1.0000 Uani . . . . . .
C14 C 0.4761(15) 0.5223(11) 0.1661(6) 0.0613 1.0000 Uani . . . . . .
C15 C 0.5246(18) 0.5701(13) 0.1131(8) 0.0731 1.0000 Uani . . . . . .
C16 C 0.6112(18) 0.5098(12) 0.0695(7) 0.0702 1.0000 Uani . . . . . .
C17 C 0.6601(16) 0.3950(13) 0.0775(7) 0.0669 1.0000 Uani . . . . . .
C18 C 0.6167(13) 0.3451(11) 0.1318(6) 0.0513 1.0000 Uani . . . . . .
C19 C 0.4638(11) -0.1170(9) 0.3091(5) 0.0413 1.0000 Uani . . . . . .
C20 C 0.5017(13) -0.2290(10) 0.3093(6) 0.0503 1.0000 Uani . . . . . .
C21 C 0.4428(14) -0.2773(11) 0.2738(7) 0.0580 1.0000 Uani . . . . . .
C22 C 0.3387(13) -0.2118(11) 0.2342(7) 0.0563 1.0000 Uani . . . . . .
C23 C 0.2948(12) -0.0973(11) 0.2341(6) 0.0502 1.0000 Uani . . . . . .
C24 C 0.3561(11) -0.0479(10) 0.2691(6) 0.0462 1.0000 Uani . . . . . .
C25 C 0.6507(11) -0.1626(9) 0.4138(5) 0.0405 1.0000 Uani . . . . . .
C26 C 0.7857(12) -0.1957(10) 0.4132(6) 0.0486 1.0000 Uani . . . . . .
C27 C 0.8620(13) -0.2816(12) 0.4562(6) 0.0553 1.0000 Uani . . . . . .
C28 C 0.8063(13) -0.3339(11) 0.5013(6) 0.0555 1.0000 Uani . . . . . .
C29 C 0.6717(16) -0.3020(12) 0.5048(6) 0.0614 1.0000 Uani . . . . . .
C30 C 0.5946(13) -0.2171(10) 0.4598(7) 0.0551 1.0000 Uani . . . . . .
C31 C 0.9218(11) -0.0492(9) 0.2960(5) 0.0409 1.0000 Uani . . . . . .
C32 C 1.0115(11) -0.1552(10) 0.2909(6) 0.0485 1.0000 Uani . . . . . .
C33 C 0.9551(12) -0.2142(9) 0.2598(6) 0.0485 1.0000 Uani . . . . . .
C34 C 0.8249(11) -0.1412(9) 0.2474(5) 0.0403 1.0000 Uani . . . . . .
C35 C 0.9356(10) 0.0499(9) 0.3191(5) 0.0401 1.0000 Uani . . . . . .
C36 C 0.7331(11) -0.1674(10) 0.2067(5) 0.0443 1.0000 Uani . U . . . .
C37 C 0.9248(11) 0.1493(9) 0.1881(5) 0.0424 1.0000 Uani . . . . . .
C38 C 1.0293(12) 0.1833(11) 0.1772(6) 0.0503 1.0000 Uani . . . . . .
C39 C 1.0994(13) 0.1652(12) 0.1181(7) 0.0579 1.0000 Uani . . . . . .
C40 C 1.0697(13) 0.1125(12) 0.0713(7) 0.0604 1.0000 Uani . . . . . .
C41 C 0.9696(14) 0.0737(13) 0.0817(6) 0.0607 1.0000 Uani . . . . . .
C42 C 0.8981(12) 0.0917(10) 0.1396(5) 0.0470 1.0000 Uani . . . . . .
C43 C 0.8366(10) 0.2930(9) 0.2959(5) 0.0377 1.0000 Uani . . . . . .
C44 C 0.8096(11) 0.3898(10) 0.2547(6) 0.0453 1.0000 Uani . . . . . .
C45 C 0.8029(13) 0.4860(10) 0.2797(7) 0.0533 1.0000 Uani . . . . . .
C46 C 0.8236(12) 0.4889(11) 0.3447(7) 0.0553 1.0000 Uani . . . . . .
C47 C 0.8526(12) 0.3948(12) 0.3853(6) 0.0546 1.0000 Uani . . . . . .
