# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_pf2b2cam
_database_code_depnum_ccdc_archive 'CCDC 2262037'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2023-05-10 deposited with the CCDC.	2023-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H44 F6 N4 O4 P2, 6(H2 O)'
_chemical_formula_sum            'C30 H56 F6 N4 O10 P2'
_chemical_formula_weight         808.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9086(3)
_cell_length_b                   10.8155(4)
_cell_length_c                   11.9920(4)
_cell_angle_alpha                63.6730(10)
_cell_angle_beta                 70.0310(10)
_cell_angle_gamma                76.3980(10)
_cell_volume                     968.51(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7892
_cell_measurement_theta_min      2.4446
_cell_measurement_theta_max      27.5542

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_F_000             428
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.570
_exptl_crystal_size_mid          0.323
_exptl_crystal_size_min          0.192
_exptl_absorpt_coefficient_mu    0.197
_shelx_estimated_absorpt_T_min   0.896
_shelx_estimated_absorpt_T_max   0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            14239
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.969
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4447
_reflns_number_gt                3810
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Instrument Service v2015.3.1.0'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 758)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0485P)²+0.2990P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4447
_refine_ls_number_parameters     271
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0930
_refine_ls_wR_factor_gt          0.0876
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N -0.02163(12) 0.25232(10) 0.43726(10) 0.0171(2) Uani 1 1 d . . . . .
C2 C -0.18335(14) 0.24759(13) 0.52409(12) 0.0199(3) Uani 1 1 d . . . . .
H21 H -0.2411 0.1855 0.5160 0.024 Uiso 1 1 calc R U . . .
H22 H -0.2412 0.3416 0.4966 0.024 Uiso 1 1 calc R U . . .
C3 C -0.18757(15) 0.19721(13) 0.66541(13) 0.0214(3) Uani 1 1 d . . . . .
H31 H -0.1683 0.2750 0.6796 0.026 Uiso 1 1 calc R U . . .
H32 H -0.2964 0.1707 0.7198 0.026 Uiso 1 1 calc R U . . .
N4 N -0.06743(13) 0.07652(10) 0.70933(10) 0.0176(2) Uani 1 1 d . . . . .
H41 H 0.033(2) 0.0994(16) 0.6605(16) 0.028(4) Uiso 1 1 d . . . . .
C5 C -0.09217(15) -0.04961(12) 0.69724(12) 0.0199(3) Uani 1 1 d . . . . .
H51 H -0.1122 -0.0214 0.6125 0.024 Uiso 1 1 calc R U . . .
H52 H -0.1881 -0.0911 0.7657 0.024 Uiso 1 1 calc R U . . .
C6 C 0.05236(15) -0.15754(13) 0.70875(13) 0.0206(3) Uani 1 1 d . . . . .
H61 H 0.0718 -0.1873 0.7939 0.025 Uiso 1 1 calc R U . . .
H62 H 0.1488 -0.1163 0.6408 0.025 Uiso 1 1 calc R U . . .
C7 C 0.02419(16) -0.28298(12) 0.69456(12) 0.0198(3) Uani 1 1 d . . . . .
H71 H 0.1101 -0.3583 0.7182 0.024 Uiso 1 1 calc R U . . .
H72 H -0.0794 -0.3165 0.7557 0.024 Uiso 1 1 calc R U . . .
C8 C 0.07552(15) 0.34663(12) 0.43571(13) 0.0191(2) Uani 1 1 d . . . . .
H81 H 0.0264 0.3728 0.5108 0.023 Uiso 1 1 calc R U . . .
H82 H 0.0859 0.4319 0.3553 0.023 Uiso 1 1 calc R U . . .
P1 P 0.27070(4) 0.24760(3) 0.44423(3) 0.01708(10) Uani 1 1 d . . . . .
O11 O 0.24162(10) 0.12668(9) 0.57398(9) 0.0210(2) Uani 1 1 d . . . . .
O12 O 0.34941(11) 0.21911(9) 0.32520(9) 0.0224(2) Uani 1 1 d . . . . .
C9 C 0.39031(16) 0.35646(14) 0.45447(13) 0.0235(3) Uani 1 1 d . . . . .
H91 H 0.3193 0.4048 0.5099 0.028 Uiso 1 1 calc R U . . .
H92 H 0.4729 0.2954 0.4982 0.028 Uiso 1 1 calc R U . . .
C10 C 0.47213(16) 0.46231(14) 0.32913(14) 0.0262(3) Uani 1 1 d . . . . .
F1 F 0.53414(12) 0.55264(10) 0.34724(10) 0.0447(3) Uani 1 1 d . . . . .
F2 F 0.37288(11) 0.53982(9) 0.25535(9) 0.0352(2) Uani 1 1 d . . . . .
F3 F 0.59380(10) 0.40814(10) 0.25738(9) 0.0392(2) Uani 1 1 d . . . . .
C11 C -0.07608(17) 0.04242(13) 0.84794(12) 0.0223(3) Uani 1 1 d . . . . .
H111 H -0.1874 0.0242 0.9017 0.027 Uiso 1 1 calc R U . . .
H112 H -0.0056 -0.0438 0.8793 0.027 Uiso 1 1 calc R U . . .
C12 C -0.02751(16) 0.15476(13) 0.86697(12) 0.0208(3) Uani 1 1 d . . . . .
C13 C 0.13431(17) 0.16505(15) 0.84334(13) 0.0274(3) Uani 1 1 d . . . . .
H131 H 0.2140 0.1059 0.8090 0.033 Uiso 1 1 calc R U . . .
C14 C 0.1796(2) 0.26174(17) 0.86985(15) 0.0376(4) Uani 1 1 d . . . . .
H141 H 0.2901 0.2678 0.8544 0.045 Uiso 1 1 calc R U . . .
C15 C 0.0648(2) 0.34859(16) 0.91842(16) 0.0412(4) Uani 1 1 d . . . . .
H151 H 0.0964 0.4144 0.9363 0.049 Uiso 1 1 calc R U . . .
C16 C -0.0955(2) 0.34050(15) 0.94114(16) 0.0396(4) Uani 1 1 d . . . . .
H161 H -0.1744 0.4015 0.9735 0.047 Uiso 1 1 calc R U . . .
C17 C -0.14216(18) 0.24248(15) 0.91663(14) 0.0286(3) Uani 1 1 d . . . . .
H171 H -0.2529 0.2358 0.9340 0.034 Uiso 1 1 calc R U . . .
O1W O 0.49550(13) -0.03090(11) 0.31930(11) 0.0287(2) Uani 1 1 d . . . . .
H11W H 0.449(3) 0.042(2) 0.331(2) 0.055(6) Uiso 1 1 d . . . . .
H12W H 0.579(3) -0.055(2) 0.3486(19) 0.046(5) Uiso 1 1 d . . . . .
O2W O 0.4190(2) 0.37078(17) 0.05582(14) 0.0539(4) Uani 1 1 d D . . . .
H21W H 0.414(3) 0.333(2) 0.132(2) 0.054(6) Uiso 1 1 d . . . . .
H22W H 0.449(8) 0.316(6) 0.019(6) 0.12(3) Uiso 0.5 1 d D . P A 1
H23W H 0.469(6) 0.435(5) 0.018(5) 0.069(17) Uiso 0.5 1 d . . P B 2
O3W O 0.48709(18) 0.09065(17) 0.05800(14) 0.0449(3) Uani 1 1 d . . . . .
H31W H 0.505(3) 0.048(2) 0.129(2) 0.054(6) Uiso 1 1 d . . . . .
H32W H 0.514(6) 0.043(5) 0.012(5) 0.069(15) Uiso 0.5 1 d . . P C 1
H33W H 0.463(6) 0.170(6) 0.045(5) 0.069(16) Uiso 0.5 1 d . . P D 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
N1 C2 1.4578(16) . ?
N1 C7 1.4715(16) 2_556 ?
N1 C8 1.4756(14) . ?
C2 C3 1.5223(18) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.4983(16) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C5 1.5064(14) . ?
N4 C11 1.5123(16) . ?
N4 H41 0.907(18) . ?
C5 C6 1.5202(17) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 C7 1.5254(16) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
C7 N1 1.4714(16) 2_556 ?
C7 H71 0.9900 . ?
C7 H72 0.9900 . ?
C8 P1 1.8246(13) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
P1 O12 1.4929(9) . ?
P1 O11 1.5092(9) . ?
P1 C9 1.8288(12) . ?
C9 C10 1.4896(19) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
C10 F3 1.3303(17) . ?
C10 F2 1.3398(16) . ?
C10 F1 1.3531(15) . ?
C11 C12 1.5087(17) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 C17 1.3886(19) . ?
C12 C13 1.393(2) . ?
C13 C14 1.392(2) . ?
C13 H131 0.9500 . ?
C14 C15 1.376(3) . ?
C14 H141 0.9500 . ?
C15 C16 1.376(3) . ?
C15 H151 0.9500 . ?
C16 C17 1.396(2) . ?
C16 H161 0.9500 . ?
C17 H171 0.9500 . ?
O1W H11W 0.85(2) . ?
O1W H12W 0.87(2) . ?
O2W H21W 0.81(2) . ?
O2W H22W 0.84(2) . ?
O2W H23W 0.78(5) . ?
O3W H31W 0.82(3) . ?
O3W H32W 0.86(5) . ?
O3W H33W 0.79(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C7 111.43(10) . 2_556 ?
C2 N1 C8 114.32(10) . . ?
C7 N1 C8 110.91(10) 2_556 . ?
N1 C2 C3 113.78(10) . . ?
N1 C2 H21 108.8 . . ?
C3 C2 H21 108.8 . . ?
N1 C2 H22 108.8 . . ?
C3 C2 H22 108.8 . . ?
H21 C2 H22 107.7 . . ?
N4 C3 C2 114.40(10) . . ?
N4 C3 H31 108.7 . . ?
C2 C3 H31 108.7 . . ?
N4 C3 H32 108.7 . . ?
C2 C3 H32 108.7 . . ?
H31 C3 H32 107.6 . . ?
C3 N4 C5 112.55(9) . . ?
C3 N4 C11 109.34(10) . . ?
C5 N4 C11 110.03(9) . . ?
C3 N4 H41 109.7(10) . . ?
C5 N4 H41 107.5(10) . . ?
C11 N4 H41 107.6(10) . . ?
N4 C5 C6 111.88(10) . . ?
N4 C5 H51 109.2 . . ?
C6 C5 H51 109.2 . . ?
N4 C5 H52 109.2 . . ?
C6 C5 H52 109.2 . . ?
H51 C5 H52 107.9 . . ?
C5 C6 C7 110.54(10) . . ?
C5 C6 H61 109.5 . . ?
C7 C6 H61 109.5 . . ?
C5 C6 H62 109.5 . . ?
C7 C6 H62 109.5 . . ?
H61 C6 H62 108.1 . . ?
N1 C7 C6 112.96(10) 2_556 . ?
N1 C7 H71 109.0 2_556 . ?
C6 C7 H71 109.0 . . ?
N1 C7 H72 109.0 2_556 . ?
C6 C7 H72 109.0 . . ?
H71 C7 H72 107.8 . . ?
N1 C8 P1 104.71(8) . . ?
N1 C8 H81 110.8 . . ?
P1 C8 H81 110.8 . . ?
N1 C8 H82 110.8 . . ?
P1 C8 H82 110.8 . . ?
H81 C8 H82 108.9 . . ?
O12 P1 O11 118.71(5) . . ?
O12 P1 C8 110.23(6) . . ?
O11 P1 C8 105.94(6) . . ?
O12 P1 C9 109.83(6) . . ?
O11 P1 C9 105.29(6) . . ?
C8 P1 C9 106.05(6) . . ?
C10 C9 P1 115.90(9) . . ?
C10 C9 H91 108.3 . . ?
P1 C9 H91 108.3 . . ?
C10 C9 H92 108.3 . . ?
P1 C9 H92 108.3 . . ?
H91 C9 H92 107.4 . . ?
F3 C10 F2 106.64(12) . . ?
F3 C10 F1 106.08(11) . . ?
F2 C10 F1 105.71(11) . . ?
F3 C10 C9 113.41(12) . . ?
F2 C10 C9 112.90(11) . . ?
F1 C10 C9 111.55(11) . . ?
C12 C11 N4 114.23(10) . . ?
C12 C11 H111 108.7 . . ?
N4 C11 H111 108.7 . . ?
C12 C11 H112 108.7 . . ?
N4 C11 H112 108.7 . . ?
H111 C11 H112 107.6 . . ?
C17 C12 C13 119.03(12) . . ?
C17 C12 C11 120.93(12) . . ?
C13 C12 C11 119.88(12) . . ?
C14 C13 C12 120.17(14) . . ?
C14 C13 H131 119.9 . . ?
C12 C13 H131 119.9 . . ?
C15 C14 C13 120.24(15) . . ?
C15 C14 H141 119.9 . . ?
C13 C14 H141 119.9 . . ?
C16 C15 C14 120.25(14) . . ?
C16 C15 H151 119.9 . . ?
C14 C15 H151 119.9 . . ?
C15 C16 C17 119.94(15) . . ?
C15 C16 H161 120.0 . . ?
C17 C16 H161 120.0 . . ?
C12 C17 C16 120.36(14) . . ?
C12 C17 H171 119.8 . . ?
C16 C17 H171 119.8 . . ?
H11W O1W H12W 106.4(19) . . ?
H21W O2W H22W 113(5) . . ?
H21W O2W H23W 114(4) . . ?
H31W O3W H32W 114(4) . . ?
H31W O3W H33W 110(4) . . ?

_refine_diff_density_max         0.319
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.048



####################################################################### 
# 
# 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_campf2
_database_code_depnum_ccdc_archive 'CCDC 2262042'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2023-05-10 deposited with the CCDC.	2023-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H32 F6 N4 O4 P2, 4(C2 H4 O2)'
_chemical_formula_sum            'C24 H48 F6 N4 O12 P2'
_chemical_formula_weight         760.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   8.1091(3)
_cell_length_b                   19.7189(8)
_cell_length_c                   10.8818(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.755(2)
_cell_angle_gamma                90
_cell_volume                     1739.88(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6896
_cell_measurement_theta_min      2.7161
_cell_measurement_theta_max      27.4869

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_F_000             800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.369
_exptl_crystal_size_min          0.258
_exptl_absorpt_coefficient_mu    0.219
_shelx_estimated_absorpt_T_min   0.915
_shelx_estimated_absorpt_T_max   0.946
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            13629
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.066
_diffrn_reflns_theta_max         27.516
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4007
_reflns_number_gt                3515
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Instrument Service v2016.1.0.1'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 758)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0394P)²+0.7850P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4007
_refine_ls_number_parameters     235
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0842
_refine_ls_wR_factor_gt          0.0804
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
N1 N 0.30564(13) 0.56106(5) 0.42828(11) 0.0227(2) Uani 1 1 d . . . . .
C2 C 0.19557(16) 0.54993(7) 0.53330(15) 0.0308(3) Uani 1 1 d . . . . .
H21 H 0.1572 0.5023 0.5323 0.037 Uiso 1 1 calc R U . . .
H22 H 0.0975 0.5794 0.5238 0.037 Uiso 1 1 calc R U . . .
C3 C 0.27777(18) 0.56447(7) 0.65590(14) 0.0312(3) Uani 1 1 d . . . . .
H31 H 0.3156 0.6122 0.6586 0.037 Uiso 1 1 calc R U . . .
H32 H 0.1982 0.5575 0.7229 0.037 Uiso 1 1 calc R U . . .
N4 N 0.42037(15) 0.51821(6) 0.67262(10) 0.0238(2) Uani 1 1 d . . . . .
H41 H 0.384(2) 0.4741(10) 0.6711(16) 0.037(5) Uiso 1 1 d . . . . .
H42 H 0.485(2) 0.5243(9) 0.6112(16) 0.030(4) Uiso 1 1 d . . . . .
C5 C 0.5248(2) 0.52759(8) 0.78475(12) 0.0350(4) Uani 1 1 d . . . . .
H51 H 0.4547 0.5260 0.8585 0.042 Uiso 1 1 calc R U . . .
H52 H 0.5789 0.5726 0.7821 0.042 Uiso 1 1 calc R U . . .
C6 C 0.6547(2) 0.47270(8) 0.79331(14) 0.0407(4) Uani 1 1 d . . . . .
H61 H 0.5986 0.4284 0.8023 0.049 Uiso 1 1 calc R U . . .
H62 H 0.7217 0.4804 0.8687 0.049 Uiso 1 1 calc R U . . .
C7 C 0.77014(19) 0.46837(8) 0.68461(15) 0.0358(4) Uani 1 1 d . . . . .
H71 H 0.8104 0.5145 0.6655 0.043 Uiso 1 1 calc R U . . .
H72 H 0.8669 0.4405 0.7086 0.043 Uiso 1 1 calc R U . . .
C8 C 0.34230(16) 0.63470(6) 0.41287(13) 0.0243(3) Uani 1 1 d . . . . .
H81 H 0.2757 0.6616 0.4709 0.029 Uiso 1 1 calc R U . . .
H82 H 0.3129 0.6491 0.3282 0.029 Uiso 1 1 calc R U . . .
P1 P 0.56089(4) 0.64981(2) 0.44232(3) 0.01679(9) Uani 1 1 d . . . . .
O11 O 0.65634(12) 0.61517(5) 0.34263(9) 0.0265(2) Uani 1 1 d . . . . .
O12 O 0.60120(11) 0.62828(5) 0.57144(8) 0.0231(2) Uani 1 1 d . . . . .
C9 C 0.60001(16) 0.74035(6) 0.42376(11) 0.0210(3) Uani 1 1 d . . . . .
H91 H 0.7182 0.7486 0.4423 0.025 Uiso 1 1 calc R U . . .
H92 H 0.5813 0.7519 0.3361 0.025 Uiso 1 1 calc R U . . .
C10 C 0.50182(17) 0.78849(6) 0.49897(12) 0.0222(3) Uani 1 1 d . . . . .
F1 F 0.55161(12) 0.85301(4) 0.48547(9) 0.0374(2) Uani 1 1 d . . . . .
F2 F 0.50897(14) 0.77580(5) 0.61904(8) 0.0419(2) Uani 1 1 d . . . . .
F3 F 0.34131(11) 0.78811(5) 0.46858(11) 0.0481(3) Uani 1 1 d . . . . .
C1A C 0.9812(2) 0.60708(8) -0.01335(14) 0.0336(3) Uani 1 1 d . . . . .
H11A H 1.0411 0.5662 -0.0376 0.040 Uiso 1 1 calc R U . . .
H12A H 1.0602 0.6430 0.0078 0.040 Uiso 1 1 calc R U . . .
H13A H 0.9104 0.6222 -0.0817 0.040 Uiso 1 1 calc R U . . .
C2A C 0.87722(16) 0.59170(7) 0.09586(13) 0.0246(3) Uani 1 1 d . . . . .
O21A O 0.85835(15) 0.64425(5) 0.16864(11) 0.0363(3) Uani 1 1 d . . . . .
H21A H 0.792(3) 0.6331(12) 0.229(2) 0.065(7) Uiso 1 1 d . . . . .
O22A O 0.81490(16) 0.53726(5) 0.11500(11) 0.0419(3) Uani 1 1 d . . . . .
C1B C 1.08822(17) 0.73227(8) 0.74019(14) 0.0298(3) Uani 1 1 d . . . . .
H11B H 1.1667 0.7603 0.6950 0.036 Uiso 1 1 calc R U . . .
H12B H 1.1472 0.6949 0.7807 0.036 Uiso 1 1 calc R U . . .
H13B H 1.0335 0.7601 0.8022 0.036 Uiso 1 1 calc R U . . .
C2B C 0.96173(16) 0.70409(7) 0.65258(12) 0.0221(3) Uani 1 1 d . . . . .
O21B O 0.83438(13) 0.67663(6) 0.70984(9) 0.0301(2) Uani 1 1 d . . . . .
H21B H 0.760(3) 0.6606(11) 0.654(2) 0.060(6) Uiso 1 1 d . . . . .
O22B O 0.97438(13) 0.70498(6) 0.54237(9) 0.0316(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C2 1.4757(18) . ?
N1 C7 1.4845(18) 3_666 ?
N1 C8 1.4923(16) . ?
C2 C3 1.511(2) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.4822(19) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C5 1.4876(19) . ?
N4 H41 0.919(19) . ?
N4 H42 0.866(18) . ?
C5 C6 1.512(3) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 C7 1.520(3) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
C7 N1 1.4845(18) 3_666 ?
C7 H71 0.9900 . ?
C7 H72 0.9900 . ?
C8 P1 1.8217(13) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
P1 O12 1.4997(9) . ?
P1 O11 1.5049(9) . ?
P1 C9 1.8251(13) . ?
C9 C10 1.4906(18) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
C10 F2 1.3308(16) . ?
C10 F3 1.3388(16) . ?
C10 F1 1.3434(15) . ?
C1A C2A 1.4972(19) . ?
C1A H11A 0.9800 . ?
C1A H12A 0.9800 . ?
C1A H13A 0.9800 . ?
C2A O22A 1.2058(17) . ?
C2A O21A 1.3144(17) . ?
O21A H21A 0.88(2) . ?
C1B C2B 1.4980(19) . ?
C1B H11B 0.9800 . ?
C1B H12B 0.9800 . ?
C1B H13B 0.9800 . ?
C2B O22B 1.2052(16) . ?
C2B O21B 1.3285(16) . ?
O21B H21B 0.90(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C7 109.56(11) . 3_666 ?
C2 N1 C8 110.80(11) . . ?
C7 N1 C8 111.61(11) 3_666 . ?
N1 C2 C3 113.03(11) . . ?
N1 C2 H21 109.0 . . ?
C3 C2 H21 109.0 . . ?
N1 C2 H22 109.0 . . ?
C3 C2 H22 109.0 . . ?
H21 C2 H22 107.8 . . ?
N4 C3 C2 109.03(11) . . ?
N4 C3 H31 109.9 . . ?
C2 C3 H31 109.9 . . ?
N4 C3 H32 109.9 . . ?
C2 C3 H32 109.9 . . ?
H31 C3 H32 108.3 . . ?
C3 N4 C5 117.32(12) . . ?
C3 N4 H41 109.2(11) . . ?
C5 N4 H41 108.2(11) . . ?
C3 N4 H42 107.6(11) . . ?
C5 N4 H42 105.7(11) . . ?
H41 N4 H42 108.5(15) . . ?
N4 C5 C6 110.49(11) . . ?
N4 C5 H51 109.6 . . ?
C6 C5 H51 109.6 . . ?
N4 C5 H52 109.6 . . ?
C6 C5 H52 109.6 . . ?
H51 C5 H52 108.1 . . ?
C5 C6 C7 115.32(12) . . ?
C5 C6 H61 108.4 . . ?
C7 C6 H61 108.4 . . ?
C5 C6 H62 108.4 . . ?
C7 C6 H62 108.4 . . ?
H61 C6 H62 107.5 . . ?
N1 C7 C6 114.42(12) 3_666 . ?
N1 C7 H71 108.7 3_666 . ?
C6 C7 H71 108.7 . . ?
N1 C7 H72 108.7 3_666 . ?
C6 C7 H72 108.7 . . ?
H71 C7 H72 107.6 . . ?
N1 C8 P1 109.52(8) . . ?
N1 C8 H81 109.8 . . ?
P1 C8 H81 109.8 . . ?
N1 C8 H82 109.8 . . ?
P1 C8 H82 109.8 . . ?
H81 C8 H82 108.2 . . ?
O12 P1 O11 116.04(6) . . ?
O12 P1 C8 108.55(6) . . ?
O11 P1 C8 107.90(6) . . ?
O12 P1 C9 110.16(6) . . ?
O11 P1 C9 105.82(6) . . ?
C8 P1 C9 108.10(6) . . ?
C10 C9 P1 117.86(9) . . ?
C10 C9 H91 107.8 . . ?
P1 C9 H91 107.8 . . ?
C10 C9 H92 107.8 . . ?
P1 C9 H92 107.8 . . ?
H91 C9 H92 107.2 . . ?
F2 C10 F3 105.73(12) . . ?
F2 C10 F1 106.03(11) . . ?
F3 C10 F1 105.72(11) . . ?
F2 C10 C9 113.74(11) . . ?
F3 C10 C9 112.67(11) . . ?
F1 C10 C9 112.30(11) . . ?
C2A C1A H11A 109.5 . . ?
C2A C1A H12A 109.5 . . ?
H11A C1A H12A 109.5 . . ?
C2A C1A H13A 109.5 . . ?
H11A C1A H13A 109.5 . . ?
H12A C1A H13A 109.5 . . ?
O22A C2A O21A 123.05(13) . . ?
O22A C2A C1A 124.00(13) . . ?
O21A C2A C1A 112.94(12) . . ?
C2A O21A H21A 109.2(15) . . ?
C2B C1B H11B 109.5 . . ?
C2B C1B H12B 109.5 . . ?
H11B C1B H12B 109.5 . . ?
C2B C1B H13B 109.5 . . ?
H11B C1B H13B 109.5 . . ?
H12B C1B H13B 109.5 . . ?
O22B C2B O21B 123.34(12) . . ?
O22B C2B C1B 124.15(13) . . ?
O21B C2B C1B 112.51(12) . . ?
C2B O21B H21B 110.1(14) . . ?

_refine_diff_density_max         0.347
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.046



####################################################################### 
# 
# 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_cul2trans
_database_code_depnum_ccdc_archive 'CCDC 2262038'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2023-05-10 deposited with the CCDC.	2023-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H30 Cu F6 N4 O4 P2, Cl O4, H3 O, H2 O'
_chemical_formula_sum            'C16 H35 Cl Cu F6 N4 O10 P2'
_chemical_formula_weight         718.41

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8024(3)
_cell_length_b                   10.5793(3)
_cell_length_c                   13.9063(4)
_cell_angle_alpha                86.5240(10)
_cell_angle_beta                 83.3100(10)
_cell_angle_gamma                72.3210(10)
_cell_volume                     1364.17(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9936
_cell_measurement_theta_min      2.498
_cell_measurement_theta_max      27.4728

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark blue-violet'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_F_000             738
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.112
_exptl_absorpt_coefficient_mu    1.114
_shelx_estimated_absorpt_T_min   0.826
_shelx_estimated_absorpt_T_max   0.885
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            26816
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.021
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6257
_reflns_number_gt                5931
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0279P)²+1.5388P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6257
_refine_ls_number_parameters     392
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0276
_refine_ls_wR_factor_ref         0.0685
_refine_ls_wR_factor_gt          0.0673
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1A Cu 0.5000 1.0000 0.0000 0.01202(7) Uani 1 2 d S . P . .
N1A N 0.34411(15) 0.98828(14) 0.11103(10) 0.0166(3) Uani 1 1 d . . . . .
C2A C 0.42016(19) 0.97418(17) 0.20031(12) 0.0197(3) Uani 1 1 d . . . . .
H21A H 0.3641 0.9427 0.2553 0.024 Uiso 1 1 calc R U . . .
H22A H 0.4266 1.0619 0.2165 0.024 Uiso 1 1 calc R U . . .
C3A C 0.56947(18) 0.87761(17) 0.18583(12) 0.0190(3) Uani 1 1 d . . . . .
H31A H 0.6234 0.8806 0.2412 0.023 Uiso 1 1 calc R U . . .
H32A H 0.5635 0.7863 0.1823 0.023 Uiso 1 1 calc R U . . .
N4A N 0.64530(15) 0.91397(14) 0.09440(10) 0.0173(3) Uani 1 1 d . . . . .
H41A H 0.680(2) 0.979(2) 0.1095(17) 0.027(6) Uiso 1 1 d . . . . .
C5A C 0.76943(18) 0.80206(18) 0.05779(13) 0.0214(3) Uani 1 1 d . . . . .
H51A H 0.7339 0.7294 0.0398 0.026 Uiso 1 1 calc R U . . .
H52A H 0.8326 0.7678 0.1101 0.026 Uiso 1 1 calc R U . . .
C6A C 0.85626(19) 0.84250(17) -0.02934(13) 0.0213(3) Uani 1 1 d . . . . .
H61A H 0.9431 0.7669 -0.0459 0.026 Uiso 1 1 calc R U . . .
H62A H 0.8891 0.9167 -0.0110 0.026 Uiso 1 1 calc R U . . .
C7A C 0.77732(18) 0.88504(17) -0.11903(13) 0.0195(3) Uani 1 1 d . . . . .
H71A H 0.8476 0.8949 -0.1739 0.023 Uiso 1 1 calc R U . . .
H72A H 0.7388 0.8133 -0.1347 0.023 Uiso 1 1 calc R U . . .
C8A C 0.28687(18) 0.87350(17) 0.10388(13) 0.0196(3) Uani 1 1 d . . . . .
H81A H 0.1951 0.9058 0.0742 0.024 Uiso 1 1 calc R U . . .
H82A H 0.2652 0.8402 0.1702 0.024 Uiso 1 1 calc R U . . .
P1A P 0.40743(5) 0.73430(4) 0.03361(3) 0.01609(9) Uani 1 1 d . . . . .
O11A O 0.47826(13) 0.79412(12) -0.05186(9) 0.0183(2) Uani 1 1 d . . . . .
O12A O 0.50477(13) 0.63504(12) 0.09691(9) 0.0209(3) Uani 1 1 d . . . . .
C9A C 0.29052(19) 0.65364(17) -0.01423(13) 0.0195(3) Uani 1 1 d . . . . .
H91A H 0.2237 0.7200 -0.0537 0.023 Uiso 1 1 calc R U . . .
H92A H 0.3509 0.5833 -0.0582 0.023 Uiso 1 1 calc R U . . .
C10A C 0.2035(2) 0.59297(18) 0.05913(14) 0.0236(4) Uani 1 1 d . . . . .
F1A F 0.11486(14) 0.68395(13) 0.12001(10) 0.0392(3) Uani 1 1 d . . . . .
F2A F 0.28163(14) 0.49643(13) 0.11380(10) 0.0394(3) Uani 1 1 d . . . . .
F3A F 0.11728(13) 0.53937(12) 0.01780(10) 0.0358(3) Uani 1 1 d . . . . .
Cu1X Cu 0.0000 0.5000 0.5000 0.01405(7) Uani 1 2 d S . P . .
N1X N -0.05975(15) 0.70796(14) 0.50257(11) 0.0188(3) Uani 1 1 d . . . . .
C2X C -0.1480(2) 0.73618(18) 0.59938(13) 0.0229(4) Uani 1 1 d . . . . .
H21X H -0.2432 0.7231 0.5964 0.027 Uiso 1 1 calc R U . . .
H22X H -0.1634 0.8294 0.6163 0.027 Uiso 1 1 calc R U . . .
C3X C -0.0689(2) 0.64305(18) 0.67554(13) 0.0250(4) Uani 1 1 d . . . . .
H31X H 0.0229 0.6610 0.6822 0.030 Uiso 1 1 calc R U . . .
H32X H -0.1281 0.6571 0.7389 0.030 Uiso 1 1 calc R U . . .
N4X N -0.04013(17) 0.50486(15) 0.64604(11) 0.0207(3) Uani 1 1 d . . . . .
H41X H -0.125(3) 0.484(2) 0.6601(18) 0.033(6) Uiso 1 1 d . . . . .
C5X C 0.0708(2) 0.40975(18) 0.69984(13) 0.0236(4) Uani 1 1 d . . . . .
H51X H 0.0447 0.4226 0.7703 0.028 Uiso 1 1 calc R U . . .
H52X H 0.1647 0.4265 0.6823 0.028 Uiso 1 1 calc R U . . .
C6X C 0.0835(2) 0.26813(18) 0.67626(13) 0.0241(4) Uani 1 1 d . . . . .
H61X H 0.1405 0.2070 0.7237 0.029 Uiso 1 1 calc R U . . .
H62X H -0.0138 0.2570 0.6835 0.029 Uiso 1 1 calc R U . . .
C7X C 0.1538(2) 0.22947(18) 0.57487(14) 0.0233(4) Uani 1 1 d . . . . .
H71X H 0.2434 0.2553 0.5636 0.028 Uiso 1 1 calc R U . . .
H72X H 0.1806 0.1318 0.5703 0.028 Uiso 1 1 calc R U . . .
C8X C 0.06513(18) 0.76375(16) 0.49814(13) 0.0193(3) Uani 1 1 d . . . . .
H81X H 0.0653 0.8010 0.5617 0.023 Uiso 1 1 calc R U . . .
H82X H 0.0517 0.8373 0.4492 0.023 Uiso 1 1 calc R U . . .
P1X P 0.23984(5) 0.64043(4) 0.46738(3) 0.01700(9) Uani 1 1 d . . . . .
O11X O 0.23655(13) 0.50876(12) 0.51132(10) 0.0223(3) Uani 1 1 d . . . . .
O2X O 0.27424(14) 0.64780(13) 0.35830(9) 0.0241(3) Uani 1 1 d . . . . .
C9X C 0.36909(18) 0.69361(17) 0.52620(12) 0.0188(3) Uani 1 1 d . . . . .
H91X H 0.3295 0.7134 0.5943 0.023 Uiso 1 1 calc R U . . .
H92X H 0.4583 0.6182 0.5273 0.023 Uiso 1 1 calc R U . . .
C10X C 0.40864(19) 0.81168(18) 0.48180(14) 0.0228(4) Uani 1 1 d . . . . .
F1X F 0.29300(13) 0.91514(11) 0.46641(10) 0.0346(3) Uani 1 1 d . . . . .
F2X F 0.48781(13) 0.78501(13) 0.39580(9) 0.0331(3) Uani 1 1 d . . . . .
F3X F 0.48739(13) 0.85483(12) 0.53768(9) 0.0327(3) Uani 1 1 d . . . . .
Cl1 Cl 0.85545(5) 0.09076(4) 0.24111(3) 0.02129(9) Uani 1 1 d . . . . .
O1P O 0.72278(15) 0.06908(14) 0.28507(11) 0.0292(3) Uani 1 1 d . . . . .
O2P O 0.83590(18) 0.23145(14) 0.23357(12) 0.0363(3) Uani 1 1 d . . . . .
O3P O 0.96933(16) 0.02814(15) 0.30032(11) 0.0336(3) Uani 1 1 d . . . . .
O4P O 0.88861(17) 0.03620(17) 0.14591(11) 0.0365(3) Uani 1 1 d . . . . .
O1W O 0.49181(15) 0.52219(14) 0.26154(10) 0.0228(3) Uani 1 1 d . . . . .
H11W H 0.388(4) 0.585(3) 0.311(3) 0.074(10) Uiso 1 1 d . . . . .
H12W H 0.491(3) 0.558(3) 0.212(2) 0.039(7) Uiso 1 1 d . . . . .
H13W H 0.486(3) 0.448(3) 0.254(2) 0.043(8) Uiso 1 1 d . . . . .
O2W O 0.47444(16) 0.28671(14) 0.23720(11) 0.0244(3) Uani 1 1 d . . . . .
H21W H 0.536(3) 0.233(3) 0.2602(19) 0.034(7) Uiso 1 1 d . . . . .
H22W H 0.484(3) 0.271(3) 0.178(2) 0.041(7) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1A N4A 2.0208(14) 2_675 ?
Cu1A N4A 2.0208(14) . ?
Cu1A N1A 2.0680(14) . ?
Cu1A N1A 2.0680(14) 2_675 ?
Cu1A O11A 2.4120(12) 2_675 ?
Cu1A O11A 2.4120(12) . ?
N1A C8A 1.497(2) . ?
N1A C7A 1.498(2) 2_675 ?
N1A C2A 1.498(2) . ?
C2A C3A 1.508(2) . ?
C2A H21A 0.9900 . ?
C2A H22A 0.9900 . ?
C3A N4A 1.487(2) . ?
C3A H31A 0.9900 . ?
C3A H32A 0.9900 . ?
N4A C5A 1.482(2) . ?
N4A H41A 0.90(2) . ?
C5A C6A 1.514(2) . ?
C5A H51A 0.9900 . ?
C5A H52A 0.9900 . ?
C6A C7A 1.517(2) . ?
C6A H61A 0.9900 . ?
C6A H62A 0.9900 . ?
C7A N1A 1.498(2) 2_675 ?
C7A H71A 0.9900 . ?
C7A H72A 0.9900 . ?
C8A P1A 1.8354(18) . ?
C8A H81A 0.9900 . ?
C8A H82A 0.9900 . ?
P1A O12A 1.5043(13) . ?
P1A O11A 1.5095(12) . ?
P1A C9A 1.8234(17) . ?
C9A C10A 1.493(2) . ?
C9A H91A 0.9900 . ?
C9A H92A 0.9900 . ?
C10A F2A 1.332(2) . ?
C10A F3A 1.346(2) . ?
C10A F1A 1.348(2) . ?
Cu1X N4X 2.0239(15) 2_566 ?
Cu1X N4X 2.0239(15) . ?
Cu1X N1X 2.0992(14) . ?
Cu1X N1X 2.0992(14) 2_566 ?
Cu1X O11X 2.3722(12) 2_566 ?
Cu1X O11X 2.3722(12) . ?
N1X C7X 1.491(2) 2_566 ?
N1X C8X 1.506(2) . ?
N1X C2X 1.507(2) . ?
C2X C3X 1.514(3) . ?
C2X H21X 0.9900 . ?
C2X H22X 0.9900 . ?
C3X N4X 1.477(2) . ?
C3X H31X 0.9900 . ?
C3X H32X 0.9900 . ?
N4X C5X 1.479(2) . ?
N4X H41X 0.92(3) . ?
C5X C6X 1.518(3) . ?
C5X H51X 0.9900 . ?
C5X H52X 0.9900 . ?
C6X C7X 1.517(3) . ?
C6X H61X 0.9900 . ?
C6X H62X 0.9900 . ?
C7X N1X 1.491(2) 2_566 ?
C7X H71X 0.9900 . ?
C7X H72X 0.9900 . ?
C8X P1X 1.8324(18) . ?
C8X H81X 0.9900 . ?
C8X H82X 0.9900 . ?
P1X O11X 1.4948(13) . ?
P1X O2X 1.5176(13) . ?
P1X C9X 1.8224(17) . ?
O2X H11W 1.24(4) . ?
C9X C10X 1.495(2) . ?
C9X H91X 0.9900 . ?
C9X H92X 0.9900 . ?
C10X F1X 1.343(2) . ?
C10X F2X 1.343(2) . ?
C10X F3X 1.344(2) . ?
Cl1 O3P 1.4359(15) . ?
Cl1 O4P 1.4388(15) . ?
Cl1 O2P 1.4407(15) . ?
Cl1 O1P 1.4479(14) . ?
O1W H11W 1.20(4) . ?
O1W H12W 0.77(3) . ?
O1W H13W 0.82(3) . ?
O2W H21W 0.78(3) . ?
O2W H22W 0.84(3) . ?