C48 C 0.8572(11) 0.2975(10) 0.3624(6) 0.0445 1.0000 Uani . . . . . .
C49 C 0.6444(12) -0.1668(9) 0.0745(6) 0.0451 1.0000 Uani . U . . . .
C50 C 0.5154(13) -0.1139(12) 0.0958(7) 0.0570 1.0000 Uani . U . . . .
C51 C 0.4141(15) -0.1135(13) 0.0587(8) 0.0693 1.0000 Uani . . . . . .
C52 C 0.4413(15) -0.1652(13) 0.0001(7) 0.0673 1.0000 Uani . . . . . .
C53 C 0.5688(15) -0.2166(12) -0.0192(7) 0.0644 1.0000 Uani . . . . . .
C54 C 0.6700(13) -0.2191(11) 0.0161(6) 0.0527 1.0000 Uani . U . . . .
C55 C 0.923(7) -0.271(5) 0.1082(8) 0.0526 0.30(5) Uani . U P 1 1 .
C56 C 1.042(5) -0.247(6) 0.0969(7) 0.0613 0.30(5) Uani . U P 1 1 .
C57 C 1.156(5) -0.355(6) 0.0896(7) 0.0638 0.30(5) Uani . U P 1 1 .
C58 C 1.156(6) -0.462(7) 0.0928(8) 0.0686 0.30(5) Uani . U P 1 1 .
C59 C 1.032(7) -0.474(6) 0.1043(8) 0.0695 0.30(5) Uani . U P 1 1 .
C60 C 0.926(6) -0.374(6) 0.1110(7) 0.0619 0.30(5) Uani . U P 1 1 .
C61 C 0.908(3) -0.294(2) 0.1074(5) 0.0510 0.70(5) Uani . U P 1 2 .
C62 C 1.037(2) -0.300(3) 0.0935(5) 0.0664 0.70(5) Uani . U P 1 2 .
C63 C 1.139(3) -0.410(3) 0.0846(5) 0.0698 0.70(5) Uani . U P 1 2 .
C64 C 1.105(4) -0.499(3) 0.0904(6) 0.0785 0.70(5) Uani . U P 1 2 .
C65 C 0.980(3) -0.497(2) 0.1041(6) 0.0738 0.70(5) Uani . U P 1 2 .
C66 C 0.885(3) -0.393(2) 0.1123(5) 0.0658 0.70(5) Uani . U P 1 2 .
P1 P 0.4779(3) 0.3364(2) 0.24788(13) 0.0375 1.0000 Uani . . . . . .
P2 P 0.5457(3) -0.0518(2) 0.35680(13) 0.0388 1.0000 Uani . . . . . .
P3 P 0.8301(3) 0.1686(2) 0.26564(13) 0.0361 1.0000 Uani . . . . . .
P4 P 0.7776(3) -0.1505(3) 0.11755(14) 0.0478 1.0000 Uani . U . . . .
N1 N 0.3965(9) 0.1739(7) 0.3117(4) 0.0392 1.0000 Uani . . . . . .
N2 N 0.8002(9) -0.0390(7) 0.2697(4) 0.0386 1.0000 Uani . . . . . .
Cl2 Cl 0.6488(2) 0.1494(2) 0.39621(12) 0.0413 1.0000 Uani . . . . . .
Cl1 Cl 0.5614(3) 0.0998(2) 0.17488(12) 0.0443 1.0000 Uani . . . . . .
Hf1 Hf 0.61238(5) 0.10929(4) 0.28695(2) 0.0358 1.0000 Uani . . . . . .
H21 H 0.0928 0.3287 0.2965 0.0611 1.0000 Uiso R . . . . .
H31 H 0.1388 0.1832 0.3930 0.0522 1.0000 Uiso R . . . . .
H52 H 0.2572 0.3999 0.2142 0.0590 1.0000 Uiso R . . . . .
H51 H 0.3434 0.2868 0.1820 0.0590 1.0000 Uiso R . . . . .
H62 H 0.4522 0.0651 0.4435 0.0539 1.0000 Uiso R . . . . .
H61 H 0.3614 0.0023 0.4293 0.0538 1.0000 Uiso R . . . . .
H81 H 0.2240 0.4970 0.2960 0.0681 1.0000 Uiso R . . . . .