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
N4A Cu1A N4A 180.0 2_675 . ?
N4A Cu1A N1A 93.56(6) 2_675 . ?
N4A Cu1A N1A 86.44(6) . . ?
N4A Cu1A N1A 86.44(6) 2_675 2_675 ?
N4A Cu1A N1A 93.56(6) . 2_675 ?
N1A Cu1A N1A 180.00(8) . 2_675 ?
N4A Cu1A O11A 95.14(5) 2_675 2_675 ?
N4A Cu1A O11A 84.86(5) . 2_675 ?
N1A Cu1A O11A 94.51(5) . 2_675 ?
N1A Cu1A O11A 85.49(5) 2_675 2_675 ?
N4A Cu1A O11A 84.86(5) 2_675 . ?
N4A Cu1A O11A 95.14(5) . . ?
N1A Cu1A O11A 85.49(5) . . ?
N1A Cu1A O11A 94.51(5) 2_675 . ?
O11A Cu1A O11A 180.00(5) 2_675 . ?
C8A N1A C7A 110.08(13) . 2_675 ?
C8A N1A C2A 110.63(13) . . ?
C7A N1A C2A 106.95(13) 2_675 . ?
C8A N1A Cu1A 113.68(10) . . ?
C7A N1A Cu1A 111.55(10) 2_675 . ?
C2A N1A Cu1A 103.57(10) . . ?
N1A C2A C3A 111.14(14) . . ?
N1A C2A H21A 109.4 . . ?
C3A C2A H21A 109.4 . . ?
N1A C2A H22A 109.4 . . ?
C3A C2A H22A 109.4 . . ?
H21A C2A H22A 108.0 . . ?
N4A C3A C2A 109.03(14) . . ?
N4A C3A H31A 109.9 . . ?
C2A C3A H31A 109.9 . . ?
N4A C3A H32A 109.9 . . ?
C2A C3A H32A 109.9 . . ?
H31A C3A H32A 108.3 . . ?
C5A N4A C3A 112.03(13) . . ?
C5A N4A Cu1A 116.36(11) . . ?
C3A N4A Cu1A 109.36(10) . . ?
C5A N4A H41A 107.4(15) . . ?
C3A N4A H41A 105.9(15) . . ?
Cu1A N4A H41A 105.1(15) . . ?
N4A C5A C6A 112.25(14) . . ?
N4A C5A H51A 109.2 . . ?
C6A C5A H51A 109.2 . . ?
N4A C5A H52A 109.2 . . ?
C6A C5A H52A 109.2 . . ?
H51A C5A H52A 107.9 . . ?
C5A C6A C7A 115.27(15) . . ?
C5A C6A H61A 108.5 . . ?
C7A C6A H61A 108.5 . . ?
C5A C6A H62A 108.5 . . ?
C7A C6A H62A 108.5 . . ?
H61A C6A H62A 107.5 . . ?
N1A C7A C6A 115.33(14) 2_675 . ?
N1A C7A H71A 108.4 2_675 . ?
C6A C7A H71A 108.4 . . ?
N1A C7A H72A 108.4 2_675 . ?
C6A C7A H72A 108.4 . . ?
H71A C7A H72A 107.5 . . ?
N1A C8A P1A 115.17(11) . . ?
N1A C8A H81A 108.5 . . ?
P1A C8A H81A 108.5 . . ?
N1A C8A H82A 108.5 . . ?
P1A C8A H82A 108.5 . . ?
H81A C8A H82A 107.5 . . ?
O12A P1A O11A 117.20(7) . . ?
O12A P1A C9A 108.26(7) . . ?
O11A P1A C9A 106.99(8) . . ?
O12A P1A C8A 111.38(8) . . ?
O11A P1A C8A 106.62(7) . . ?
C9A P1A C8A 105.73(8) . . ?
P1A O11A Cu1A 107.07(6) . . ?
C10A C9A P1A 116.00(13) . . ?
C10A C9A H91A 108.3 . . ?
P1A C9A H91A 108.3 . . ?
C10A C9A H92A 108.3 . . ?
P1A C9A H92A 108.3 . . ?
H91A C9A H92A 107.4 . . ?
F2A C10A F3A 105.92(14) . . ?
F2A C10A F1A 106.86(16) . . ?
F3A C10A F1A 105.43(15) . . ?
F2A C10A C9A 114.23(15) . . ?
F3A C10A C9A 112.05(16) . . ?
F1A C10A C9A 111.76(15) . . ?
N4X Cu1X N4X 180.0 2_566 . ?
N4X Cu1X N1X 93.71(6) 2_566 . ?
N4X Cu1X N1X 86.29(6) . . ?
N4X Cu1X N1X 86.29(6) 2_566 2_566 ?
N4X Cu1X N1X 93.71(6) . 2_566 ?
N1X Cu1X N1X 180.0 . 2_566 ?
N4X Cu1X O11X 90.11(6) 2_566 2_566 ?
N4X Cu1X O11X 89.89(6) . 2_566 ?
N1X Cu1X O11X 94.66(5) . 2_566 ?
N1X Cu1X O11X 85.34(5) 2_566 2_566 ?
N4X Cu1X O11X 89.89(6) 2_566 . ?
N4X Cu1X O11X 90.11(6) . . ?
N1X Cu1X O11X 85.34(5) . . ?
N1X Cu1X O11X 94.66(5) 2_566 . ?
O11X Cu1X O11X 180.00(6) 2_566 . ?
C7X N1X C8X 110.29(13) 2_566 . ?
C7X N1X C2X 108.54(14) 2_566 . ?
C8X N1X C2X 109.68(13) . . ?
C7X N1X Cu1X 111.60(11) 2_566 . ?
C8X N1X Cu1X 114.18(10) . . ?
C2X N1X Cu1X 102.14(10) . . ?
N1X C2X C3X 109.04(14) . . ?
N1X C2X H21X 109.9 . . ?
C3X C2X H21X 109.9 . . ?
N1X C2X H22X 109.9 . . ?
C3X C2X H22X 109.9 . . ?
H21X C2X H22X 108.3 . . ?
N4X C3X C2X 108.91(14) . . ?
N4X C3X H31X 109.9 . . ?
C2X C3X H31X 109.9 . . ?
N4X C3X H32X 109.9 . . ?
C2X C3X H32X 109.9 . . ?
H31X C3X H32X 108.3 . . ?
C3X N4X C5X 112.43(14) . . ?
C3X N4X Cu1X 108.25(11) . . ?
C5X N4X Cu1X 115.29(11) . . ?
C3X N4X H41X 106.7(15) . . ?
C5X N4X H41X 108.3(15) . . ?
Cu1X N4X H41X 105.3(15) . . ?
N4X C5X C6X 110.52(15) . . ?
N4X C5X H51X 109.5 . . ?
C6X C5X H51X 109.5 . . ?
N4X C5X H52X 109.5 . . ?
C6X C5X H52X 109.5 . . ?
H51X C5X H52X 108.1 . . ?
C7X C6X C5X 113.60(15) . . ?
C7X C6X H61X 108.8 . . ?
C5X C6X H61X 108.8 . . ?
C7X C6X H62X 108.8 . . ?
C5X C6X H62X 108.8 . . ?
H61X C6X H62X 107.7 . . ?
N1X C7X C6X 113.47(15) 2_566 . ?
N1X C7X H71X 108.9 2_566 . ?
C6X C7X H71X 108.9 . . ?
N1X C7X H72X 108.9 2_566 . ?
C6X C7X H72X 108.9 . . ?
H71X C7X H72X 107.7 . . ?
N1X C8X P1X 113.29(11) . . ?
N1X C8X H81X 108.9 . . ?
P1X C8X H81X 108.9 . . ?
N1X C8X H82X 108.9 . . ?
P1X C8X H82X 108.9 . . ?
H81X C8X H82X 107.7 . . ?
O11X P1X O2X 116.98(8) . . ?
O11X P1X C9X 107.68(8) . . ?
O2X P1X C9X 109.47(8) . . ?
O11X P1X C8X 109.19(8) . . ?
O2X P1X C8X 107.37(8) . . ?
C9X P1X C8X 105.59(8) . . ?
P1X O11X Cu1X 105.28(6) . . ?
P1X O2X H11W 126.0(16) . . ?
C10X C9X P1X 116.65(12) . . ?
C10X C9X H91X 108.1 . . ?
P1X C9X H91X 108.1 . . ?
C10X C9X H92X 108.1 . . ?
P1X C9X H92X 108.1 . . ?
H91X C9X H92X 107.3 . . ?
F1X C10X F2X 106.58(15) . . ?
F1X C10X F3X 106.70(15) . . ?
F2X C10X F3X 106.13(14) . . ?
F1X C10X C9X 112.65(15) . . ?
F2X C10X C9X 112.18(15) . . ?
F3X C10X C9X 112.15(15) . . ?
O3P Cl1 O4P 110.47(10) . . ?
O3P Cl1 O2P 109.68(9) . . ?
O4P Cl1 O2P 109.51(10) . . ?
O3P Cl1 O1P 109.50(9) . . ?
O4P Cl1 O1P 108.87(9) . . ?
O2P Cl1 O1P 108.79(9) . . ?
H11W O1W H12W 107(3) . . ?
H11W O1W H13W 110(2) . . ?
H12W O1W H13W 108(3) . . ?
H21W O2W H22W 106(3) . . ?

_refine_diff_density_max         0.703
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.060



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

data_cute2pf
_database_code_depnum_ccdc_archive 'CCDC 2262043'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2023-05-10 deposited with the CCDC.	2023-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C16 H30 Cu F6 N4 O4 P2, 0.46(Br), 0.54(Cl), H4 N
;
_chemical_formula_sum            'C16 H34 Br0.46 Cl0.54 Cu F6 N5 O4 P2'
_chemical_formula_weight         655.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   15.9852(6)
_cell_length_b                   12.6453(5)
_cell_length_c                   12.6956(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.1106(12)
_cell_angle_gamma                90
_cell_volume                     2509.15(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9427
_cell_measurement_theta_min      2.4673
_cell_measurement_theta_max      27.4943

_exptl_crystal_description       prism
_exptl_crystal_colour            'light violet-blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_F_000             1341
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.052
_exptl_absorpt_coefficient_mu    1.867
_shelx_estimated_absorpt_T_min   0.752
_shelx_estimated_absorpt_T_max   0.909
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            32090
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.467
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2907
_reflns_number_gt                2734
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Instrument Service vV6.2.1'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XS, VERSION 2013/1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 758)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0274P)²+4.0368P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2907
_refine_ls_number_parameters     170
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0250
_refine_ls_wR_factor_ref         0.0660
_refine_ls_wR_factor_gt          0.0648
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_restrained_S_all      1.164
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.2500 0.2500 0.0000 0.01293(8) Uani 1 2 d S . P . .
N1 N 0.19229(9) 0.32104(10) 0.11320(10) 0.0152(3) Uani 1 1 d . . . . .
C2 C 0.24877(11) 0.28916(14) 0.21729(12) 0.0184(3) Uani 1 1 d . . . . .
H21 H 0.2197 0.3042 0.2773 0.022 Uiso 1 1 calc R U . . .
H22 H 0.3024 0.3308 0.2292 0.022 Uiso 1 1 calc R U . . .
C3 C 0.26942(11) 0.17249(13) 0.21573(13) 0.0184(3) Uani 1 1 d . . . . .
H31 H 0.3120 0.1531 0.2814 0.022 Uiso 1 1 calc R U . . .
H32 H 0.2171 0.1300 0.2136 0.022 Uiso 1 1 calc R U . . .
N4 N 0.30443(10) 0.15138(11) 0.11845(11) 0.0163(3) Uani 1 1 d . . . . .
H4 H 0.3577(14) 0.1691(17) 0.1325(17) 0.020 Uiso 1 1 d . U . . .
C5 C 0.30325(12) 0.03711(13) 0.09242(14) 0.0226(4) Uani 1 1 d . . . . .
H51 H 0.2432 0.0127 0.0714 0.027 Uiso 1 1 calc R U . . .
H52 H 0.3312 -0.0029 0.1573 0.027 Uiso 1 1 calc R U . . .
C6 C 0.34908(13) 0.01440(14) 0.00144(14) 0.0246(4) Uani 1 1 d . . . . .
H61 H 0.4081 0.0425 0.0219 0.030 Uiso 1 1 calc R U . . .
H62 H 0.3533 -0.0632 -0.0064 0.030 Uiso 1 1 calc R U . . .
C7 C 0.30680(12) 0.06075(13) -0.10695(13) 0.0211(3) Uani 1 1 d . . . . .
H71 H 0.3359 0.0321 -0.1624 0.025 Uiso 1 1 calc R U . . .
H72 H 0.2466 0.0365 -0.1250 0.025 Uiso 1 1 calc R U . . .
C8 C 0.10271(11) 0.28369(13) 0.10692(13) 0.0181(3) Uani 1 1 d . . . . .
H81 H 0.0633 0.3373 0.0670 0.022 Uiso 1 1 calc R U . . .
H82 H 0.0924 0.2806 0.1811 0.022 Uiso 1 1 calc R U . . .
P1 P 0.07429(3) 0.15400(3) 0.04261(3) 0.01460(10) Uani 1 1 d . . . . .
O11 O 0.12017(8) 0.14494(9) -0.04916(9) 0.0185(2) Uani 1 1 d . . . . .
O12 O 0.08450(7) 0.06707(9) 0.12455(9) 0.0189(2) Uani 1 1 d . . . . .
C9 C -0.03913(11) 0.16867(14) -0.01888(13) 0.0191(3) Uani 1 1 d . . . . .
H91 H -0.0448 0.2284 -0.0703 0.023 Uiso 1 1 calc R U . . .
H92 H -0.0576 0.1040 -0.0614 0.023 Uiso 1 1 calc R U . . .
C10 C -0.10020(11) 0.18708(15) 0.05319(15) 0.0227(4) Uani 1 1 d . . . . .
F1 F -0.08389(9) 0.27603(10) 0.11189(11) 0.0385(3) Uani 1 1 d . . . . .
F2 F -0.10297(8) 0.10929(10) 0.12305(11) 0.0396(3) Uani 1 1 d . . . . .
F3 F -0.18076(8) 0.19772(13) -0.00357(11) 0.0463(4) Uani 1 1 d . . . . .
N1A N 0.0000 -0.05519(17) 0.2500 0.0213(4) Uani 1 2 d S T P . .
H11A H -0.0316(14) -0.0110(18) 0.2882(17) 0.026 Uiso 1 1 d . U . . .
H12A H 0.0375(14) -0.1025(18) 0.2944(17) 0.026 Uiso 1 1 d . U . . .
Br1 Br 0.0000 0.34870(5) -0.2500 0.04487(14) Uani 0.46 2 d S T P . .
Cl1 Cl 0.0000 0.34870(5) -0.2500 0.04487(14) Uani 0.54 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 2.0062(14) 7 ?
Cu1 N4 2.0062(14) . ?
Cu1 N1 2.0687(13) . ?
Cu1 N1 2.0687(13) 7 ?
Cu1 O11 2.4326(12) 7 ?
Cu1 O11 2.4326(12) . ?
N1 C2 1.491(2) . ?
N1 C8 1.494(2) . ?
N1 C7 1.497(2) 7 ?
C2 C3 1.513(2) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.483(2) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C5 1.482(2) . ?
N4 H4 0.86(2) . ?
C5 C6 1.519(2) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 C7 1.518(2) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
C7 N1 1.497(2) 7 ?
C7 H71 0.9900 . ?
C7 H72 0.9900 . ?
C8 P1 1.8457(17) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
P1 O12 1.4986(12) . ?
P1 O11 1.5056(12) . ?
P1 C9 1.8268(17) . ?
C9 C10 1.490(2) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
C10 F2 1.331(2) . ?
C10 F3 1.344(2) . ?
C10 F1 1.344(2) . ?
N1A H11A 0.95(2) . ?
N1A H12A 0.94(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cu1 N4 180.00(8) 7 . ?
N4 Cu1 N1 93.68(5) 7 . ?
N4 Cu1 N1 86.32(5) . . ?
N4 Cu1 N1 86.32(5) 7 7 ?
N4 Cu1 N1 93.68(5) . 7 ?
N1 Cu1 N1 180.00(5) . 7 ?
N4 Cu1 O11 93.75(5) 7 7 ?
N4 Cu1 O11 86.25(5) . 7 ?
N1 Cu1 O11 93.75(5) . 7 ?
N1 Cu1 O11 86.25(5) 7 7 ?
N4 Cu1 O11 86.25(5) 7 . ?
N4 Cu1 O11 93.75(5) . . ?
N1 Cu1 O11 86.25(5) . . ?
N1 Cu1 O11 93.75(5) 7 . ?
O11 Cu1 O11 180.00(5) 7 . ?
C2 N1 C8 110.92(13) . . ?
C2 N1 C7 107.82(13) . 7 ?
C8 N1 C7 109.44(13) . 7 ?
C2 N1 Cu1 102.88(10) . . ?
C8 N1 Cu1 112.82(10) . . ?
C7 N1 Cu1 112.71(10) 7 . ?
N1 C2 C3 110.19(13) . . ?
N1 C2 H21 109.6 . . ?
C3 C2 H21 109.6 . . ?
N1 C2 H22 109.6 . . ?
C3 C2 H22 109.6 . . ?
H21 C2 H22 108.1 . . ?
N4 C3 C2 107.94(13) . . ?
N4 C3 H31 110.1 . . ?
C2 C3 H31 110.1 . . ?
N4 C3 H32 110.1 . . ?
C2 C3 H32 110.1 . . ?
H31 C3 H32 108.4 . . ?
C5 N4 C3 111.83(13) . . ?
C5 N4 Cu1 117.12(11) . . ?
C3 N4 Cu1 109.40(10) . . ?
C5 N4 H4 105.4(14) . . ?
C3 N4 H4 108.0(14) . . ?
Cu1 N4 H4 104.3(14) . . ?
N4 C5 C6 111.61(14) . . ?
N4 C5 H51 109.3 . . ?
C6 C5 H51 109.3 . . ?
N4 C5 H52 109.3 . . ?
C6 C5 H52 109.3 . . ?
H51 C5 H52 108.0 . . ?
C7 C6 C5 114.98(16) . . ?
C7 C6 H61 108.5 . . ?
C5 C6 H61 108.5 . . ?
C7 C6 H62 108.5 . . ?
C5 C6 H62 108.5 . . ?
H61 C6 H62 107.5 . . ?
N1 C7 C6 115.22(14) 7 . ?
N1 C7 H71 108.5 7 . ?
C6 C7 H71 108.5 . . ?
N1 C7 H72 108.5 7 . ?
C6 C7 H72 108.5 . . ?
H71 C7 H72 107.5 . . ?
N1 C8 P1 116.66(11) . . ?
N1 C8 H81 108.1 . . ?
P1 C8 H81 108.1 . . ?
N1 C8 H82 108.1 . . ?
P1 C8 H82 108.1 . . ?
H81 C8 H82 107.3 . . ?
O12 P1 O11 118.79(7) . . ?
O12 P1 C9 108.96(7) . . ?
O11 P1 C9 106.14(7) . . ?
O12 P1 C8 111.33(7) . . ?
O11 P1 C8 107.17(7) . . ?
C9 P1 C8 103.23(8) . . ?
P1 O11 Cu1 106.73(6) . . ?
C10 C9 P1 118.23(12) . . ?
C10 C9 H91 107.8 . . ?
P1 C9 H91 107.8 . . ?
C10 C9 H92 107.8 . . ?
P1 C9 H92 107.8 . . ?
H91 C9 H92 107.1 . . ?
F2 C10 F3 105.61(16) . . ?
F2 C10 F1 106.17(15) . . ?
F3 C10 F1 105.43(15) . . ?
F2 C10 C9 114.29(15) . . ?
F3 C10 C9 111.35(15) . . ?
F1 C10 C9 113.29(15) . . ?
H11A N1A H12A 114.0(18) . . ?