H91 H 0.1593 0.6211 0.3775 0.0811 1.0000 Uiso R . . . . .
H101 H 0.3149 0.6276 0.4455 0.0760 1.0000 Uiso R . . . . .
H111 H 0.5349 0.5109 0.4340 0.0691 1.0000 Uiso R . . . . .
H121 H 0.6002 0.3939 0.3494 0.0571 1.0000 Uiso R . . . . .
H141 H 0.4077 0.5687 0.1929 0.0740 1.0000 Uiso R . . . . .
H151 H 0.4947 0.6483 0.1069 0.0840 1.0000 Uiso R . . . . .
H161 H 0.6419 0.5451 0.0343 0.0790 1.0000 Uiso R . . . . .
H171 H 0.7227 0.3527 0.0469 0.0781 1.0000 Uiso R . . . . .
H181 H 0.6479 0.2670 0.1366 0.0611 1.0000 Uiso R . . . . .
H201 H 0.5728 -0.2743 0.3349 0.0591 1.0000 Uiso R . . . . .
H211 H 0.4725 -0.3559 0.2783 0.0691 1.0000 Uiso R . . . . .
H221 H 0.2982 -0.2442 0.2064 0.0700 1.0000 Uiso R . . . . .
H231 H 0.2193 -0.0509 0.2090 0.0621 1.0000 Uiso R . . . . .
H241 H 0.3292 0.0299 0.2676 0.0560 1.0000 Uiso R . . . . .
H261 H 0.8252 -0.1585 0.3830 0.0580 1.0000 Uiso R . . . . .
H271 H 0.9548 -0.3038 0.4547 0.0681 1.0000 Uiso R . . . . .
H281 H 0.8590 -0.3922 0.5303 0.0690 1.0000 Uiso R . . . . .
H291 H 0.6304 -0.3372 0.5348 0.0722 1.0000 Uiso R . . . . .
H301 H 0.5021 -0.1958 0.4611 0.0641 1.0000 Uiso R . . . . .
H321 H 1.0978 -0.1840 0.3059 0.0579 1.0000 Uiso R . . . . .
H331 H 0.9966 -0.2890 0.2495 0.0580 1.0000 Uiso R . . . . .
H351 H 1.0272 0.0423 0.3151 0.0490 1.0000 Uiso R . . . . .
H352 H 0.9070 0.0601 0.3648 0.0488 1.0000 Uiso R . . . . .
H362 H 0.7404 -0.2434 0.2180 0.0528 1.0000 Uiso R . . . . .
H361 H 0.6420 -0.1173 0.2157 0.0530 1.0000 Uiso R . . . . .
H381 H 1.0529 0.2170 0.2101 0.0620 1.0000 Uiso R . . . . .
H391 H 1.1673 0.1900 0.1104 0.0701 1.0000 Uiso R . . . . .
H401 H 1.1180 0.1022 0.0311 0.0719 1.0000 Uiso R . . . . .
H411 H 0.9508 0.0365 0.0489 0.0711 1.0000 Uiso R . . . . .
H421 H 0.8316 0.0637 0.1482 0.0570 1.0000 Uiso R . . . . .
H441 H 0.7934 0.3891 0.2092 0.0559 1.0000 Uiso R . . . . .
H451 H 0.7850 0.5512 0.2506 0.0640 1.0000 Uiso R . . . . .
H461 H 0.8200 0.5552 0.3621 0.0670 1.0000 Uiso R . . . . .
H471 H 0.8706 0.3957 0.4301 0.0651 1.0000 Uiso R . . . . .
H481 H 0.8744 0.2334 0.3920 0.0531 1.0000 Uiso R . . . . .
H501 H 0.4961 -0.0772 0.1349 0.0681 1.0000 Uiso R . . . . .
H511 H 0.3268 -0.0799 0.0761 0.0850 1.0000 Uiso R . . . . .
H521 H 0.3708 -0.1622 -0.0266 0.0821 1.0000 Uiso R . . . . .
H531 H 0.5880 -0.2544 -0.0587 0.0781 1.0000 Uiso R . . . . .
H541 H 0.7592 -0.2556 0.0019 0.0640 1.0000 Uiso R . . . . .
H561 H 1.0478 -0.1709 0.0930 0.0630 0.30(5) Uiso R . P 1 1 .
H571 H 1.2403 -0.3549 0.0816 0.0620 0.30(5) Uiso R . P 1 1 .
H581 H 1.2352 -0.5237 0.0870 0.0730 0.30(5) Uiso R . P 1 1 .
H591 H 1.0194 -0.5454 0.1074 0.0750 0.30(5) Uiso R . P 1 1 .
H601 H 0.8419 -0.3805 0.1191 0.0690 0.30(5) Uiso R . P 1 1 .
H621 H 1.0553 -0.2332 0.0902 0.0801 0.70(5) Uiso R . P 1 2 .
H631 H 1.2263 -0.4189 0.0750 0.0850 0.70(5) Uiso R . P 1 2 .
H641 H 1.1721 -0.5692 0.0841 0.0960 0.70(5) Uiso R . P 1 2 .
H651 H 0.9626 -0.5633 0.1075 0.0871 0.70(5) Uiso R . P 1 2 .
H661 H 0.7952 -0.3867 0.1223 0.0791 0.70(5) Uiso R . P 1 2 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          1.286(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C2 . 1.362(16) yes
C1 . C5 . 1.485(16) yes
C1 . N1 . 1.392(13) yes
C2 . C3 . 1.411(17) yes
C2 . H21 . 0.945 no
C3 . C4 . 1.386(15) yes
C3 . H31 . 0.943 no
C4 . C6 . 1.486(15) yes
C4 . N1 . 1.381(14) yes
C5 . P1 . 1.823(11) yes
C5 . H52 . 0.990 no
C5 . H51 . 0.990 no
C6 . P2 . 1.830(12) yes
C6 . H62 . 0.971 no
C6 . H61 . 0.976 no
C7 . C8 . 1.398(16) yes
C7 . C12 . 1.390(16) yes
C7 . P1 . 1.835(11) yes
C8 . C9 . 1.37(2) yes
C8 . H81 . 0.937 no
C9 . C10 . 1.38(2) yes
C9 . H91 . 0.942 no
C10 . C11 . 1.368(19) yes
C10 . H101 . 0.931 no
C11 . C12 . 1.360(18) yes
C11 . H111 . 0.945 no
C12 . H121 . 0.939 no
C13 . C14 . 1.395(17) yes
C13 . C18 . 1.357(17) yes
C13 . P1 . 1.835(12) yes
C14 . C15 . 1.39(2) yes
C14 . H141 . 0.943 no
C15 . C16 . 1.33(2) yes
C15 . H151 . 0.944 no
C16 . C17 . 1.38(2) yes
C16 . H161 . 0.942 no
C17 . C18 . 1.395(18) yes
C17 . H171 . 0.941 no
C18 . H181 . 0.941 no
C19 . C20 . 1.360(16) yes
C19 . C24 . 1.424(15) yes
C19 . P2 . 1.836(12) yes
C20 . C21 . 1.349(18) yes
C20 . H201 . 0.929 no
C21 . C22 . 1.382(18) yes
C21 . H211 . 0.948 no
C22 . C23 . 1.385(18) yes
C22 . H221 . 0.963 no
C23 . C24 . 1.371(17) yes
C23 . H231 . 0.958 no
C24 . H241 . 0.941 no
C25 . C26 . 1.379(16) yes
C25 . C30 . 1.397(16) yes
C25 . P2 . 1.823(11) yes
C26 . C27 . 1.380(17) yes
C26 . H261 . 0.947 no
C27 . C28 . 1.364(18) yes
C27 . H271 . 0.949 no
C28 . C29 . 1.378(19) yes
C28 . H281 . 0.937 no
C29 . C30 . 1.400(18) yes
C29 . H291 . 0.941 no
C30 . H301 . 0.947 no
C31 . C32 . 1.360(16) yes
C31 . C35 . 1.491(16) yes
C31 . N2 . 1.428(14) yes
C32 . C33 . 1.384(18) yes
C32 . H321 . 0.935 no
C33 . C34 . 1.399(15) yes
C33 . H331 . 0.942 no