_refine_diff_density_max         0.469
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.062



####################################################################### 
# 
# 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_nite2pf_sq
_database_code_depnum_ccdc_archive 'CCDC 2262040'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2023-05-10 deposited with the CCDC.	2023-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H30 F6 N4 Ni O4 P2, 3.5(H2 O)'
_chemical_formula_sum            'C16 H37 F6 N4 Ni O7.50 P2'
_chemical_formula_weight         640.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.6825(3)
_cell_length_b                   13.4090(4)
_cell_length_c                   20.7058(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.3180(10)
_cell_angle_gamma                90
_cell_volume                     2686.09(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9983
_cell_measurement_theta_min      2.5961
_cell_measurement_theta_max      27.5017

_exptl_crystal_description       prism
_exptl_crystal_colour            'light blue-violet'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_F_000             1332
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          1.081
_exptl_crystal_size_mid          0.558
_exptl_crystal_size_min          0.320
_exptl_absorpt_coefficient_mu    0.927
_shelx_estimated_absorpt_T_min   0.434
_shelx_estimated_absorpt_T_max   0.756
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_T_max  0.76

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            20124
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.810
_diffrn_reflns_theta_max         27.527
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6178
_reflns_number_gt                5583
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Instrument Service v2016.1.0.1'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 758)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0278P)²+1.3384P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6178
_refine_ls_number_parameters     323
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0241
_refine_ls_wR_factor_ref         0.0608
_refine_ls_wR_factor_gt          0.0592
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ni1 Ni 0.25434(2) 0.37002(2) 0.34085(2) 0.01178(5) Uani 1 1 d . . . . .
N1 N 0.44491(11) 0.35456(8) 0.29163(5) 0.0149(2) Uani 1 1 d . . . . .
C2 C 0.40405(14) 0.36196(12) 0.22188(6) 0.0213(3) Uani 1 1 d . . . . .
H21 H 0.4756 0.3298 0.1961 0.026 Uiso 1 1 calc R U . . .
H22 H 0.3987 0.4331 0.2093 0.026 Uiso 1 1 calc R U . . .
C3 C 0.26616(14) 0.31277(11) 0.20674(6) 0.0192(3) Uani 1 1 d . . . . .
H31 H 0.2393 0.3220 0.1605 0.023 Uiso 1 1 calc R U . . .
H32 H 0.2726 0.2403 0.2156 0.023 Uiso 1 1 calc R U . . .
N4 N 0.16158(11) 0.35847(9) 0.24747(5) 0.0154(2) Uani 1 1 d . . . . .
H41 H 0.1472(17) 0.4188(14) 0.2328(8) 0.020(4) Uiso 1 1 d . . . . .
C5 C 0.03214(14) 0.30025(11) 0.24246(7) 0.0194(3) Uani 1 1 d . . . . .
H51 H 0.0504 0.2316 0.2583 0.023 Uiso 1 1 calc R U . . .
H52 H 0.0004 0.2959 0.1965 0.023 Uiso 1 1 calc R U . . .
C6 C -0.08145(14) 0.34642(12) 0.28115(7) 0.0229(3) Uani 1 1 d . . . . .
H61 H -0.1705 0.3148 0.2678 0.027 Uiso 1 1 calc R U . . .
H62 H -0.0884 0.4182 0.2702 0.027 Uiso 1 1 calc R U . . .
C7 C -0.06002(13) 0.33616(12) 0.35413(7) 0.0219(3) Uani 1 1 d . . . . .
H71 H -0.1449 0.3593 0.3746 0.026 Uiso 1 1 calc R U . . .
H72 H -0.0484 0.2645 0.3646 0.026 Uiso 1 1 calc R U . . .
N8 N 0.06054(11) 0.39190(8) 0.38379(5) 0.0155(2) Uani 1 1 d . . . . .
C9 C 0.03443(14) 0.50121(11) 0.37808(7) 0.0193(3) Uani 1 1 d . . . . .
H91 H -0.0327 0.5216 0.4104 0.023 Uiso 1 1 calc R U . . .
H92 H -0.0066 0.5161 0.3346 0.023 Uiso 1 1 calc R U . . .
C10 C 0.16660(14) 0.56055(10) 0.38870(6) 0.0184(3) Uani 1 1 d . . . . .
H101 H 0.1479 0.6324 0.3817 0.022 Uiso 1 1 calc R U . . .
H102 H 0.2036 0.5513 0.4336 0.022 Uiso 1 1 calc R U . . .
N11 N 0.26819(11) 0.52504(9) 0.34257(5) 0.0151(2) Uani 1 1 d . . . . .
H111 H 0.2397(17) 0.5451(13) 0.3050(8) 0.021(4) Uiso 1 1 d . . . . .
C12 C 0.40771(14) 0.56637(10) 0.35748(7) 0.0190(3) Uani 1 1 d . . . . .
H121 H 0.4430 0.5404 0.3998 0.023 Uiso 1 1 calc R U . . .
H122 H 0.4018 0.6399 0.3607 0.023 Uiso 1 1 calc R U . . .
C13 C 0.50749(14) 0.53864(11) 0.30570(7) 0.0221(3) Uani 1 1 d . . . . .
H131 H 0.5901 0.5819 0.3107 0.027 Uiso 1 1 calc R U . . .
H132 H 0.4628 0.5530 0.2629 0.027 Uiso 1 1 calc R U . . .
C14 C 0.55467(13) 0.43038(11) 0.30663(7) 0.0199(3) Uani 1 1 d . . . . .
H141 H 0.6280 0.4227 0.2750 0.024 Uiso 1 1 calc R U . . .
H142 H 0.5966 0.4156 0.3500 0.024 Uiso 1 1 calc R U . . .
C15 C 0.50309(14) 0.25411(11) 0.30757(7) 0.0204(3) Uani 1 1 d . . . . .
H151 H 0.5721 0.2613 0.3439 0.025 Uiso 1 1 calc R U . . .
H152 H 0.5523 0.2293 0.2698 0.025 Uiso 1 1 calc R U . . .
P1 P 0.37477(3) 0.15990(3) 0.32982(2) 0.01525(8) Uani 1 1 d . . . . .
O11 O 0.24675(9) 0.21607(7) 0.34802(5) 0.0187(2) Uani 1 1 d . . . . .
O12 O 0.36120(10) 0.07930(7) 0.28013(5) 0.0221(2) Uani 1 1 d . . . . .
C16 C 0.44780(15) 0.10548(11) 0.40457(7) 0.0221(3) Uani 1 1 d . . . . .
H161 H 0.4776 0.1605 0.4338 0.027 Uiso 1 1 calc R U . . .
H162 H 0.3736 0.0687 0.4259 0.027 Uiso 1 1 calc R U . . .
C17 C 0.56733(17) 0.03642(12) 0.39755(7) 0.0281(3) Uani 1 1 d . . . . .
F1 F 0.66710(11) 0.07596(10) 0.36312(6) 0.0539(3) Uani 1 1 d . . . . .
F2 F 0.53142(13) -0.04874(8) 0.36865(6) 0.0571(4) Uani 1 1 d . . . . .
F3 F 0.62761(11) 0.01059(9) 0.45466(5) 0.0438(3) Uani 1 1 d . . . . .
C18 C 0.07331(14) 0.36038(11) 0.45285(6) 0.0193(3) Uani 1 1 d . . . . .
H181 H 0.0447 0.2897 0.4558 0.023 Uiso 1 1 calc R U . . .
H182 H 0.0084 0.4005 0.4779 0.023 Uiso 1 1 calc R U . . .
P2 P 0.24771(3) 0.37338(3) 0.49038(2) 0.01615(8) Uani 1 1 d . . . . .
O21 O 0.34599(9) 0.36948(7) 0.43523(4) 0.0178(2) Uani 1 1 d . . . . .
O22 O 0.25692(10) 0.45824(8) 0.53669(5) 0.0239(2) Uani 1 1 d . . . . .
C19 C 0.27595(14) 0.25674(11) 0.53514(7) 0.0222(3) Uani 1 1 d . . . . .
H191 H 0.2581 0.2006 0.5049 0.027 Uiso 1 1 calc R U . . .
H192 H 0.3747 0.2535 0.5494 0.027 Uiso 1 1 calc R U . . .
C20 C 0.19087(15) 0.24100(12) 0.59293(7) 0.0240(3) Uani 1 1 d . . . . .
F4 F 0.05540(9) 0.25407(8) 0.57950(5) 0.0370(2) Uani 1 1 d . . . . .
F5 F 0.22194(13) 0.30214(10) 0.64184(5) 0.0530(3) Uani 1 1 d . . . . .
F6 F 0.20226(12) 0.14846(8) 0.61682(6) 0.0467(3) Uani 1 1 d . . . . .
O1W O 0.62885(13) 0.35477(10) 0.46285(6) 0.0328(3) Uani 1 1 d D . . . .
H11W H 0.660(2) 0.4083(19) 0.4671(11) 0.051(7) Uiso 1 1 d . . . . .
H12W H 0.5457(17) 0.3649(16) 0.4592(10) 0.046(6) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O11 2.0712(10) . ?
Ni1 N11 2.0832(12) . ?
Ni1 N4 2.1044(11) . ?
Ni1 O21 2.1134(9) . ?
Ni1 N8 2.1291(11) . ?
Ni1 N1 2.1537(11) . ?
N1 C2 1.4852(17) . ?
N1 C15 1.4918(17) . ?
N1 C14 1.4943(17) . ?
C2 C3 1.5107(19) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.4769(17) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C5 1.4767(17) . ?
N4 H41 0.873(18) . ?
C5 C6 1.5184(19) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 C7 1.523(2) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
C7 N8 1.4968(17) . ?
C7 H71 0.9900 . ?
C7 H72 0.9900 . ?
N8 C18 1.4913(17) . ?
N8 C9 1.4913(18) . ?
C9 C10 1.515(2) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
C10 N11 1.4774(17) . ?
C10 H101 0.9900 . ?
C10 H102 0.9900 . ?
N11 C12 1.4811(17) . ?
N11 H111 0.858(17) . ?
C12 C13 1.518(2) . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C13 C14 1.522(2) . ?
C13 H131 0.9900 . ?
C13 H132 0.9900 . ?
C14 H141 0.9900 . ?
C14 H142 0.9900 . ?
C15 P1 1.8433(14) . ?
C15 H151 0.9900 . ?
C15 H152 0.9900 . ?
P1 O12 1.4944(10) . ?
P1 O11 1.5111(10) . ?
P1 C16 1.8275(14) . ?
C16 C17 1.494(2) . ?
C16 H161 0.9900 . ?
C16 H162 0.9900 . ?
C17 F2 1.3290(19) . ?
C17 F1 1.333(2) . ?
C17 F3 1.3427(17) . ?
C18 P2 1.8384(14) . ?
C18 H181 0.9900 . ?
C18 H182 0.9900 . ?
P2 O22 1.4884(11) . ?
P2 O21 1.5167(10) . ?
P2 C19 1.8328(15) . ?
C19 C20 1.4949(19) . ?
C19 H191 0.9900 . ?
C19 H192 0.9900 . ?
C20 F5 1.3279(19) . ?
C20 F6 1.3387(18) . ?
C20 F4 1.3413(17) . ?
O1W H11W 0.78(2) . ?
O1W H12W 0.817(16) . ?

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
O11 Ni1 N11 174.71(4) . . ?
O11 Ni1 N4 88.71(4) . . ?
N11 Ni1 N4 96.54(4) . . ?
O11 Ni1 O21 86.85(4) . . ?
N11 Ni1 O21 87.89(4) . . ?
N4 Ni1 O21 175.56(4) . . ?
O11 Ni1 N8 94.18(4) . . ?
N11 Ni1 N8 84.99(4) . . ?
N4 Ni1 N8 92.48(4) . . ?
O21 Ni1 N8 87.62(4) . . ?
O11 Ni1 N1 88.37(4) . . ?
N11 Ni1 N1 92.77(4) . . ?
N4 Ni1 N1 84.27(4) . . ?
O21 Ni1 N1 95.83(4) . . ?
N8 Ni1 N1 175.83(4) . . ?
C2 N1 C15 111.03(11) . . ?
C2 N1 C14 108.41(10) . . ?
C15 N1 C14 108.02(10) . . ?
C2 N1 Ni1 104.72(8) . . ?
C15 N1 Ni1 107.78(8) . . ?
C14 N1 Ni1 116.86(8) . . ?
N1 C2 C3 111.79(11) . . ?
N1 C2 H21 109.3 . . ?
C3 C2 H21 109.3 . . ?
N1 C2 H22 109.3 . . ?
C3 C2 H22 109.3 . . ?
H21 C2 H22 107.9 . . ?
N4 C3 C2 108.72(11) . . ?
N4 C3 H31 109.9 . . ?
C2 C3 H31 109.9 . . ?
N4 C3 H32 109.9 . . ?
C2 C3 H32 109.9 . . ?
H31 C3 H32 108.3 . . ?
C5 N4 C3 109.88(10) . . ?
C5 N4 Ni1 115.65(8) . . ?
C3 N4 Ni1 106.15(8) . . ?
C5 N4 H41 110.0(11) . . ?
C3 N4 H41 106.8(11) . . ?
Ni1 N4 H41 108.0(11) . . ?
N4 C5 C6 112.22(11) . . ?
N4 C5 H51 109.2 . . ?
C6 C5 H51 109.2 . . ?
N4 C5 H52 109.2 . . ?
C6 C5 H52 109.2 . . ?
H51 C5 H52 107.9 . . ?
C5 C6 C7 114.46(11) . . ?
C5 C6 H61 108.6 . . ?
C7 C6 H61 108.6 . . ?
C5 C6 H62 108.6 . . ?
C7 C6 H62 108.6 . . ?
H61 C6 H62 107.6 . . ?
N8 C7 C6 115.76(12) . . ?
N8 C7 H71 108.3 . . ?
C6 C7 H71 108.3 . . ?
N8 C7 H72 108.3 . . ?
C6 C7 H72 108.3 . . ?
H71 C7 H72 107.4 . . ?
C18 N8 C9 111.21(10) . . ?
C18 N8 C7 106.56(10) . . ?
C9 N8 C7 109.35(11) . . ?
C18 N8 Ni1 108.73(8) . . ?
C9 N8 Ni1 104.58(8) . . ?
C7 N8 Ni1 116.47(8) . . ?
N8 C9 C10 111.42(11) . . ?
N8 C9 H91 109.3 . . ?
C10 C9 H91 109.3 . . ?
N8 C9 H92 109.3 . . ?
C10 C9 H92 109.3 . . ?
H91 C9 H92 108.0 . . ?
N11 C10 C9 108.51(11) . . ?
N11 C10 H101 110.0 . . ?
C9 C10 H101 110.0 . . ?
N11 C10 H102 110.0 . . ?
C9 C10 H102 110.0 . . ?
H101 C10 H102 108.4 . . ?
C10 N11 C12 111.73(10) . . ?
C10 N11 Ni1 106.77(8) . . ?
C12 N11 Ni1 115.75(8) . . ?
C10 N11 H111 106.7(11) . . ?
C12 N11 H111 109.2(11) . . ?
Ni1 N11 H111 106.2(11) . . ?
N11 C12 C13 111.24(11) . . ?
N11 C12 H121 109.4 . . ?
C13 C12 H121 109.4 . . ?
N11 C12 H122 109.4 . . ?
C13 C12 H122 109.4 . . ?
H121 C12 H122 108.0 . . ?
C12 C13 C14 115.09(12) . . ?
C12 C13 H131 108.5 . . ?
C14 C13 H131 108.5 . . ?
C12 C13 H132 108.5 . . ?
C14 C13 H132 108.5 . . ?
H131 C13 H132 107.5 . . ?
N1 C14 C13 115.84(11) . . ?
N1 C14 H141 108.3 . . ?
C13 C14 H141 108.3 . . ?
N1 C14 H142 108.3 . . ?
C13 C14 H142 108.3 . . ?
H141 C14 H142 107.4 . . ?
N1 C15 P1 114.94(9) . . ?
N1 C15 H151 108.5 . . ?
P1 C15 H151 108.5 . . ?
N1 C15 H152 108.5 . . ?
P1 C15 H152 108.5 . . ?
H151 C15 H152 107.5 . . ?
O12 P1 O11 118.82(6) . . ?
O12 P1 C16 108.33(6) . . ?
O11 P1 C16 106.32(6) . . ?
O12 P1 C15 111.41(6) . . ?
O11 P1 C15 106.79(6) . . ?
C16 P1 C15 104.10(7) . . ?
P1 O11 Ni1 116.55(5) . . ?
C17 C16 P1 116.10(10) . . ?
C17 C16 H161 108.3 . . ?
P1 C16 H161 108.3 . . ?
C17 C16 H162 108.3 . . ?
P1 C16 H162 108.3 . . ?
H161 C16 H162 107.4 . . ?
F2 C17 F1 106.43(14) . . ?
F2 C17 F3 105.75(13) . . ?
F1 C17 F3 105.95(13) . . ?
F2 C17 C16 112.75(13) . . ?
F1 C17 C16 112.73(13) . . ?
F3 C17 C16 112.66(13) . . ?
N8 C18 P2 114.68(9) . . ?
N8 C18 H181 108.6 . . ?
P2 C18 H181 108.6 . . ?
N8 C18 H182 108.6 . . ?
P2 C18 H182 108.6 . . ?
H181 C18 H182 107.6 . . ?
O22 P2 O21 119.23(6) . . ?
O22 P2 C19 108.83(7) . . ?
O21 P2 C19 105.43(6) . . ?
O22 P2 C18 112.02(6) . . ?
O21 P2 C18 105.78(6) . . ?
C19 P2 C18 104.39(7) . . ?
P2 O21 Ni1 116.32(5) . . ?
C20 C19 P2 116.71(10) . . ?
C20 C19 H191 108.1 . . ?
P2 C19 H191 108.1 . . ?
C20 C19 H192 108.1 . . ?
P2 C19 H192 108.1 . . ?
H191 C19 H192 107.3 . . ?
F5 C20 F6 106.13(13) . . ?
F5 C20 F4 105.48(13) . . ?
F6 C20 F4 105.24(12) . . ?
F5 C20 C19 114.09(13) . . ?
F6 C20 C19 112.75(13) . . ?
F4 C20 C19 112.43(12) . . ?
H11W O1W H12W 104(2) . . ?

_refine_diff_density_max         0.340
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.048




####################################################################### 
# 
# 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_2p6f_hcl
_database_code_depnum_ccdc_archive 'CCDC 2262045'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2023-05-10 deposited with the CCDC.	2023-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H34 F6 N4 O4 P2, 2(Cl), 4(H2 O)'
_chemical_formula_sum            'C16 H42 Cl2 F6 N4 O8 P2'
_chemical_formula_weight         665.37

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'
F F 0.0727 0.0534 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.5425(4)
_cell_length_b                   9.9805(5)
_cell_length_c                   11.3345(5)
_cell_angle_alpha                71.9230(10)
_cell_angle_beta                 72.7220(10)
_cell_angle_gamma                69.5340(10)
_cell_volume                     742.71(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9906
_cell_measurement_theta_min      4.1981
_cell_measurement_theta_max      72.1076

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_F_000             348
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.671
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.032
_exptl_absorpt_coefficient_mu    3.745
_shelx_estimated_absorpt_T_min   0.188
_shelx_estimated_absorpt_T_max   0.890
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            14930
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.198
_diffrn_reflns_theta_max         72.101
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             2900
_reflns_number_gt                2854
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Instrument Service vV6.2.15'
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 994)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0362P)²+0.3717P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2900
_refine_ls_number_parameters     200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_ref         0.0701
_refine_ls_wR_factor_gt          0.0698
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
N1 N 0.49045(14) 0.66165(11) 0.61175(10) 0.0116(2) Uani 1 1 d . . . . .
H1 H 0.468(2) 0.6257(18) 0.5594(16) 0.016(4) Uiso 1 1 d . . . . .
C2 C 0.67913(17) 0.69897(13) 0.55196(12) 0.0137(2) Uani 1 1 d . . . . .
H21 H 0.7827 0.6091 0.5348 0.016 Uiso 1 1 calc R U . . .
H22 H 0.7135 0.7347 0.6121 0.016 Uiso 1 1 calc R U . . .
C3 C 0.66779(18) 0.81596(15) 0.42849(13) 0.0189(3) Uani 1 1 d . . . . .
H31 H 0.6602 0.7738 0.3623 0.023 Uiso 1 1 calc R U . . .
H32 H 0.5494 0.8985 0.4414 0.023 Uiso 1 1 calc R U . . .
N4 N 0.84157(15) 0.87103(12) 0.38583(10) 0.0122(2) Uani 1 1 d . . . . .
H41 H 0.945(3) 0.792(2) 0.3688(18) 0.030(5) Uiso 1 1 d . . . . .
H42 H 0.853(2) 0.9007(19) 0.4465(17) 0.021(4) Uiso 1 1 d . . . . .
C5 C 0.83860(17) 0.98993(13) 0.26539(11) 0.0133(2) Uani 1 1 d . . . . .
H51 H 0.8294 0.9509 0.1977 0.016 Uiso 1 1 calc R U . . .
H52 H 0.9628 1.0149 0.2390 0.016 Uiso 1 1 calc R U . . .
C6 C 0.67326(17) 1.13008(13) 0.27623(12) 0.0135(2) Uani 1 1 d . . . . .
H61 H 0.6744 1.1977 0.1912 0.016 Uiso 1 1 calc R U . . .
H62 H 0.5488 1.1052 0.3048 0.016 Uiso 1 1 calc R U . . .
C7 C 0.68509(17) 1.20860(13) 0.36795(11) 0.0123(2) Uani 1 1 d . . . . .
H71 H 0.6979 1.1381 0.4507 0.015 Uiso 1 1 calc R U . . .
H72 H 0.8025 1.2432 0.3345 0.015 Uiso 1 1 calc R U . . .
C8 C 0.50795(18) 0.54522(13) 0.73271(11) 0.0138(2) Uani 1 1 d . . . . .
H81 H 0.3776 0.5374 0.7810 0.017 Uiso 1 1 calc R U . . .
H82 H 0.5664 0.5730 0.7858 0.017 Uiso 1 1 calc R U . . .
P1 P 0.65920(4) 0.36658(3) 0.69763(3) 0.01174(10) Uani 1 1 d . . . . .
O11 O 0.86495(12) 0.34366(10) 0.70323(8) 0.01604(19) Uani 1 1 d . . . . .
O12 O 0.62220(14) 0.36470(10) 0.57603(9) 0.0195(2) Uani 1 1 d . . . . .
C9 C 0.55686(19) 0.23300(14) 0.82396(12) 0.0164(3) Uani 1 1 d . . . . .
H91 H 0.4149 0.2651 0.8314 0.020 Uiso 1 1 calc R U . . .
H92 H 0.6078 0.1377 0.7989 0.020 Uiso 1 1 calc R U . . .
C10 C 0.5962(2) 0.20892(15) 0.95164(13) 0.0203(3) Uani 1 1 d . . . . .
F101 F 0.55257(15) 0.33667(9) 0.98603(8) 0.0307(2) Uani 1 1 d . . . . .
F102 F 0.78152(13) 0.13968(11) 0.95843(8) 0.0337(2) Uani 1 1 d . . . . .
F103 F 0.49105(15) 0.12875(10) 1.04402(8) 0.0336(2) Uani 1 1 d . . . . .
Cl1 Cl 0.19701(4) 1.06088(3) 0.34737(3) 0.01594(10) Uani 1 1 d . . . . .
O1W O 1.07425(17) 0.38791(15) 0.85335(12) 0.0327(3) Uani 1 1 d . . . . .
H11W H 1.012(4) 0.372(3) 0.822(2) 0.049(7) Uiso 1 1 d . . . . .
H12W H 1.039(6) 0.484(5) 0.851(4) 0.124(14) Uiso 1 1 d . . . . .
O2W O 0.9842(2) 0.67551(15) 0.87816(14) 0.0360(3) Uani 1 1 d . . . . .
H21W H 0.910(4) 0.744(3) 0.840(3) 0.060(8) Uiso 1 1 d . . . . .
H22W H 0.945(4) 0.683(3) 0.943(3) 0.069(10) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C8 1.5030(15) . ?
N1 C2 1.5048(15) . ?
N1 C7 1.5126(15) 2_676 ?
N1 H1 0.863(18) . ?
C2 C3 1.5220(17) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.4887(16) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C5 1.5055(15) . ?
N4 H41 0.92(2) . ?
N4 H42 0.865(19) . ?
C5 C6 1.5241(16) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 C7 1.5206(16) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
C7 N1 1.5126(15) 2_676 ?
C7 H71 0.9900 . ?
C7 H72 0.9900 . ?
C8 P1 1.8402(12) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
P1 O12 1.4920(9) . ?
P1 O11 1.5053(9) . ?
P1 C9 1.8172(13) . ?
C9 C10 1.4931(18) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
C10 F102 1.3392(17) . ?
C10 F103 1.3400(16) . ?
C10 F101 1.3509(16) . ?
O1W H11W 0.75(3) . ?
O1W H12W 0.89(4) . ?
O2W H21W 0.81(3) . ?
O2W H22W 0.72(3) . ?