C34 . C36 . 1.506(16) yes
C34 . N2 . 1.374(14) yes
C35 . P3 . 1.836(10) yes
C35 . H351 . 0.978 no
C35 . H352 . 0.971 no
C36 . P4 . 1.873(11) yes
C36 . H362 . 0.977 no
C36 . H361 . 0.978 no
C37 . C38 . 1.398(16) yes
C37 . C42 . 1.409(17) yes
C37 . P3 . 1.827(12) yes
C38 . C39 . 1.382(18) yes
C38 . H381 . 0.938 no
C39 . C40 . 1.35(2) yes
C39 . H391 . 0.932 no
C40 . C41 . 1.393(19) yes
C40 . H401 . 0.944 no
C41 . C42 . 1.369(16) yes
C41 . H411 . 0.940 no
C42 . H421 . 0.949 no
C43 . C44 . 1.395(15) yes
C43 . C48 . 1.398(16) yes
C43 . P3 . 1.827(11) yes
C44 . C45 . 1.379(18) yes
C44 . H441 . 0.956 no
C45 . C46 . 1.366(19) yes
C45 . H451 . 0.956 no
C46 . C47 . 1.360(19) yes
C46 . H461 . 0.955 no
C47 . C48 . 1.381(18) yes
C47 . H471 . 0.947 no
C48 . H481 . 0.952 no
C49 . C50 . 1.380(17) yes
C49 . C54 . 1.388(17) yes
C49 . P4 . 1.849(13) yes
C50 . C51 . 1.385(19) yes
C50 . H501 . 0.940 no
C51 . C52 . 1.39(2) yes
C51 . H511 . 0.951 no
C52 . C53 . 1.35(2) yes
C52 . H521 . 0.962 no
C53 . C54 . 1.353(19) yes
C53 . H531 . 0.954 no
C54 . H541 . 0.951 no
C55 . C56 . 1.47(8) yes
C55 . C60 . 1.34(9) yes
C55 . P4 . 1.77(6) yes
C56 . C57 . 1.49(7) yes
C56 . H561 . 1.028 no
C57 . C58 . 1.40(9) yes
C57 . H571 . 0.937 no
C58 . C59 . 1.46(9) yes
C58 . H581 . 0.940 no
C59 . C60 . 1.39(8) yes
C59 . H591 . 0.991 no
C60 . H601 . 0.972 no
C61 . C62 . 1.41(3) yes
C61 . C66 . 1.42(3) yes
C61 . P4 . 1.88(3) yes
C62 . C63 . 1.45(4) yes
C62 . H621 . 0.978 no
C63 . C64 . 1.37(4) yes
C63 . H631 . 0.942 no
C64 . C65 . 1.39(4) yes
C64 . H641 . 0.936 no
C65 . C66 . 1.37(3) yes
C65 . H651 . 0.965 no
C66 . H661 . 0.972 no
P1 . Hf1 . 2.815(3) yes
P2 . Hf1 . 2.766(3) yes
P3 . Hf1 . 2.817(3) yes
N1 . Hf1 . 2.240(9) yes
N2 . Hf1 . 2.249(8) yes
Cl2 . Hf1 . 2.426(2) yes
Cl1 . Hf1 . 2.410(3) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . C5 . 130.8(10) yes
C2 . C1 . N1 . 110.6(10) yes
C5 . C1 . N1 . 118.5(9) yes
C1 . C2 . C3 . 107.5(10) yes
C1 . C2 . H21 . 126.7 no
C3 . C2 . H21 . 125.8 no
C2 . C3 . C4 . 106.0(10) yes
C2 . C3 . H31 . 127.6 no
C4 . C3 . H31 . 126.4 no
C3 . C4 . C6 . 128.8(11) yes
C3 . C4 . N1 . 110.7(10) yes
C6 . C4 . N1 . 120.5(10) yes
C1 . C5 . P1 . 104.5(7) yes
C1 . C5 . H52 . 112.3 no
P1 . C5 . H52 . 111.0 no
C1 . C5 . H51 . 111.1 no
P1 . C5 . H51 . 111.2 no
H52 . C5 . H51 . 106.9 no
C4 . C6 . P2 . 104.7(8) yes
C4 . C6 . H62 . 110.9 no
P2 . C6 . H62 . 111.1 no
C4 . C6 . H61 . 110.6 no