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 N1 C2 110.16(9) . . ?
C8 N1 C7 111.37(9) . 2_676 ?
C2 N1 C7 115.16(9) . 2_676 ?
C8 N1 H1 107.9(11) . . ?
C2 N1 H1 107.3(11) . . ?
C7 N1 H1 104.5(11) 2_676 . ?
N1 C2 C3 111.78(10) . . ?
N1 C2 H21 109.3 . . ?
C3 C2 H21 109.3 . . ?
N1 C2 H22 109.3 . . ?
C3 C2 H22 109.3 . . ?
H21 C2 H22 107.9 . . ?
N4 C3 C2 110.10(10) . . ?
N4 C3 H31 109.6 . . ?
C2 C3 H31 109.6 . . ?
N4 C3 H32 109.6 . . ?
C2 C3 H32 109.6 . . ?
H31 C3 H32 108.2 . . ?
C3 N4 C5 113.21(9) . . ?
C3 N4 H41 105.8(12) . . ?
C5 N4 H41 107.3(12) . . ?
C3 N4 H42 109.3(11) . . ?
C5 N4 H42 111.0(11) . . ?
H41 N4 H42 110.1(16) . . ?
N4 C5 C6 114.44(10) . . ?
N4 C5 H51 108.7 . . ?
C6 C5 H51 108.7 . . ?
N4 C5 H52 108.7 . . ?
C6 C5 H52 108.7 . . ?
H51 C5 H52 107.6 . . ?
C7 C6 C5 113.22(10) . . ?
C7 C6 H61 108.9 . . ?
C5 C6 H61 108.9 . . ?
C7 C6 H62 108.9 . . ?
C5 C6 H62 108.9 . . ?
H61 C6 H62 107.7 . . ?
N1 C7 C6 112.62(10) 2_676 . ?
N1 C7 H71 109.1 2_676 . ?
C6 C7 H71 109.1 . . ?
N1 C7 H72 109.1 2_676 . ?
C6 C7 H72 109.1 . . ?
H71 C7 H72 107.8 . . ?
N1 C8 P1 110.43(8) . . ?
N1 C8 H81 109.6 . . ?
P1 C8 H81 109.6 . . ?
N1 C8 H82 109.6 . . ?
P1 C8 H82 109.6 . . ?
H81 C8 H82 108.1 . . ?
O12 P1 O11 117.79(5) . . ?
O12 P1 C9 108.02(6) . . ?
O11 P1 C9 110.24(6) . . ?
O12 P1 C8 106.08(5) . . ?
O11 P1 C8 109.53(5) . . ?
C9 P1 C8 104.29(6) . . ?
C10 C9 P1 115.76(9) . . ?
C10 C9 H91 108.3 . . ?
P1 C9 H91 108.3 . . ?
C10 C9 H92 108.3 . . ?
P1 C9 H92 108.3 . . ?
H91 C9 H92 107.4 . . ?
F102 C10 F103 106.23(11) . . ?
F102 C10 F101 106.27(12) . . ?
F103 C10 F101 105.69(11) . . ?
F102 C10 C9 113.41(11) . . ?
F103 C10 C9 112.64(12) . . ?
F101 C10 C9 112.03(11) . . ?
H11W O1W H12W 110(3) . . ?
H21W O2W H22W 102(3) . . ?

_refine_diff_density_max         0.432
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.048



####################################################################### 
# 
# 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_zn2p6f
_database_code_depnum_ccdc_archive 'CCDC 2262046'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2023-05-10 deposited with the CCDC.	2023-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C16 H30 F6 N4 O4 P2 Zn, 0.5(C3 H6 O), 2(H2 O)
;
_chemical_formula_sum            'C17.50 H37 F6 N4 O6.50 P2 Zn'
_chemical_formula_weight         648.82

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'
F F 0.0171 0.0103 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.7340(2)
_cell_length_b                   13.3794(3)
_cell_length_c                   20.7034(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.6720(10)
_cell_angle_gamma                90
_cell_volume                     2690.77(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9800
_cell_measurement_theta_min      2.3733
_cell_measurement_theta_max      27.4837

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_F_000             1344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.163
_exptl_absorpt_coefficient_mu    1.115
_shelx_estimated_absorpt_T_min   0.757
_shelx_estimated_absorpt_T_max   0.839
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            32389
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.971
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6164
_reflns_number_gt                5843
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1380)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0254P)²+2.4115P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6164
_refine_ls_number_parameters     372
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0253
_refine_ls_wR_factor_ref         0.0651
_refine_ls_wR_factor_gt          0.0643
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Zn1 Zn 0.25472(2) 0.36980(2) 0.34178(2) 0.01144(5) Uani 1 1 d . . . . .
N1 N 0.05839(12) 0.39620(9) 0.38397(6) 0.0143(2) Uani 1 1 d . . . . .
C2 C 0.03863(15) 0.50630(11) 0.37800(8) 0.0167(3) Uani 1 1 d . . . . .
H21 H -0.0266 0.5286 0.4098 0.020 Uiso 1 1 calc R U . . .
H22 H -0.0025 0.5220 0.3342 0.020 Uiso 1 1 calc R U . . .
C3 C 0.17300(16) 0.56342(11) 0.38929(7) 0.0164(3) Uani 1 1 d . . . . .
H31 H 0.1562 0.6359 0.3833 0.020 Uiso 1 1 calc R U . . .
H32 H 0.2114 0.5524 0.4342 0.020 Uiso 1 1 calc R U . . .
N4 N 0.27141(13) 0.52827(9) 0.34307(6) 0.0141(2) Uani 1 1 d . . . . .
H41 H 0.241(2) 0.5484(15) 0.3049(10) 0.019(5) Uiso 1 1 d . . . . .
C5 C 0.41198(15) 0.56702(11) 0.35751(8) 0.0171(3) Uani 1 1 d . . . . .
H51 H 0.4501 0.5389 0.3991 0.021 Uiso 1 1 calc R U . . .
H52 H 0.4087 0.6406 0.3619 0.021 Uiso 1 1 calc R U . . .
C6 C 0.50534(16) 0.53935(12) 0.30396(8) 0.0192(3) Uani 1 1 d . . . . .
H61 H 0.5871 0.5835 0.3075 0.023 Uiso 1 1 calc R U . . .
H62 H 0.4555 0.5532 0.2617 0.023 Uiso 1 1 calc R U . . .
C7 C 0.55449(15) 0.43101(11) 0.30414(8) 0.0181(3) Uani 1 1 d . . . . .
H71 H 0.6244 0.4243 0.2717 0.022 Uiso 1 1 calc R U . . .
H72 H 0.6007 0.4164 0.3471 0.022 Uiso 1 1 calc R U . . .
N8 N 0.44578(13) 0.35359(9) 0.29010(6) 0.0142(2) Uani 1 1 d . . . . .
C9 C 0.39818(16) 0.35946(12) 0.22078(7) 0.0192(3) Uani 1 1 d . . . . .
H91 H 0.4670 0.3268 0.1946 0.023 Uiso 1 1 calc R U . . .
H92 H 0.3919 0.4306 0.2077 0.023 Uiso 1 1 calc R U . . .
C10 C 0.25941(15) 0.31010(12) 0.20636(7) 0.0170(3) Uani 1 1 d . . . . .
H101 H 0.2311 0.3171 0.1598 0.020 Uiso 1 1 calc R U . . .
H102 H 0.2658 0.2380 0.2167 0.020 Uiso 1 1 calc R U . . .
N11 N 0.15671(13) 0.35795(10) 0.24561(6) 0.0147(2) Uani 1 1 d . . . . .
H111 H 0.143(2) 0.4175(17) 0.2303(10) 0.022(5) Uiso 1 1 d . . . . .
C12 C 0.02640(15) 0.30148(11) 0.24192(8) 0.0177(3) Uani 1 1 d . . . . .
H121 H 0.0434 0.2335 0.2596 0.021 Uiso 1 1 calc R U . . .
H122 H -0.0074 0.2947 0.1960 0.021 Uiso 1 1 calc R U . . .
C13 C -0.08349(16) 0.35219(13) 0.27929(8) 0.0203(3) Uani 1 1 d . . . . .
H131 H -0.1740 0.3232 0.2651 0.024 Uiso 1 1 calc R U . . .
H132 H -0.0860 0.4240 0.2677 0.024 Uiso 1 1 calc R U . . .
C14 C -0.06397(15) 0.34332(13) 0.35256(8) 0.0200(3) Uani 1 1 d . . . . .
H141 H -0.1477 0.3695 0.3715 0.024 Uiso 1 1 calc R U . . .
H142 H -0.0567 0.2715 0.3638 0.024 Uiso 1 1 calc R U . . .
C20 C 0.07100(15) 0.36412(12) 0.45291(7) 0.0172(3) Uani 1 1 d . . . . .
H201 H 0.0413 0.2935 0.4553 0.021 Uiso 1 1 calc R U . . .
H202 H 0.0069 0.4046 0.4774 0.021 Uiso 1 1 calc R U . . .
P1 P 0.24478(4) 0.37522(3) 0.49292(2) 0.01467(8) Uani 1 1 d . . . . .
O11 O 0.34381(11) 0.37132(8) 0.43949(5) 0.0165(2) Uani 1 1 d . . . . .
O12 O 0.25362(12) 0.45971(9) 0.53982(5) 0.0209(2) Uani 1 1 d . . . . .
C21 C 0.27117(16) 0.25697(12) 0.53694(8) 0.0205(3) Uani 1 1 d . . . . .
H211 H 0.2525 0.2015 0.5060 0.025 Uiso 1 1 calc R U . . .
H212 H 0.3694 0.2527 0.5523 0.025 Uiso 1 1 calc R U . . .
C22 C 0.18609(17) 0.24075(12) 0.59363(8) 0.0213(3) Uani 1 1 d . . . . .
F1 F 0.05099(10) 0.25476(9) 0.57855(5) 0.0303(2) Uani 1 1 d . . . . .
F2 F 0.21834(14) 0.30080(10) 0.64359(5) 0.0412(3) Uani 1 1 d . . . . .
F3 F 0.19669(12) 0.14709(8) 0.61670(6) 0.0370(3) Uani 1 1 d . . . . .
C30 C 0.50513(15) 0.25375(11) 0.30683(8) 0.0179(3) Uani 1 1 d . . . . .
H301 H 0.5760 0.2619 0.3429 0.021 Uiso 1 1 calc R U . . .
H302 H 0.5519 0.2282 0.2691 0.021 Uiso 1 1 calc R U . . .
P2 P 0.37945(4) 0.15931(3) 0.33037(2) 0.01422(8) Uani 1 1 d . . . . .
O21 O 0.25252(11) 0.21482(8) 0.34856(5) 0.0175(2) Uani 1 1 d . . . . .
O22 O 0.36369(12) 0.07803(8) 0.28094(5) 0.0204(2) Uani 1 1 d . . . . .
C31 C 0.45563(17) 0.10657(13) 0.40571(8) 0.0213(3) Uani 1 1 d . . . . .
H311 H 0.4877 0.1624 0.4342 0.026 Uiso 1 1 calc R U . . .
H312 H 0.3826 0.0710 0.4276 0.026 Uiso 1 1 calc R U . . .
C32 C 0.57295(18) 0.03630(13) 0.39944(8) 0.0248(3) Uani 1 1 d . . . . .
F4 F 0.67060(12) 0.07432(11) 0.36426(6) 0.0449(3) Uani 1 1 d . . . . .
F5 F 0.53485(15) -0.04972(9) 0.37158(7) 0.0520(4) Uani 1 1 d . . . . .
F6 F 0.63623(13) 0.01189(10) 0.45680(5) 0.0398(3) Uani 1 1 d . . . . .
O1S O 0.8201(3) 0.0558(2) 0.57059(15) 0.0413(7) Uani 0.5 1 d . . P . .
C1S C 0.9680(6) 0.0584(4) 0.4831(2) 0.0538(14) Uani 0.5 1 d . . P . .
H1S1 H 0.9206 0.1213 0.4720 0.081 Uiso 0.5 1 d R U P . .
H1S2 H 1.0675 0.0704 0.4884 0.081 Uiso 0.5 1 d R U P . .
H1S3 H 0.9486 0.0097 0.4484 0.081 Uiso 0.5 1 d R U P . .
C2S C 0.9178(4) 0.0181(3) 0.5455(2) 0.0372(9) Uani 0.5 1 d . . P . .
C3S C 0.9918(5) -0.0670(4) 0.5755(3) 0.0583(15) Uani 0.5 1 d . . P . .
H3S1 H 0.9321 -0.1031 0.6040 0.087 Uiso 0.5 1 d R U P . .
H3S2 H 1.0195 -0.1119 0.5413 0.087 Uiso 0.5 1 d R U P . .
H3S3 H 1.0738 -0.0431 0.6008 0.087 Uiso 0.5 1 d R U P . .
O1W O 0.62804(14) 0.35370(11) 0.46062(7) 0.0286(3) Uani 1 1 d . . . . .
H11W H 0.551(3) 0.3628(18) 0.4582(12) 0.039(7) Uiso 1 1 d . . . . .
H12W H 0.665(3) 0.413(2) 0.4643(14) 0.058(8) Uiso 1 1 d . . . . .
O2W O 0.6150(3) 0.20920(19) 0.54877(12) 0.0625(7) Uani 0.782(4) 1 d . . P A 1
H21W H 0.6654 0.2490 0.5187 0.075 Uiso 1 1 d R U . . .
H22W H 0.6705 0.1433 0.5403 0.075 Uiso 1 1 d R U . . .
O2V O 0.7316(12) 0.1998(7) 0.5414(4) 0.0625(7) Uani 0.218(4) 1 d . . 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
Zn1 O21 2.0785(11) . ?
Zn1 N4 2.1265(13) . ?
Zn1 O11 2.1494(11) . ?
Zn1 N11 2.1578(13) . ?
Zn1 N1 2.1803(12) . ?
Zn1 N8 2.2149(12) . ?
N1 C20 1.4879(19) . ?
N1 C2 1.4897(19) . ?
N1 C14 1.4976(19) . ?
C2 C3 1.520(2) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.4737(19) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C5 1.4758(19) . ?
N4 H41 0.87(2) . ?
C5 C6 1.524(2) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 C7 1.526(2) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
C7 N8 1.4959(19) . ?
C7 H71 0.9900 . ?
C7 H72 0.9900 . ?
N8 C9 1.4815(19) . ?
N8 C30 1.4875(19) . ?
C9 C10 1.516(2) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
C10 N11 1.4744(19) . ?
C10 H101 0.9900 . ?
C10 H102 0.9900 . ?
N11 C12 1.4742(19) . ?
N11 H111 0.86(2) . ?
C12 C13 1.520(2) . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C13 C14 1.521(2) . ?
C13 H131 0.9900 . ?
C13 H132 0.9900 . ?
C14 H141 0.9900 . ?
C14 H142 0.9900 . ?
C20 P1 1.8413(16) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.4892(12) . ?
P1 O11 1.5139(11) . ?
P1 C21 1.8357(16) . ?
C21 C22 1.495(2) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
C22 F2 1.331(2) . ?
C22 F3 1.3427(19) . ?
C22 F1 1.3451(19) . ?
C30 P2 1.8458(16) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
P2 O22 1.4945(11) . ?
P2 O21 1.5098(11) . ?
P2 C31 1.8256(16) . ?
C31 C32 1.491(2) . ?
C31 H311 0.9900 . ?
C31 H312 0.9900 . ?
C32 F5 1.330(2) . ?
C32 F4 1.335(2) . ?
C32 F6 1.3428(19) . ?
O1S C2S 1.222(5) . ?
C1S C2S 1.509(6) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
C2S C3S 1.465(7) . ?
C3S H3S1 0.9800 . ?
C3S H3S2 0.9800 . ?
C3S H3S3 0.9800 . ?
O1W H11W 0.76(3) . ?
O1W H12W 0.88(3) . ?
O2W H21W 0.9744 . ?
O2W H22W 1.0541 . ?
O2V H21W 1.0149 . ?
O2V H22W 0.9612 . ?

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
O21 Zn1 N4 174.24(5) . . ?
O21 Zn1 O11 87.21(4) . . ?
N4 Zn1 O11 87.30(5) . . ?
O21 Zn1 N11 89.03(5) . . ?
N4 Zn1 N11 96.53(5) . . ?
O11 Zn1 N11 175.55(5) . . ?
O21 Zn1 N1 96.98(4) . . ?
N4 Zn1 N1 84.35(5) . . ?
O11 Zn1 N1 86.13(4) . . ?
N11 Zn1 N1 91.98(5) . . ?
O21 Zn1 N8 86.99(4) . . ?
N4 Zn1 N8 92.17(5) . . ?
O11 Zn1 N8 98.91(4) . . ?
N11 Zn1 N8 83.24(5) . . ?
N1 Zn1 N8 173.75(5) . . ?
C20 N1 C2 111.54(12) . . ?
C20 N1 C14 107.14(12) . . ?
C2 N1 C14 109.64(12) . . ?
C20 N1 Zn1 108.48(9) . . ?
C2 N1 Zn1 103.82(9) . . ?
C14 N1 Zn1 116.27(9) . . ?
N1 C2 C3 112.27(12) . . ?
N1 C2 H21 109.1 . . ?
C3 C2 H21 109.1 . . ?
N1 C2 H22 109.1 . . ?
C3 C2 H22 109.1 . . ?
H21 C2 H22 107.9 . . ?
N4 C3 C2 109.17(12) . . ?
N4 C3 H31 109.8 . . ?
C2 C3 H31 109.8 . . ?
N4 C3 H32 109.8 . . ?
C2 C3 H32 109.8 . . ?
H31 C3 H32 108.3 . . ?
C3 N4 C5 112.90(12) . . ?
C3 N4 Zn1 105.90(9) . . ?
C5 N4 Zn1 114.95(9) . . ?
C3 N4 H41 107.0(13) . . ?
C5 N4 H41 109.6(13) . . ?
Zn1 N4 H41 106.0(13) . . ?
N4 C5 C6 110.84(12) . . ?
N4 C5 H51 109.5 . . ?
C6 C5 H51 109.5 . . ?
N4 C5 H52 109.5 . . ?
C6 C5 H52 109.5 . . ?
H51 C5 H52 108.1 . . ?
C5 C6 C7 115.50(13) . . ?
C5 C6 H61 108.4 . . ?
C7 C6 H61 108.4 . . ?
C5 C6 H62 108.4 . . ?
C7 C6 H62 108.4 . . ?
H61 C6 H62 107.5 . . ?
N8 C7 C6 116.07(12) . . ?
N8 C7 H71 108.3 . . ?
C6 C7 H71 108.3 . . ?
N8 C7 H72 108.3 . . ?
C6 C7 H72 108.3 . . ?
H71 C7 H72 107.4 . . ?
C9 N8 C30 111.47(12) . . ?
C9 N8 C7 108.96(12) . . ?
C30 N8 C7 108.49(11) . . ?
C9 N8 Zn1 104.04(9) . . ?
C30 N8 Zn1 107.52(9) . . ?
C7 N8 Zn1 116.34(9) . . ?
N8 C9 C10 112.78(12) . . ?
N8 C9 H91 109.0 . . ?
C10 C9 H91 109.0 . . ?
N8 C9 H92 109.0 . . ?
C10 C9 H92 109.0 . . ?
H91 C9 H92 107.8 . . ?
N11 C10 C9 109.23(12) . . ?
N11 C10 H101 109.8 . . ?
C9 C10 H101 109.8 . . ?
N11 C10 H102 109.8 . . ?
C9 C10 H102 109.8 . . ?
H101 C10 H102 108.3 . . ?
C12 N11 C10 111.12(12) . . ?
C12 N11 Zn1 114.43(10) . . ?
C10 N11 Zn1 105.38(9) . . ?
C12 N11 H111 109.7(13) . . ?
C10 N11 H111 107.2(13) . . ?
Zn1 N11 H111 108.7(13) . . ?
N11 C12 C13 112.10(12) . . ?
N11 C12 H121 109.2 . . ?
C13 C12 H121 109.2 . . ?
N11 C12 H122 109.2 . . ?
C13 C12 H122 109.2 . . ?
H121 C12 H122 107.9 . . ?
C12 C13 C14 115.20(13) . . ?
C12 C13 H131 108.5 . . ?
C14 C13 H131 108.5 . . ?
C12 C13 H132 108.5 . . ?
C14 C13 H132 108.5 . . ?
H131 C13 H132 107.5 . . ?
N1 C14 C13 116.18(13) . . ?
N1 C14 H141 108.2 . . ?
C13 C14 H141 108.2 . . ?
N1 C14 H142 108.2 . . ?
C13 C14 H142 108.2 . . ?
H141 C14 H142 107.4 . . ?
N1 C20 P1 115.17(10) . . ?
N1 C20 H201 108.5 . . ?
P1 C20 H201 108.5 . . ?
N1 C20 H202 108.5 . . ?
P1 C20 H202 108.5 . . ?
H201 C20 H202 107.5 . . ?
O12 P1 O11 119.32(7) . . ?
O12 P1 C21 109.28(7) . . ?
O11 P1 C21 104.93(7) . . ?
O12 P1 C20 111.57(7) . . ?
O11 P1 C20 106.15(7) . . ?
C21 P1 C20 104.43(7) . . ?
P1 O11 Zn1 116.78(6) . . ?
C22 C21 P1 116.61(11) . . ?
C22 C21 H211 108.1 . . ?
P1 C21 H211 108.1 . . ?
C22 C21 H212 108.1 . . ?
P1 C21 H212 108.1 . . ?
H211 C21 H212 107.3 . . ?
F2 C22 F3 106.13(14) . . ?
F2 C22 F1 105.94(14) . . ?
F3 C22 F1 105.33(13) . . ?
F2 C22 C21 114.04(14) . . ?
F3 C22 C21 112.40(14) . . ?
F1 C22 C21 112.33(13) . . ?
N8 C30 P2 114.97(10) . . ?
N8 C30 H301 108.5 . . ?
P2 C30 H301 108.5 . . ?
N8 C30 H302 108.5 . . ?
P2 C30 H302 108.5 . . ?
H301 C30 H302 107.5 . . ?
O22 P2 O21 118.61(7) . . ?
O22 P2 C31 108.79(7) . . ?
O21 P2 C31 105.73(7) . . ?
O22 P2 C30 110.98(7) . . ?
O21 P2 C30 107.22(6) . . ?
C31 P2 C30 104.50(8) . . ?
P2 O21 Zn1 117.50(6) . . ?
C32 C31 P2 116.14(12) . . ?
C32 C31 H311 108.3 . . ?
P2 C31 H311 108.3 . . ?
C32 C31 H312 108.3 . . ?
P2 C31 H312 108.3 . . ?
H311 C31 H312 107.4 . . ?
F5 C32 F4 106.37(16) . . ?
F5 C32 F6 105.81(14) . . ?
F4 C32 F6 105.84(14) . . ?
F5 C32 C31 112.93(15) . . ?
F4 C32 C31 112.55(15) . . ?
F6 C32 C31 112.75(14) . . ?
C2S C1S H1S1 109.5 . . ?
C2S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
C2S C1S H1S3 109.4 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
O1S C2S C3S 121.0(5) . . ?
O1S C2S C1S 121.4(5) . . ?
C3S C2S C1S 117.7(5) . . ?
C2S C3S H3S1 110.2 . . ?
C2S C3S H3S2 108.7 . . ?
H3S1 C3S H3S2 109.5 . . ?
C2S C3S H3S3 109.6 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?
H11W O1W H12W 105(3) . . ?
H21W O2W H22W 93.9 . . ?
H21W O2V H22W 97.2 . . ?

_refine_diff_density_max         0.459
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.057



####################################################################### 
# 
# 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_cubn2te2fp
_database_code_depnum_ccdc_archive 'CCDC 2262047'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2023-05-10 deposited with the CCDC.	2023-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H30 Cu F6 N4 O4 P2, 3(H2 O)'
_chemical_formula_sum            'C16 H36 Cu F6 N4 O7 P2'
_chemical_formula_weight         635.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0011(4)
_cell_length_b                   10.5012(4)
_cell_length_c                   13.4258(5)
_cell_angle_alpha                85.7250(10)
_cell_angle_beta                 71.9070(10)
_cell_angle_gamma                76.1410(10)
_cell_volume                     1301.29(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    127
_cell_measurement_theta_min      2.4947
_cell_measurement_theta_max      26.6881

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_F_000             658
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    1.048
_shelx_estimated_absorpt_T_min   0.820
_shelx_estimated_absorpt_T_max   0.930
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            48653
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.200
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5984
_reflns_number_gt                5459
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Instrument Service vV6.2.1'
_computing_cell_refinement       'APEX3 v2016.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 758)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0295P)²+0.9380P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5984
_refine_ls_number_parameters     357
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0634
_refine_ls_wR_factor_gt          0.0615
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cu1 Cu 0.28920(2) 0.59488(2) 0.25706(2) 0.00941(5) Uani 1 1 d . . . . .
N1 N 0.25848(13) 0.76283(12) 0.16849(10) 0.0131(2) Uani 1 1 d . . . . .
C2 C 0.22556(17) 0.71724(16) 0.07771(12) 0.0180(3) Uani 1 1 d . . . . .
H21 H 0.3163 0.6714 0.0265 0.022 Uiso 1 1 calc R U . . .
H22 H 0.1801 0.7937 0.0423 0.022 Uiso 1 1 calc R U . . .
C3 C 0.12409(17) 0.62491(16) 0.11584(13) 0.0189(3) Uani 1 1 d . . . . .
H31 H 0.0295 0.6730 0.1612 0.023 Uiso 1 1 calc R U . . .
H32 H 0.1084 0.5890 0.0553 0.023 Uiso 1 1 calc R U . . .
N4 N 0.18943(14) 0.51661(13) 0.17569(10) 0.0143(3) Uani 1 1 d . . . . .
H41 H 0.257(2) 0.464(2) 0.1304(17) 0.023(5) Uiso 1 1 d . . . . .
C5 C 0.07987(17) 0.44571(16) 0.23986(13) 0.0188(3) Uani 1 1 d . . . . .
H51 H 0.0351 0.4133 0.1936 0.023 Uiso 1 1 calc R U . . .
H52 H 0.0029 0.5074 0.2907 0.023 Uiso 1 1 calc R U . . .
C6 C 0.14455(17) 0.33066(16) 0.29883(13) 0.0191(3) Uani 1 1 d . . . . .
H61 H 0.2258 0.2725 0.2479 0.023 Uiso 1 1 calc R U . . .
H62 H 0.0705 0.2798 0.3315 0.023 Uiso 1 1 calc R U . . .
C7 C 0.19939(16) 0.36883(15) 0.38374(12) 0.0162(3) Uani 1 1 d . . . . .
H71 H 0.1207 0.4333 0.4311 0.019 Uiso 1 1 calc R U . . .
H72 H 0.2233 0.2900 0.4258 0.019 Uiso 1 1 calc R U . . .
N8 N 0.32948(13) 0.42622(12) 0.34264(9) 0.0115(2) Uani 1 1 d . . . . .
C9 C 0.36715(17) 0.47181(15) 0.43123(12) 0.0153(3) Uani 1 1 d . . . . .
H91 H 0.4680 0.4824 0.4065 0.018 Uiso 1 1 calc R U . . .
H92 H 0.3600 0.4052 0.4877 0.018 Uiso 1 1 calc R U . . .
C10 C 0.26589(17) 0.60145(15) 0.47396(12) 0.0158(3) Uani 1 1 d . . . . .
H101 H 0.1669 0.5886 0.5080 0.019 Uiso 1 1 calc R U . . .
H102 H 0.2983 0.6359 0.5270 0.019 Uiso 1 1 calc R U . . .
N11 N 0.26596(14) 0.69607(12) 0.38607(10) 0.0119(2) Uani 1 1 d . . . . .
H111 H 0.340(2) 0.7285(18) 0.3749(15) 0.013(4) Uiso 1 1 d . . . . .
C12 C 0.13589(16) 0.80631(15) 0.41315(12) 0.0157(3) Uani 1 1 d . . . . .
H121 H 0.1267 0.8456 0.4804 0.019 Uiso 1 1 calc R U . . .
H122 H 0.0488 0.7720 0.4225 0.019 Uiso 1 1 calc R U . . .
C13 C 0.14362(17) 0.91136(15) 0.32906(12) 0.0169(3) Uani 1 1 d . . . . .
H131 H 0.2352 0.9395 0.3162 0.020 Uiso 1 1 calc R U . . .
H132 H 0.0635 0.9883 0.3561 0.020 Uiso 1 1 calc R U . . .
C14 C 0.13548(17) 0.87073(15) 0.22480(12) 0.0175(3) Uani 1 1 d . . . . .
H141 H 0.0441 0.8422 0.2376 0.021 Uiso 1 1 calc R U . . .
H142 H 0.1318 0.9485 0.1784 0.021 Uiso 1 1 calc R U . . .
C15 C 0.39406(16) 0.81183(15) 0.12969(12) 0.0152(3) Uani 1 1 d . . . . .
H151 H 0.4032 0.8621 0.1858 0.018 Uiso 1 1 calc R U . . .
H152 H 0.3901 0.8712 0.0693 0.018 Uiso 1 1 calc R U . . .
P1 P 0.55123(4) 0.67342(4) 0.08977(3) 0.01281(8) Uani 1 1 d . . . . .
O11 O 0.51367(12) 0.56900(11) 0.16940(9) 0.0202(2) Uani 1 1 d . . . . .
O12 O 0.59165(13) 0.64695(12) -0.02447(9) 0.0224(3) Uani 1 1 d . . . . .
C16 C 0.69872(17) 0.72370(16) 0.11758(13) 0.0179(3) Uani 1 1 d . . . . .
H161 H 0.6599 0.7681 0.1866 0.021 Uiso 1 1 calc R U . . .
H162 H 0.7717 0.6437 0.1239 0.021 Uiso 1 1 calc R U . . .
C17 C 0.7728(2) 0.81164(18) 0.04024(14) 0.0254(4) Uani 1 1 d . . . . .
F1 F 0.67853(18) 0.91904(14) 0.02287(14) 0.0602(5) Uani 1 1 d . . . . .
F2 F 0.84657(18) 0.75466(18) -0.05179(10) 0.0697(6) Uani 1 1 d . . . . .
F3 F 0.86792(12) 0.85668(11) 0.07249(9) 0.0303(2) Uani 1 1 d . . . . .
C18 C 0.45584(15) 0.33175(14) 0.27471(11) 0.0124(3) Uani 1 1 d . . . . .
H181 H 0.5362 0.3771 0.2487 0.015 Uiso 1 1 calc R U . . .
H182 H 0.4294 0.3132 0.2129 0.015 Uiso 1 1 calc R U . . .
P2 P 0.52594(4) 0.17424(4) 0.32888(3) 0.01186(8) Uani 1 1 d . . . . .
O21 O 0.42812(12) 0.08194(11) 0.33905(9) 0.0190(2) Uani 1 1 d . . . . .
O22 O 0.57147(12) 0.19373(11) 0.42222(9) 0.0187(2) Uani 1 1 d . . . . .
C19 C 0.68837(16) 0.10885(15) 0.22103(12) 0.0165(3) Uani 1 1 d . . . . .
H191 H 0.7196 0.0139 0.2339 0.020 Uiso 1 1 calc R U . . .
H192 H 0.6602 0.1173 0.1559 0.020 Uiso 1 1 calc R U . . .
C20 C 0.81673(17) 0.16704(17) 0.20056(13) 0.0208(3) Uani 1 1 d . . . . .
F4 F 0.78998(12) 0.29512(11) 0.17703(11) 0.0384(3) Uani 1 1 d . . . . .
F5 F 0.87092(12) 0.15409(14) 0.28136(9) 0.0386(3) Uani 1 1 d . . . . .
F6 F 0.92542(11) 0.10859(11) 0.11850(9) 0.0328(3) Uani 1 1 d . . . . .
O1W O 0.23086(13) 0.03570(13) 0.52976(10) 0.0215(2) Uani 1 1 d . . . . .
H11W H 0.278(3) -0.029(3) 0.549(2) 0.046(7) Uiso 1 1 d . . . . .
H12W H 0.282(3) 0.057(2) 0.474(2) 0.040(7) Uiso 1 1 d . . . . .
O2W O 0.48483(12) 0.18432(12) 0.63278(9) 0.0168(2) Uani 1 1 d . . . . .
H21W H 0.505(3) 0.110(2) 0.6433(18) 0.032(6) Uiso 1 1 d . . . . .
H22W H 0.503(3) 0.188(2) 0.568(2) 0.036(6) Uiso 1 1 d . . . . .
O3W O 0.17466(16) 0.25228(16) 0.65743(12) 0.0340(3) Uani 1 1 d . . . . .
H31W H 0.256(3) 0.251(3) 0.658(2) 0.048(8) Uiso 1 1 d . . . . .
H32W H 0.185(3) 0.188(3) 0.621(2) 0.040(7) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 2.0171(13) . ?
Cu1 N11 2.0222(12) . ?
Cu1 N8 2.0643(12) . ?
Cu1 N1 2.0673(13) . ?
Cu1 O11 2.1478(11) . ?
N1 C15 1.4933(19) . ?
N1 C2 1.4950(19) . ?
N1 C14 1.5003(19) . ?
C2 C3 1.519(2) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.483(2) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C5 1.485(2) . ?
N4 H41 0.86(2) . ?
C5 C6 1.519(2) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 C7 1.524(2) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
C7 N8 1.4968(18) . ?
C7 H71 0.9900 . ?
C7 H72 0.9900 . ?
N8 C18 1.4938(18) . ?
N8 C9 1.4951(18) . ?
C9 C10 1.518(2) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
C10 N11 1.4848(19) . ?
C10 H101 0.9900 . ?
C10 H102 0.9900 . ?
N11 C12 1.4874(18) . ?
N11 H111 0.85(2) . ?
C12 C13 1.516(2) . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C13 C14 1.525(2) . ?
C13 H131 0.9900 . ?
C13 H132 0.9900 . ?
C14 H141 0.9900 . ?
C14 H142 0.9900 . ?
C15 P1 1.8355(15) . ?
C15 H151 0.9900 . ?
C15 H152 0.9900 . ?
P1 O12 1.4893(12) . ?
P1 O11 1.5031(11) . ?
P1 C16 1.8271(16) . ?
C16 C17 1.479(2) . ?
C16 H161 0.9900 . ?
C16 H162 0.9900 . ?
C17 F2 1.327(2) . ?
C17 F1 1.343(2) . ?
C17 F3 1.349(2) . ?
C18 P2 1.8270(15) . ?
C18 H181 0.9900 . ?
C18 H182 0.9900 . ?
P2 O22 1.5023(11) . ?
P2 O21 1.5056(11) . ?
P2 C19 1.8330(16) . ?
C19 C20 1.493(2) . ?
C19 H191 0.9900 . ?
C19 H192 0.9900 . ?
C20 F5 1.340(2) . ?
C20 F4 1.341(2) . ?
C20 F6 1.345(2) . ?
O1W H11W 0.81(3) . ?
O1W H12W 0.81(3) . ?
O2W H21W 0.78(2) . ?
O2W H22W 0.84(3) . ?
O3W H31W 0.81(3) . ?
O3W H32W 0.83(3) . ?

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
N4 Cu1 N11 146.28(5) . . ?
N4 Cu1 N8 93.81(5) . . ?
N11 Cu1 N8 87.09(5) . . ?
N4 Cu1 N1 87.29(5) . . ?
N11 Cu1 N1 93.24(5) . . ?
N8 Cu1 N1 177.50(5) . . ?
N4 Cu1 O11 109.00(5) . . ?
N11 Cu1 O11 104.65(5) . . ?
N8 Cu1 O11 92.06(4) . . ?
N1 Cu1 O11 85.46(5) . . ?
C15 N1 C2 109.41(12) . . ?
C15 N1 C14 109.83(12) . . ?
C2 N1 C14 109.50(11) . . ?
C15 N1 Cu1 110.48(9) . . ?
C2 N1 Cu1 103.51(9) . . ?
C14 N1 Cu1 113.88(9) . . ?
N1 C2 C3 109.79(12) . . ?
N1 C2 H21 109.7 . . ?
C3 C2 H21 109.7 . . ?
N1 C2 H22 109.7 . . ?
C3 C2 H22 109.7 . . ?
H21 C2 H22 108.2 . . ?
N4 C3 C2 108.77(12) . . ?
N4 C3 H31 109.9 . . ?
C2 C3 H31 109.9 . . ?
N4 C3 H32 109.9 . . ?
C2 C3 H32 109.9 . . ?
H31 C3 H32 108.3 . . ?
C3 N4 C5 110.98(12) . . ?
C3 N4 Cu1 107.09(9) . . ?
C5 N4 Cu1 115.09(10) . . ?
C3 N4 H41 106.9(13) . . ?
C5 N4 H41 110.1(14) . . ?
Cu1 N4 H41 106.3(13) . . ?
N4 C5 C6 112.32(13) . . ?
N4 C5 H51 109.1 . . ?
C6 C5 H51 109.1 . . ?
N4 C5 H52 109.1 . . ?
C6 C5 H52 109.1 . . ?
H51 C5 H52 107.9 . . ?
C5 C6 C7 114.55(13) . . ?
C5 C6 H61 108.6 . . ?
C7 C6 H61 108.6 . . ?
C5 C6 H62 108.6 . . ?
C7 C6 H62 108.6 . . ?
H61 C6 H62 107.6 . . ?
N8 C7 C6 114.10(12) . . ?
N8 C7 H71 108.7 . . ?
C6 C7 H71 108.7 . . ?
N8 C7 H72 108.7 . . ?
C6 C7 H72 108.7 . . ?
H71 C7 H72 107.6 . . ?
C18 N8 C9 110.68(11) . . ?
C18 N8 C7 111.99(11) . . ?
C9 N8 C7 110.28(11) . . ?
C18 N8 Cu1 108.11(9) . . ?
C9 N8 Cu1 103.57(9) . . ?
C7 N8 Cu1 111.88(9) . . ?
N8 C9 C10 110.47(12) . . ?
N8 C9 H91 109.6 . . ?
C10 C9 H91 109.6 . . ?
N8 C9 H92 109.6 . . ?
C10 C9 H92 109.6 . . ?
H91 C9 H92 108.1 . . ?
N11 C10 C9 108.86(12) . . ?
N11 C10 H101 109.9 . . ?
C9 C10 H101 109.9 . . ?
N11 C10 H102 109.9 . . ?
C9 C10 H102 109.9 . . ?
H101 C10 H102 108.3 . . ?
C10 N11 C12 111.59(12) . . ?
C10 N11 Cu1 107.90(9) . . ?
C12 N11 Cu1 113.91(9) . . ?
C10 N11 H111 107.5(13) . . ?
C12 N11 H111 107.5(12) . . ?
Cu1 N11 H111 108.3(13) . . ?
N11 C12 C13 111.89(12) . . ?
N11 C12 H121 109.2 . . ?
C13 C12 H121 109.2 . . ?
N11 C12 H122 109.2 . . ?
C13 C12 H122 109.2 . . ?
H121 C12 H122 107.9 . . ?
C12 C13 C14 115.35(13) . . ?
C12 C13 H131 108.4 . . ?
C14 C13 H131 108.4 . . ?
C12 C13 H132 108.4 . . ?
C14 C13 H132 108.4 . . ?
H131 C13 H132 107.5 . . ?
N1 C14 C13 114.94(12) . . ?
N1 C14 H141 108.5 . . ?
C13 C14 H141 108.5 . . ?
N1 C14 H142 108.5 . . ?
C13 C14 H142 108.5 . . ?
H141 C14 H142 107.5 . . ?
N1 C15 P1 110.07(10) . . ?
N1 C15 H151 109.6 . . ?
P1 C15 H151 109.6 . . ?
N1 C15 H152 109.6 . . ?
P1 C15 H152 109.6 . . ?
H151 C15 H152 108.2 . . ?
O12 P1 O11 120.95(7) . . ?
O12 P1 C16 109.19(7) . . ?
O11 P1 C16 105.01(7) . . ?
O12 P1 C15 110.95(7) . . ?
O11 P1 C15 103.85(7) . . ?
C16 P1 C15 105.78(7) . . ?
P1 O11 Cu1 115.93(6) . . ?
C17 C16 P1 116.54(12) . . ?
C17 C16 H161 108.2 . . ?
P1 C16 H161 108.2 . . ?
C17 C16 H162 108.2 . . ?
P1 C16 H162 108.2 . . ?
H161 C16 H162 107.3 . . ?
F2 C17 F1 107.40(18) . . ?
F2 C17 F3 106.13(15) . . ?
F1 C17 F3 105.42(14) . . ?
F2 C17 C16 113.20(15) . . ?
F1 C17 C16 111.39(15) . . ?
F3 C17 C16 112.79(15) . . ?
N8 C18 P2 119.45(10) . . ?
N8 C18 H181 107.5 . . ?
P2 C18 H181 107.5 . . ?
N8 C18 H182 107.5 . . ?
P2 C18 H182 107.5 . . ?
H181 C18 H182 107.0 . . ?
O22 P2 O21 118.41(7) . . ?
O22 P2 C18 110.88(7) . . ?
O21 P2 C18 110.89(7) . . ?
O22 P2 C19 108.40(7) . . ?
O21 P2 C19 105.36(7) . . ?
C18 P2 C19 101.29(7) . . ?
C20 C19 P2 118.90(12) . . ?
C20 C19 H191 107.6 . . ?
P2 C19 H191 107.6 . . ?
C20 C19 H192 107.6 . . ?
P2 C19 H192 107.6 . . ?
H191 C19 H192 107.0 . . ?
F5 C20 F4 106.77(15) . . ?
F5 C20 F6 105.94(13) . . ?
F4 C20 F6 105.76(13) . . ?
F5 C20 C19 113.26(14) . . ?
F4 C20 C19 113.40(13) . . ?
F6 C20 C19 111.13(14) . . ?
H11W O1W H12W 107(2) . . ?
H21W O2W H22W 103(2) . . ?
H31W O3W H32W 104(2) . . ?