P2 . C6 . H61 . 110.5 no
H62 . C6 . H61 . 109.0 no
C8 . C7 . C12 . 118.0(11) yes
C8 . C7 . P1 . 122.6(9) yes
C12 . C7 . P1 . 119.4(9) yes
C7 . C8 . C9 . 120.7(13) yes
C7 . C8 . H81 . 119.6 no
C9 . C8 . H81 . 119.7 no
C8 . C9 . C10 . 119.5(12) yes
C8 . C9 . H91 . 120.5 no
C10 . C9 . H91 . 120.1 no
C9 . C10 . C11 . 120.6(13) yes
C9 . C10 . H101 . 118.8 no
C11 . C10 . H101 . 120.7 no
C10 . C11 . C12 . 120.0(13) yes
C10 . C11 . H111 . 120.0 no
C12 . C11 . H111 . 120.0 no
C7 . C12 . C11 . 121.3(12) yes
C7 . C12 . H121 . 118.6 no
C11 . C12 . H121 . 120.1 no
C14 . C13 . C18 . 118.9(12) yes
C14 . C13 . P1 . 121.5(10) yes
C18 . C13 . P1 . 119.6(9) yes
C13 . C14 . C15 . 118.4(13) yes
C13 . C14 . H141 . 122.3 no
C15 . C14 . H141 . 119.3 no
C14 . C15 . C16 . 122.4(14) yes
C14 . C15 . H151 . 119.6 no
C16 . C15 . H151 . 117.9 no
C15 . C16 . C17 . 119.9(14) yes
C15 . C16 . H161 . 120.0 no
C17 . C16 . H161 . 120.1 no
C16 . C17 . C18 . 118.7(14) yes
C16 . C17 . H171 . 119.4 no
C18 . C17 . H171 . 121.9 no
C17 . C18 . C13 . 121.6(13) yes
C17 . C18 . H181 . 118.8 no
C13 . C18 . H181 . 119.5 no
C20 . C19 . C24 . 117.7(11) yes
C20 . C19 . P2 . 123.3(9) yes
C24 . C19 . P2 . 118.9(9) yes
C19 . C20 . C21 . 123.5(12) yes
C19 . C20 . H201 . 117.9 no
C21 . C20 . H201 . 118.6 no
C20 . C21 . C22 . 119.7(12) yes
C20 . C21 . H211 . 118.3 no
C22 . C21 . H211 . 122.0 no
C21 . C22 . C23 . 118.5(12) yes
C21 . C22 . H221 . 121.4 no
C23 . C22 . H221 . 120.1 no
C22 . C23 . C24 . 121.9(12) yes
C22 . C23 . H231 . 119.3 no
C24 . C23 . H231 . 118.8 no
C19 . C24 . C23 . 118.5(11) yes
C19 . C24 . H241 . 119.2 no
C23 . C24 . H241 . 122.3 no
C26 . C25 . C30 . 118.0(10) yes
C26 . C25 . P2 . 122.2(8) yes
C30 . C25 . P2 . 119.7(9) yes
C25 . C26 . C27 . 120.4(11) yes
C25 . C26 . H261 . 119.1 no
C27 . C26 . H261 . 120.4 no
C26 . C27 . C28 . 121.1(12) yes
C26 . C27 . H271 . 119.2 no
C28 . C27 . H271 . 119.6 no
C27 . C28 . C29 . 120.5(12) yes
C27 . C28 . H281 . 120.6 no
C29 . C28 . H281 . 118.9 no
C28 . C29 . C30 . 118.3(12) yes
C28 . C29 . H291 . 122.6 no
C30 . C29 . H291 . 119.0 no
C29 . C30 . C25 . 121.5(12) yes
C29 . C30 . H301 . 119.0 no
C25 . C30 . H301 . 119.5 no
C32 . C31 . C35 . 130.8(11) yes
C32 . C31 . N2 . 108.8(10) yes
C35 . C31 . N2 . 120.2(9) yes
C31 . C32 . C33 . 109.2(11) yes
C31 . C32 . H321 . 125.6 no
C33 . C32 . H321 . 125.1 no
C32 . C33 . C34 . 106.4(10) yes