_refine_diff_density_max         0.685
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.061



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

data_znte2pf
_database_code_depnum_ccdc_archive 'CCDC 2262039'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2023-05-10 deposited with the CCDC.	2023-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
0.5(C16 H44 F6 Li2 N4 O10 P2), 0.5(C16 H32 F6 N4 O4 P2), Cl, 3(H2 O)
;
_chemical_formula_sum            'C16 H44 Cl F6 Li N4 O10 P2'
_chemical_formula_weight         670.88

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4863(6)
_cell_length_b                   11.7783(6)
_cell_length_c                   13.6581(8)
_cell_angle_alpha                99.947(2)
_cell_angle_beta                 90.009(2)
_cell_angle_gamma                99.799(2)
_cell_volume                     1480.50(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9281
_cell_measurement_theta_min      2.6922
_cell_measurement_theta_max      29.9791

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_F_000             704
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.129
_exptl_absorpt_coefficient_mu    0.327
_shelx_estimated_absorpt_T_min   0.918
_shelx_estimated_absorpt_T_max   0.959
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            79797
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.180
_diffrn_reflns_theta_max         30.005
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8637
_reflns_number_gt                7835
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Instrument Service vV6.2.15'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1242)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0538P)²+0.9844P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8637
_refine_ls_number_parameters     450
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.1077
_refine_ls_wR_factor_gt          0.1043
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1A N 0.51388(11) 0.60317(9) 0.38740(8) 0.01646(19) Uani 1 1 d . . . . .
C2A C 0.57845(14) 0.52270(12) 0.31336(10) 0.0194(2) Uani 1 1 d . . . . .
H21 H 0.6778 0.5225 0.3354 0.023 Uiso 1 1 calc R U . . .
H22 H 0.5825 0.5513 0.2492 0.023 Uiso 1 1 calc R U . . .
C3A C 0.49531(14) 0.39834(12) 0.29784(9) 0.0195(2) Uani 1 1 d . . . . .
H31 H 0.3963 0.3969 0.2741 0.023 Uiso 1 1 calc R U . . .
H32 H 0.5416 0.3471 0.2473 0.023 Uiso 1 1 calc R U . . .
N4A N 0.49317(12) 0.35591(10) 0.39407(8) 0.0174(2) Uani 1 1 d . . . . .
H41 H 0.449(2) 0.4007(17) 0.4363(15) 0.026(5) Uiso 1 1 d . . . . .
H42 H 0.585(2) 0.3580(18) 0.4149(16) 0.030(5) Uiso 1 1 d . . . . .
C5A C 0.41167(14) 0.23601(11) 0.39500(10) 0.0202(2) Uani 1 1 d . . . . .
H51 H 0.4478 0.1792 0.3433 0.024 Uiso 1 1 calc R U . . .
H52 H 0.3092 0.2339 0.3795 0.024 Uiso 1 1 calc R U . . .
C6A C 0.42772(15) 0.20166(11) 0.49690(11) 0.0217(2) Uani 1 1 d . . . . .
H61 H 0.5291 0.1954 0.5078 0.026 Uiso 1 1 calc R U . . .
H62 H 0.3698 0.1231 0.4959 0.026 Uiso 1 1 calc R U . . .
C7A C 0.38305(14) 0.28573(12) 0.58512(10) 0.0204(2) Uani 1 1 d . . . . .
H71 H 0.2888 0.3043 0.5688 0.024 Uiso 1 1 calc R U . . .
H72 H 0.3714 0.2457 0.6434 0.024 Uiso 1 1 calc R U . . .
C10A C 0.37524(13) 0.62277(11) 0.34836(9) 0.0169(2) Uani 1 1 d . . . . .
H101 H 0.3585 0.5817 0.2787 0.020 Uiso 1 1 calc R U . . .
H102 H 0.3785 0.7074 0.3493 0.020 Uiso 1 1 calc R U . . .
P1A P 0.22932(3) 0.56837(3) 0.42437(2) 0.01353(7) Uani 1 1 d . . . . .
O11A O 0.22703(10) 0.44052(8) 0.42394(7) 0.01942(18) Uani 1 1 d . . . . .
O12A O 0.24437(10) 0.64637(8) 0.52537(7) 0.01863(18) Uani 1 1 d . . . . .
C11A C 0.06564(13) 0.59282(11) 0.36698(9) 0.0184(2) Uani 1 1 d . . . . .
H111 H -0.0124 0.5822 0.4144 0.022 Uiso 1 1 calc R U . . .
H112 H 0.0799 0.6755 0.3577 0.022 Uiso 1 1 calc R U . . .
C12A C 0.01640(14) 0.51719(13) 0.26935(10) 0.0215(2) Uani 1 1 d . . . . .
F1A F 0.11705(10) 0.52114(11) 0.20040(7) 0.0380(2) Uani 1 1 d . . . . .
F2A F -0.09674(10) 0.54969(11) 0.22976(7) 0.0365(2) Uani 1 1 d . . . . .
F3A F -0.02272(14) 0.40450(9) 0.27603(8) 0.0428(3) Uani 1 1 d . . . . .
N1B N -0.06734(13) 0.86756(10) 1.08665(9) 0.0217(2) Uani 1 1 d . . . . .
C2B C -0.09004(17) 0.94950(14) 1.17770(11) 0.0268(3) Uani 1 1 d . . . . .
H25 H -0.1098 0.9056 1.2332 0.032 Uiso 1 1 calc R U . . .
H26 H -0.1748 0.9851 1.1671 0.032 Uiso 1 1 calc R U . . .
C3B C 0.03856(17) 1.04566(13) 1.20589(10) 0.0256(3) Uani 1 1 d . . . . .
H35 H 0.0200 1.0983 1.2675 0.031 Uiso 1 1 calc R U . . .
H36 H 0.1235 1.0111 1.2183 0.031 Uiso 1 1 calc R U . . .
N4B N 0.06572(13) 1.11301(11) 1.12337(9) 0.0217(2) Uani 1 1 d . . . . .
H45 H 0.079(2) 1.0670(19) 1.0659(16) 0.031(5) Uiso 1 1 d . . . . .
H46 H -0.015(3) 1.146(2) 1.1127(18) 0.044(6) Uiso 1 1 d . . . . .
C5B C 0.19217(17) 1.20848(13) 1.13773(13) 0.0305(3) Uani 1 1 d . . . . .
H55 H 0.2805 1.1745 1.1396 0.037 Uiso 1 1 calc R U . . .
H56 H 0.1863 1.2607 1.2021 0.037 Uiso 1 1 calc R U . . .
C6B C 0.19932(19) 1.27925(13) 1.05382(14) 0.0334(3) Uani 1 1 d . . . . .
H65 H 0.2855 1.3410 1.0653 0.040 Uiso 1 1 calc R U . . .
H66 H 0.1148 1.3186 1.0568 0.040 Uiso 1 1 calc R U . . .
C7B C 0.20420(17) 1.20809(14) 0.94929(13) 0.0312(3) Uani 1 1 d . . . . .
H75 H 0.2326 1.2627 0.9024 0.037 Uiso 1 1 calc R U . . .
H76 H 0.2788 1.1586 0.9491 0.037 Uiso 1 1 calc R U . . .
C10B C 0.04362(16) 0.79784(12) 1.10554(10) 0.0233(3) Uani 1 1 d . . . . .
H105 H 0.0015 0.7136 1.0923 0.028 Uiso 1 1 calc R U . . .
H106 H 0.0757 0.8190 1.1763 0.028 Uiso 1 1 calc R U . . .
P1B P 0.19701(4) 0.82366(3) 1.02730(3) 0.02068(8) Uani 1 1 d . . . . .
O11B O 0.15066(12) 0.77475(10) 0.92055(8) 0.0270(2) Uani 1 1 d . . . . .
O12B O 0.26719(11) 0.95053(9) 1.04762(8) 0.0260(2) Uani 1 1 d . . . . .
C11B C 0.3234(2) 0.74046(16) 1.07183(13) 0.0354(4) Uani 1 1 d . . . . .
H115 H 0.4209 0.7864 1.0714 0.043 Uiso 0.802(3) 1 calc R U P A 1
H116 H 0.3021 0.7343 1.1419 0.043 Uiso 0.802(3) 1 calc R U P A 1
H117 H 0.3978 0.7986 1.1125 0.043 Uiso 0.198(3) 1 calc R U P A 2
H118 H 0.2704 0.6939 1.1181 0.043 Uiso 0.198(3) 1 calc R U P A 2
C12B C 0.3250(3) 0.6220(2) 1.01664(15) 0.0301(4) Uani 0.802(3) 1 d . . P A 1
F125 F 0.19267(17) 0.55805(11) 1.00558(11) 0.0424(4) Uani 0.802(3) 1 d . . P A
1
F126 F 0.4043(2) 0.56348(15) 1.06587(11) 0.0455(4) Uani 0.802(3) 1 d . . P A 1
F127 F 0.3769(3) 0.6180(2) 0.92525(16) 0.0510(6) Uani 0.802(3) 1 d . . P A 1
C12X C 0.3919(10) 0.6683(8) 1.0125(7) 0.0294(17) Uani 0.198(3) 1 d . U P A 2
F12X F 0.4729(6) 0.7452(6) 0.9666(5) 0.0486(17) Uani 0.198(3) 1 d . U P A 2
F12Y F 0.4808(7) 0.6180(6) 1.0614(4) 0.0352(14) Uani 0.198(3) 1 d . U P A 2
F12Z F 0.3300(11) 0.5847(8) 0.9412(7) 0.052(2) Uani 0.198(3) 1 d . U P A 2
Cl1 Cl 0.75458(4) 1.09950(3) 0.65190(3) 0.02629(8) Uani 1 1 d . . . . .
Li1 Li 0.1724(3) 0.7694(2) 0.60921(18) 0.0207(4) Uani 1 1 d . . . . .
O1W O 0.26787(12) 0.78904(10) 0.74034(8) 0.0240(2) Uani 1 1 d . . . . .
H11W H 0.329(3) 0.844(2) 0.7613(18) 0.041(6) Uiso 1 1 d . . . . .
H12W H 0.229(3) 0.770(2) 0.788(2) 0.052(7) Uiso 1 1 d . . . . .
O2W O 0.23249(13) 0.92896(10) 0.57759(9) 0.0255(2) Uani 1 1 d . . . . .
H21W H 0.255(3) 0.924(2) 0.519(2) 0.050(7) Uiso 1 1 d . . . . .
H22W H 0.304(3) 0.965(2) 0.6050(18) 0.038(6) Uiso 1 1 d . . . . .
O3W O -0.03114(11) 0.75770(9) 0.58704(8) 0.02021(18) Uani 1 1 d . . . . .
H31W H -0.045(2) 0.790(2) 0.5474(17) 0.032(6) Uiso 1 1 d . . . . .
H32W H -0.090(2) 0.693(2) 0.5807(16) 0.034(5) Uiso 1 1 d . . . . .
O4W O -0.06933(13) 0.87644(11) 0.42949(9) 0.0279(2) Uani 1 1 d . . . . .
H41W H -0.097(3) 0.930(2) 0.4316(19) 0.046(7) Uiso 1 1 d . . . . .
H42W H 0.003(2) 0.8900(17) 0.4072(15) 0.020(4) Uiso 1 1 d . . . . .
O5W O 0.43728(14) 1.06168(13) 0.70530(10) 0.0406(3) Uani 1 1 d . . . . .
H51W H 0.4440 1.0373 0.7669 0.074(9) Uiso 1 1 d R . . . .
H52W H 0.5324 1.0680 0.6859 0.071(9) Uiso 1 1 d R . . . .
O6W O 0.54453(14) 1.02982(13) 1.12186(10) 0.0395(3) Uani 1 1 d . . . . .
H61W H 0.4433 1.0082 1.1056 0.084(10) Uiso 1 1 d R . . . .
H62W H 0.5988 1.0362 1.0668 0.093(12) Uiso 1 1 d 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
N1A C2A 1.4707(17) . ?
N1A C7A 1.4846(16) 2_666 ?
N1A C10A 1.4876(16) . ?
C2A C3A 1.5205(19) . ?
C2A H21 0.9900 . ?
C2A H22 0.9900 . ?
C3A N4A 1.4837(17) . ?
C3A H31 0.9900 . ?
C3A H32 0.9900 . ?
N4A C5A 1.4922(16) . ?
N4A H41 0.87(2) . ?
N4A H42 0.91(2) . ?
C5A C6A 1.5295(19) . ?
C5A H51 0.9900 . ?
C5A H52 0.9900 . ?
C6A C7A 1.5305(19) . ?
C6A H61 0.9900 . ?
C6A H62 0.9900 . ?
C7A N1A 1.4846(16) 2_666 ?
C7A H71 0.9900 . ?
C7A H72 0.9900 . ?
C10A P1A 1.8255(13) . ?
C10A H101 0.9900 . ?
C10A H102 0.9900 . ?
P1A O11A 1.5012(10) . ?
P1A O12A 1.5116(9) . ?
P1A C11A 1.8271(13) . ?
O12A Li1 1.908(3) . ?
C11A C12A 1.4959(18) . ?
C11A H111 0.9900 . ?
C11A H112 0.9900 . ?
C12A F3A 1.3349(17) . ?
C12A F1A 1.3419(16) . ?
C12A F2A 1.3424(16) . ?
N1B C7B 1.475(2) 2_577 ?
N1B C2B 1.4767(18) . ?
N1B C10B 1.4887(18) . ?
C2B C3B 1.516(2) . ?
C2B H25 0.9900 . ?
C2B H26 0.9900 . ?
C3B N4B 1.4850(19) . ?
C3B H35 0.9900 . ?
C3B H36 0.9900 . ?
N4B C5B 1.485(2) . ?
N4B H45 0.89(2) . ?
N4B H46 0.94(3) . ?
C5B C6B 1.524(2) . ?
C5B H55 0.9900 . ?
C5B H56 0.9900 . ?
C6B C7B 1.531(2) . ?
C6B H65 0.9900 . ?
C6B H66 0.9900 . ?
C7B N1B 1.475(2) 2_577 ?
C7B H75 0.9900 . ?
C7B H76 0.9900 . ?
C10B P1B 1.8204(15) . ?
C10B H105 0.9900 . ?
C10B H106 0.9900 . ?
P1B O12B 1.5071(12) . ?
P1B O11B 1.5081(11) . ?
P1B C11B 1.8365(16) . ?
C11B C12X 1.323(9) . ?
C11B C12B 1.470(3) . ?
C11B H115 0.9900 . ?
C11B H116 0.9900 . ?
C11B H117 0.9900 . ?
C11B H118 0.9900 . ?
C12B F127 1.338(3) . ?
C12B F125 1.343(3) . ?
C12B F126 1.353(2) . ?
C12X F12Z 1.317(13) . ?
C12X F12X 1.327(12) . ?
C12X F12Y 1.348(9) . ?
Li1 O3W 1.932(3) . ?
Li1 O1W 1.966(3) . ?
Li1 O2W 1.990(3) . ?
Li1 H31W 2.30(2) . ?
O1W H11W 0.81(3) . ?
O1W H12W 0.79(3) . ?
O2W H21W 0.82(3) . ?
O2W H22W 0.79(3) . ?
O3W H31W 0.74(2) . ?
O3W H32W 0.85(2) . ?
O4W H41W 0.71(3) . ?
O4W H42W 0.75(2) . ?
O5W H51W 0.9401 . ?
O5W H52W 0.9350 . ?
O6W H61W 0.9659 . ?
O6W H62W 0.9181 . ?