C32 . C33 . H331 . 126.3 no
C34 . C33 . H331 . 127.3 no
C33 . C34 . C36 . 123.8(10) yes
C33 . C34 . N2 . 110.3(10) yes
C36 . C34 . N2 . 125.3(10) yes
C31 . C35 . P3 . 105.4(7) yes
C31 . C35 . H351 . 110.9 no
P3 . C35 . H351 . 110.6 no
C31 . C35 . H352 . 111.1 no
P3 . C35 . H352 . 110.4 no
H351 . C35 . H352 . 108.4 no
C34 . C36 . P4 . 108.5(8) yes
C34 . C36 . H362 . 110.5 no
P4 . C36 . H362 . 110.0 no
C34 . C36 . H361 . 109.8 no
P4 . C36 . H361 . 110.5 no
H362 . C36 . H361 . 107.6 no
C38 . C37 . C42 . 118.8(11) yes
C38 . C37 . P3 . 121.9(9) yes
C42 . C37 . P3 . 119.2(9) yes
C37 . C38 . C39 . 119.8(12) yes
C37 . C38 . H381 . 120.2 no
C39 . C38 . H381 . 120.1 no
C38 . C39 . C40 . 120.5(13) yes
C38 . C39 . H391 . 119.5 no
C40 . C39 . H391 . 120.0 no
C39 . C40 . C41 . 121.2(12) yes
C39 . C40 . H401 . 119.0 no
C41 . C40 . H401 . 119.9 no
C40 . C41 . C42 . 119.3(13) yes
C40 . C41 . H411 . 120.1 no
C42 . C41 . H411 . 120.6 no
C37 . C42 . C41 . 120.5(12) yes
C37 . C42 . H421 . 119.0 no
C41 . C42 . H421 . 120.5 no
C44 . C43 . C48 . 117.7(11) yes
C44 . C43 . P3 . 121.1(8) yes
C48 . C43 . P3 . 121.0(8) yes
C43 . C44 . C45 . 120.4(11) yes
C43 . C44 . H441 . 119.2 no
C45 . C44 . H441 . 120.4 no
C44 . C45 . C46 . 121.2(12) yes
C44 . C45 . H451 . 119.1 no
C46 . C45 . H451 . 119.7 no
C45 . C46 . C47 . 119.2(13) yes
C45 . C46 . H461 . 121.4 no
C47 . C46 . H461 . 119.4 no
C46 . C47 . C48 . 121.2(12) yes
C46 . C47 . H471 . 119.4 no
C48 . C47 . H471 . 119.4 no
C43 . C48 . C47 . 120.3(11) yes
C43 . C48 . H481 . 119.9 no
C47 . C48 . H481 . 119.8 no
C50 . C49 . C54 . 118.9(12) yes
C50 . C49 . P4 . 119.7(10) yes
C54 . C49 . P4 . 120.9(10) yes
C49 . C50 . C51 . 119.9(13) yes
C49 . C50 . H501 . 120.2 no
C51 . C50 . H501 . 119.9 no
C50 . C51 . C52 . 120.5(14) yes
C50 . C51 . H511 . 117.6 no
C52 . C51 . H511 . 121.9 no
C51 . C52 . C53 . 118.1(14) yes
C51 . C52 . H521 . 120.5 no
C53 . C52 . H521 . 121.3 no
C52 . C53 . C54 . 122.8(14) yes
C52 . C53 . H531 . 118.3 no
C54 . C53 . H531 . 118.8 no
C49 . C54 . C53 . 119.8(13) yes
C49 . C54 . H541 . 118.4 no
C53 . C54 . H541 . 121.8 no
C56 . C55 . C60 . 123(6) yes
C56 . C55 . P4 . 114(4) yes
C60 . C55 . P4 . 123(5) yes
C55 . C56 . C57 . 108(5) yes
C55 . C56 . H561 . 127.3 no
C57 . C56 . H561 . 124.6 no
C56 . C57 . C58 . 128(5) yes
C56 . C57 . H571 . 119.2 no
C58 . C57 . H571 . 112.7 no
C57 . C58 . C59 . 119(5) yes
C57 . C58 . H581 . 120.2 no
C59 . C58 . H581 . 120.8 no
C58 . C59 . C60 . 113(6) yes
C58 . C59 . H591 . 126.4 no
C60 . C59 . H591 . 121.1 no
C59 . C60 . C55 . 129(6) yes
C59 . C60 . H601 . 113.8 no
C55 . C60 . H601 . 116.7 no
C62 . C61 . C66 . 119(3) yes
C62 . C61 . P4 . 116.2(19) yes
C66 . C61 . P4 . 125(2) yes
C61 . C62 . C63 . 117(3) yes
C61 . C62 . H621 . 120.3 no
C63 . C62 . H621 . 122.5 no
C62 . C63 . C64 . 119(3) yes
C62 . C63 . H631 . 120.8 no
C64 . C63 . H631 . 120.4 no
C63 . C64 . C65 . 126(3) yes
C63 . C64 . H641 . 117.4 no
C65 . C64 . H641 . 116.7 no
C64 . C65 . C66 . 115(3) yes
C64 . C65 . H651 . 121.7 no
C66 . C65 . H651 . 123.6 no
C61 . C66 . C65 . 124(3) yes
C61 . C66 . H661 . 118.1 no
C65 . C66 . H661 . 117.5 no
C13 . P1 . C7 . 107.4(5) yes
C13 . P1 . C5 . 104.8(5) yes
C7 . P1 . C5 . 103.8(6) yes
C13 . P1 . Hf1 . 123.5(4) yes
C7 . P1 . Hf1 . 117.7(4) yes
C5 . P1 . Hf1 . 96.1(4) yes
C19 . P2 . C6 . 105.1(5) yes
C19 . P2 . C25 . 105.5(5) yes
C6 . P2 . C25 . 104.6(5) yes
C19 . P2 . Hf1 . 115.2(4) yes
C6 . P2 . Hf1 . 97.7(4) yes
C25 . P2 . Hf1 . 126.0(4) yes
C35 . P3 . C37 . 102.3(5) yes
C35 . P3 . C43 . 106.6(5) yes
C37 . P3 . C43 . 104.8(5) yes
C35 . P3 . Hf1 . 92.7(4) yes
C37 . P3 . Hf1 . 122.4(4) yes
C43 . P3 . Hf1 . 123.5(3) yes
C36 . P4 . C49 . 103.2(5) yes
C36 . P4 . C55 . 102.4(10) yes
C49 . P4 . C55 . 108.2(19) yes
C61 . P4 . C36 . 99.4(6) yes
C61 . P4 . C49 . 97.6(8) yes
C36 . P4 . C49 . 103.2(5) yes
C1 . N1 . C4 . 105.2(9) yes
C1 . N1 . Hf1 . 128.0(7) yes
C4 . N1 . Hf1 . 126.8(7) yes
C31 . N2 . C34 . 105.3(8) yes
C31 . N2 . Hf1 . 121.2(7) yes
C34 . N2 . Hf1 . 132.3(7) yes
P1 . Hf1 . P3 . 80.93(8) yes
P1 . Hf1 . P2 . 135.27(8) yes
P3 . Hf1 . P2 . 139.55(8) yes
P1 . Hf1 . N2 . 142.5(2) yes
P3 . Hf1 . N2 . 68.0(2) yes
P2 . Hf1 . N2 . 81.7(2) yes
P1 . Hf1 . N1 . 66.8(2) yes
P3 . Hf1 . N1 . 144.3(2) yes
P2 . Hf1 . N1 . 68.6(2) yes
N2 . Hf1 . N1 . 147.6(3) yes
P1 . Hf1 . Cl2 . 92.36(9) yes
P3 . Hf1 . Cl2 . 77.54(8) yes
P2 . Hf1 . Cl2 . 82.74(9) yes
N2 . Hf1 . Cl2 . 100.6(2) yes
N1 . Hf1 . Cl2 . 88.4(2) yes
P1 . Hf1 . Cl1 . 78.91(9) yes
P3 . Hf1 . Cl1 . 100.25(9) yes
P2 . Hf1 . Cl1 . 103.84(9) yes
N2 . Hf1 . Cl1 . 86.2(2) yes
N1 . Hf1 . Cl1 . 88.7(2) yes
Cl2 . Hf1 . Cl1 . 171.25(9) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C24 . H241 . C4 . 125 0.94 2.52 3.15(3) yes
C24 . H241 . N1 . 140 0.94 2.54 3.32(3) yes


# looking for ARCHIVE-HKL.CIF 