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
C2A N1A C7A 108.96(10) . 2_666 ?
C2A N1A C10A 110.56(10) . . ?
C7A N1A C10A 111.90(10) 2_666 . ?
N1A C2A C3A 112.46(10) . . ?
N1A C2A H21 109.1 . . ?
C3A C2A H21 109.1 . . ?
N1A C2A H22 109.1 . . ?
C3A C2A H22 109.1 . . ?
H21 C2A H22 107.8 . . ?
N4A C3A C2A 108.39(10) . . ?
N4A C3A H31 110.0 . . ?
C2A C3A H31 110.0 . . ?
N4A C3A H32 110.0 . . ?
C2A C3A H32 110.0 . . ?
H31 C3A H32 108.4 . . ?
C3A N4A C5A 116.54(10) . . ?
C3A N4A H41 108.0(13) . . ?
C5A N4A H41 103.6(13) . . ?
C3A N4A H42 108.8(13) . . ?
C5A N4A H42 108.1(13) . . ?
H41 N4A H42 111.8(18) . . ?
N4A C5A C6A 110.39(10) . . ?
N4A C5A H51 109.6 . . ?
C6A C5A H51 109.6 . . ?
N4A C5A H52 109.6 . . ?
C6A C5A H52 109.6 . . ?
H51 C5A H52 108.1 . . ?
C5A C6A C7A 115.38(11) . . ?
C5A C6A H61 108.4 . . ?
C7A C6A H61 108.4 . . ?
C5A C6A H62 108.4 . . ?
C7A C6A H62 108.4 . . ?
H61 C6A H62 107.5 . . ?
N1A C7A C6A 114.06(11) 2_666 . ?
N1A C7A H71 108.7 2_666 . ?
C6A C7A H71 108.7 . . ?
N1A C7A H72 108.7 2_666 . ?
C6A C7A H72 108.7 . . ?
H71 C7A H72 107.6 . . ?
N1A C10A P1A 110.02(8) . . ?
N1A C10A H101 109.7 . . ?
P1A C10A H101 109.7 . . ?
N1A C10A H102 109.7 . . ?
P1A C10A H102 109.7 . . ?
H101 C10A H102 108.2 . . ?
O11A P1A O12A 116.00(6) . . ?
O11A P1A C10A 109.20(6) . . ?
O12A P1A C10A 108.29(6) . . ?
O11A P1A C11A 111.29(6) . . ?
O12A P1A C11A 105.68(6) . . ?
C10A P1A C11A 105.86(6) . . ?
P1A O12A Li1 144.84(9) . . ?
C12A C11A P1A 117.14(9) . . ?
C12A C11A H111 108.0 . . ?
P1A C11A H111 108.0 . . ?
C12A C11A H112 108.0 . . ?
P1A C11A H112 108.0 . . ?
H111 C11A H112 107.3 . . ?
F3A C12A F1A 106.22(13) . . ?
F3A C12A F2A 106.45(12) . . ?
F1A C12A F2A 105.62(11) . . ?
F3A C12A C11A 113.01(11) . . ?
F1A C12A C11A 112.95(11) . . ?
F2A C12A C11A 112.04(12) . . ?
C7B N1B C2B 109.77(12) 2_577 . ?
C7B N1B C10B 111.74(12) 2_577 . ?
C2B N1B C10B 110.45(11) . . ?
N1B C2B C3B 112.11(12) . . ?
N1B C2B H25 109.2 . . ?
C3B C2B H25 109.2 . . ?
N1B C2B H26 109.2 . . ?
C3B C2B H26 109.2 . . ?
H25 C2B H26 107.9 . . ?
N4B C3B C2B 108.99(11) . . ?
N4B C3B H35 109.9 . . ?
C2B C3B H35 109.9 . . ?
N4B C3B H36 109.9 . . ?
C2B C3B H36 109.9 . . ?
H35 C3B H36 108.3 . . ?
C3B N4B C5B 115.83(12) . . ?
C3B N4B H45 111.9(14) . . ?
C5B N4B H45 105.6(14) . . ?
C3B N4B H46 109.3(15) . . ?
C5B N4B H46 107.6(15) . . ?
H45 N4B H46 106(2) . . ?
N4B C5B C6B 110.84(12) . . ?
N4B C5B H55 109.5 . . ?
C6B C5B H55 109.5 . . ?
N4B C5B H56 109.5 . . ?
C6B C5B H56 109.5 . . ?
H55 C5B H56 108.1 . . ?
C5B C6B C7B 114.93(13) . . ?
C5B C6B H65 108.5 . . ?
C7B C6B H65 108.5 . . ?
C5B C6B H66 108.5 . . ?
C7B C6B H66 108.5 . . ?
H65 C6B H66 107.5 . . ?
N1B C7B C6B 114.00(13) 2_577 . ?
N1B C7B H75 108.8 2_577 . ?
C6B C7B H75 108.8 . . ?
N1B C7B H76 108.8 2_577 . ?
C6B C7B H76 108.8 . . ?
H75 C7B H76 107.6 . . ?
N1B C10B P1B 111.43(9) . . ?
N1B C10B H105 109.3 . . ?
P1B C10B H105 109.3 . . ?
N1B C10B H106 109.3 . . ?
P1B C10B H106 109.3 . . ?
H105 C10B H106 108.0 . . ?
O12B P1B O11B 115.46(7) . . ?
O12B P1B C10B 111.00(6) . . ?
O11B P1B C10B 108.67(7) . . ?
O12B P1B C11B 106.83(8) . . ?
O11B P1B C11B 110.97(7) . . ?
C10B P1B C11B 103.21(8) . . ?
C12X C11B P1B 123.8(4) . . ?
C12B C11B P1B 117.20(13) . . ?
C12B C11B H115 108.0 . . ?
P1B C11B H115 108.0 . . ?
C12B C11B H116 108.0 . . ?
P1B C11B H116 108.0 . . ?
H115 C11B H116 107.2 . . ?
C12X C11B H117 106.4 . . ?
P1B C11B H117 106.4 . . ?
C12X C11B H118 106.4 . . ?
P1B C11B H118 106.4 . . ?
H117 C11B H118 106.5 . . ?
F127 C12B F125 106.3(2) . . ?
F127 C12B F126 106.55(19) . . ?
F125 C12B F126 106.27(19) . . ?
F127 C12B C11B 114.8(2) . . ?
F125 C12B C11B 111.23(18) . . ?
F126 C12B C11B 111.20(18) . . ?
F12Z C12X C11B 124.5(9) . . ?
F12Z C12X F12X 105.6(9) . . ?
C11B C12X F12X 99.3(7) . . ?
F12Z C12X F12Y 105.2(8) . . ?
C11B C12X F12Y 113.5(7) . . ?
F12X C12X F12Y 107.1(8) . . ?
O12A Li1 O3W 111.25(12) . . ?
O12A Li1 O1W 106.68(12) . . ?
O3W Li1 O1W 124.84(13) . . ?
O12A Li1 O2W 115.81(13) . . ?
O3W Li1 O2W 97.62(12) . . ?
O1W Li1 O2W 100.27(12) . . ?
O12A Li1 H31W 110.0(6) . . ?
O3W Li1 H31W 17.5(6) . . ?
O1W Li1 H31W 137.4(6) . . ?
O2W Li1 H31W 82.8(6) . . ?
Li1 O1W H11W 122.8(17) . . ?
Li1 O1W H12W 124(2) . . ?
H11W O1W H12W 106(3) . . ?
Li1 O2W H21W 109.4(19) . . ?
Li1 O2W H22W 115.1(17) . . ?
H21W O2W H22W 101(2) . . ?
Li1 O3W H31W 110.5(18) . . ?
Li1 O3W H32W 123.4(15) . . ?
H31W O3W H32W 110(2) . . ?
H41W O4W H42W 103(3) . . ?
H51W O5W H52W 101.0 . . ?
H61W O6W H62W 112.7 . . ?

_refine_diff_density_max         1.291
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.064



####################################################################### 
# 
# 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_pf2b2cam2tfa2
_database_code_depnum_ccdc_archive 'CCDC 2262048'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2023-05-10 deposited with the CCDC.	2023-06-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT355_pf2b2cam2tfa2       
;
PROBLEM: Long   O-H (X0.82,N0.98A)  O11B     - H11B     .       1.17 Ang.
RESPONSE: strong hydrogen bonds influencing OH distances
;
# Added during the CSD deposition process: Wednesday 10 May 2023 02:02 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H44 F6 N4 O4 P2, 6(C2 H F3 O2), 2(H2 O)'
_chemical_formula_sum            'C42 H54 F24 N4 O18 P2'
_chemical_formula_weight         1420.83

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'
F F 0.0727 0.0534 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   12.3608(4)
_cell_length_b                   11.3394(4)
_cell_length_c                   21.7985(8)
_cell_angle_alpha                90
_cell_angle_beta                 90.019(2)
_cell_angle_gamma                90
_cell_volume                     3055.37(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9918
_cell_measurement_theta_min      3.5758
_cell_measurement_theta_max      77.1933

_exptl_crystal_description       bar
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_F_000             1448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.057
_exptl_absorpt_coefficient_mu    1.943
_shelx_estimated_absorpt_T_min   0.659
_shelx_estimated_absorpt_T_max   0.897
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            55783
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.576
_diffrn_reflns_theta_max         77.604
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6464
_reflns_number_gt                5214
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1328)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1215P)²+3.8655P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6464
_refine_ls_number_parameters     489
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0729
_refine_ls_wR_factor_ref         0.2216
_refine_ls_wR_factor_gt          0.2061
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.45920(16) 0.61587(19) 0.40694(9) 0.0253(4) Uani 1 1 d . . . . .
C2 C 0.4149(2) 0.7086(2) 0.44623(12) 0.0285(5) Uani 1 1 d . . . . .
H21 H 0.4150 0.7839 0.4232 0.034 Uiso 1 1 calc R U . . .
H22 H 0.4627 0.7185 0.4823 0.034 Uiso 1 1 calc R U . . .
C3 C 0.3007(2) 0.6840(2) 0.46842(13) 0.0308(5) Uani 1 1 d . . . . .
H31 H 0.2846 0.7373 0.5032 0.037 Uiso 1 1 calc R U . . .
H32 H 0.2495 0.7030 0.4350 0.037 Uiso 1 1 calc R U . . .
N4 N 0.28161(16) 0.55870(19) 0.48859(10) 0.0260(4) Uani 1 1 d . . . . .
H41 H 0.3020 0.5054 0.4539 0.031 Uiso 1 1 calc R U . . .
C5 C 0.3497(2) 0.5262(2) 0.54330(12) 0.0282(5) Uani 1 1 d . . . . .
H51 H 0.3213 0.5670 0.5801 0.034 Uiso 1 1 calc R U . . .
H52 H 0.4248 0.5536 0.5365 0.034 Uiso 1 1 calc R U . . .
C6 C 0.3503(2) 0.3939(2) 0.55480(13) 0.0317(6) Uani 1 1 d . . . . .
H61 H 0.2761 0.3673 0.5648 0.038 Uiso 1 1 calc R U . . .
H62 H 0.3736 0.3525 0.5170 0.038 Uiso 1 1 calc R U . . .
C7 C 0.4259(2) 0.3616(3) 0.60717(12) 0.0313(6) Uani 1 1 d . . . . .
H71 H 0.4054 0.4076 0.6440 0.038 Uiso 1 1 calc R U . . .
H72 H 0.4166 0.2770 0.6170 0.038 Uiso 1 1 calc R U . . .
C10 C 0.3970(2) 0.5970(2) 0.34989(12) 0.0314(5) Uani 1 1 d . . . . .
H101 H 0.4348 0.6329 0.3145 0.038 Uiso 1 1 calc R U . . .
H102 H 0.3241 0.6327 0.3533 0.038 Uiso 1 1 calc R U . . .
P1 P 0.38654(6) 0.43897(6) 0.34010(3) 0.0311(2) Uani 1 1 d . . . . .
O11 O 0.32406(14) 0.39304(17) 0.39465(9) 0.0328(4) Uani 1 1 d . . . . .
O12 O 0.49631(18) 0.3839(2) 0.33183(10) 0.0439(5) Uani 1 1 d . . . . .
C11 C 0.3087(4) 0.4218(4) 0.27004(19) 0.0692(12) Uani 1 1 d . . . . .
H111 H 0.2413 0.4685 0.2741 0.083 Uiso 1 1 calc R U . . .
H112 H 0.3507 0.4564 0.2358 0.083 Uiso 1 1 calc R U . . .
C12 C 0.2789(3) 0.3004(4) 0.25312(17) 0.0583(10) Uani 1 1 d . . . . .
F121 F 0.3591(3) 0.2244(3) 0.25358(18) 0.1116(12) Uani 1 1 d . . . . .
F122 F 0.2079(3) 0.2576(4) 0.29167(14) 0.1211(15) Uani 1 1 d . . . . .
F123 F 0.2368(3) 0.2919(3) 0.19709(12) 0.0963(10) Uani 1 1 d . . . . .
C20 C 0.16216(19) 0.5393(3) 0.50273(12) 0.0316(6) Uani 1 1 d . . . . .
H201 H 0.1516 0.4565 0.5159 0.038 Uiso 1 1 calc R U . . .
H202 H 0.1411 0.5908 0.5374 0.038 Uiso 1 1 calc R U . . .
C21 C 0.08864(19) 0.5642(2) 0.44901(12) 0.0300(5) Uani 1 1 d . . . . .
C22 C 0.0370(2) 0.6724(3) 0.44355(13) 0.0346(6) Uani 1 1 d . . . . .
H221 H 0.0485 0.7317 0.4736 0.041 Uiso 1 1 calc R U . . .
C23 C -0.0318(2) 0.6942(3) 0.39399(15) 0.0419(7) Uani 1 1 d . . . . .
H231 H -0.0662 0.7688 0.3901 0.050 Uiso 1 1 calc R U . . .
C24 C -0.0500(2) 0.6073(3) 0.35052(14) 0.0436(7) Uani 1 1 d . . . . .
H241 H -0.0967 0.6221 0.3168 0.052 Uiso 1 1 calc R U . . .
C25 C 0.0003(2) 0.4989(3) 0.35650(14) 0.0421(7) Uani 1 1 d . . . . .
H251 H -0.0126 0.4389 0.3269 0.050 Uiso 1 1 calc R U . . .
C26 C 0.0693(2) 0.4772(3) 0.40542(14) 0.0352(6) Uani 1 1 d . . . . .
H261 H 0.1035 0.4025 0.4092 0.042 Uiso 1 1 calc R U . . .
C1A C 0.2809(4) 0.1320(3) 0.4558(2) 0.0646(11) Uani 1 1 d . . . . .
O11A O 0.2266(2) 0.2199(2) 0.43738(12) 0.0518(6) Uani 1 1 d . . . . .
H11A H 0.2623 0.2952 0.4095 0.078 Uiso 1 1 d R U . . .
O12A O 0.3743(3) 0.1101(4) 0.4490(2) 0.1083(15) Uani 1 1 d . . . . .
C2A C 0.2138(7) 0.0465(4) 0.4947(3) 0.104(2) Uani 1 1 d . . . . .
F21A F 0.2140(6) 0.0832(4) 0.5525(2) 0.165(2) Uani 1 1 d . . . . .
F22A F 0.2477(7) -0.0550(3) 0.4940(3) 0.233(4) Uani 1 1 d . . . . .
F23A F 0.1141(5) 0.0455(7) 0.4806(4) 0.237(4) Uani 1 1 d . . . . .
C1B C 0.8157(3) 0.1671(3) 0.36338(18) 0.0560(9) Uani 1 1 d . . . . .
O11B O 0.7294(3) 0.1209(3) 0.34283(15) 0.0757(9) Uani 1 1 d . . . . .
H11B H 0.6571 0.1451 0.3753 0.113 Uiso 1 1 d R U . . .
O12B O 0.8250(3) 0.2348(3) 0.40405(16) 0.0841(10) Uani 1 1 d . . . . .
C2B C 0.9187(5) 0.1198(5) 0.3326(3) 0.0934(19) Uani 1 1 d . . . . .
F21B F 1.0049(11) 0.1731(17) 0.3494(9) 0.146(7) Uani 0.587(18) 1 d . . P A 1
F22B F 0.9126(6) 0.0131(6) 0.3205(7) 0.103(5) Uani 0.587(18) 1 d . . P A 1
F23B F 0.8973(18) 0.1602(17) 0.2682(7) 0.244(11) Uani 0.587(18) 1 d . . P A 1
F24B F 0.9576(11) 0.0228(12) 0.3699(8) 0.112(6) Uani 0.413(18) 1 d . . P A 2
F25B F 0.9164(9) 0.079(2) 0.2833(8) 0.135(8) Uani 0.413(18) 1 d . . P A 2
F26B F 0.9877(16) 0.1871(15) 0.3245(15) 0.148(11) Uani 0.413(18) 1 d . . P A 2
C1C C 0.7139(6) 0.4065(5) 0.2532(4) 0.0445(15) Uani 0.645(8) 1 d . . P B 3
O11C O 0.6155(4) 0.3770(5) 0.2376(2) 0.0581(14) Uani 0.645(8) 1 d . . P B 3
H11C H 0.5804 0.3866 0.2760 0.087 Uiso 1 1 d R U . . .
O12C O 0.7452(4) 0.4312(5) 0.30328(19) 0.0676(16) Uani 0.645(8) 1 d . . P B 3
C1D C 0.6655(12) 0.4102(10) 0.2202(6) 0.047(3) Uani 0.355(8) 1 d . . P B 4
O11D O 0.6772(8) 0.4101(8) 0.2778(5) 0.055(2) Uani 0.355(8) 1 d . . P B 4
O12D O 0.5863(7) 0.4041(12) 0.1902(4) 0.091(4) Uani 0.355(8) 1 d . . P B 4
C2C C 0.7859(4) 0.4097(5) 0.1950(2) 0.0737(14) Uani 1 1 d . . . . .
F21C F 0.7856(5) 0.3219(7) 0.1629(3) 0.087(2) Uani 0.645(8) 1 d . . P B 3
F22C F 0.7688(10) 0.5072(8) 0.1611(5) 0.171(4) Uani 0.645(8) 1 d . . P B 3
F23C F 0.8904(6) 0.4128(11) 0.2172(4) 0.129(4) Uani 0.645(8) 1 d . . P B 3
F21D F 0.8194(10) 0.2813(17) 0.2002(8) 0.148(7) Uani 0.355(8) 1 d . . P B 4
F22D F 0.7667(10) 0.413(2) 0.1373(6) 0.130(5) Uani 0.355(8) 1 d . . P B 4
F23D F 0.8493(10) 0.4773(11) 0.2114(7) 0.089(4) Uani 0.355(8) 1 d . . P B 4
O1W O 0.5637(2) 0.2007(3) 0.39812(14) 0.0689(8) Uani 1 1 d . . . . .
H11W H 0.5207 0.2436 0.3677 0.103 Uiso 1 1 d R U . . .
H12W H 0.5022 0.1331 0.4110 0.103 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C2 1.463(3) . ?
N1 C7 1.475(3) 3_666 ?
N1 C10 1.478(3) . ?
C2 C3 1.517(3) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.506(3) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C5 1.505(3) . ?
N4 C20 1.524(3) . ?
N4 H41 1.0000 . ?
C5 C6 1.522(4) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 C7 1.520(4) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
C7 N1 1.475(3) 3_666 ?
C7 H71 0.9900 . ?
C7 H72 0.9900 . ?
C10 P1 1.809(3) . ?
C10 H101 0.9900 . ?
C10 H102 0.9900 . ?
P1 O12 1.504(2) . ?
P1 O11 1.5107(19) . ?
P1 C11 1.815(4) . ?
C11 C12 1.472(6) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 F122 1.309(5) . ?
C12 F121 1.312(5) . ?
C12 F123 1.331(4) . ?
C20 C21 1.509(4) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
C21 C22 1.388(4) . ?
C21 C26 1.391(4) . ?
C22 C23 1.397(4) . ?
C22 H221 0.9500 . ?
C23 C24 1.385(5) . ?
C23 H231 0.9500 . ?
C24 C25 1.384(5) . ?
C24 H241 0.9500 . ?
C25 C26 1.387(4) . ?
C25 H251 0.9500 . ?
C26 H261 0.9500 . ?
C1A O12A 1.191(6) . ?
C1A O11A 1.267(5) . ?
C1A C2A 1.532(7) . ?
O11A H11A 1.1376 . ?
C2A F22A 1.225(6) . ?
C2A F23A 1.270(10) . ?
C2A F21A 1.326(8) . ?
C1B O12B 1.178(5) . ?
C1B O11B 1.270(5) . ?
C1B C2B 1.536(6) . ?
O11B H11B 1.1731 . ?
C2B F26B 1.159(14) . ?
C2B F25B 1.169(11) . ?
C2B F22B 1.240(8) . ?
C2B F21B 1.280(14) . ?
C2B F24B 1.450(11) . ?
C2B F23B 1.50(2) . ?
C1C O12C 1.192(9) . ?
C1C O11C 1.306(8) . ?
C1C C2C 1.549(9) . ?
O11C H11C 0.9475 . ?
C1D O12D 1.179(16) . ?
C1D O11D 1.263(15) . ?
C1D C2C 1.587(16) . ?
O11D H11C 1.2260 . ?
C2C F23D 1.154(10) . ?
C2C F21C 1.217(7) . ?
C2C F22D 1.280(14) . ?
C2C F22C 1.346(9) . ?
C2C F23C 1.380(9) . ?
C2C F21D 1.518(18) . ?
O1W H11W 0.9793 . ?
O1W H12W 1.1155 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C7 111.0(2) . 3_666 ?
C2 N1 C10 113.7(2) . . ?
C7 N1 C10 110.5(2) 3_666 . ?
N1 C2 C3 113.8(2) . . ?
N1 C2 H21 108.8 . . ?
C3 C2 H21 108.8 . . ?
N1 C2 H22 108.8 . . ?
C3 C2 H22 108.8 . . ?
H21 C2 H22 107.7 . . ?
N4 C3 C2 114.4(2) . . ?
N4 C3 H31 108.7 . . ?
C2 C3 H31 108.7 . . ?
N4 C3 H32 108.7 . . ?
C2 C3 H32 108.7 . . ?
H31 C3 H32 107.6 . . ?
C5 N4 C3 112.0(2) . . ?
C5 N4 C20 110.25(19) . . ?
C3 N4 C20 110.34(19) . . ?
C5 N4 H41 108.1 . . ?
C3 N4 H41 108.1 . . ?
C20 N4 H41 108.1 . . ?
N4 C5 C6 112.0(2) . . ?
N4 C5 H51 109.2 . . ?
C6 C5 H51 109.2 . . ?
N4 C5 H52 109.2 . . ?
C6 C5 H52 109.2 . . ?
H51 C5 H52 107.9 . . ?
C7 C6 C5 111.4(2) . . ?
C7 C6 H61 109.4 . . ?
C5 C6 H61 109.4 . . ?
C7 C6 H62 109.4 . . ?
C5 C6 H62 109.4 . . ?
H61 C6 H62 108.0 . . ?
N1 C7 C6 113.2(2) 3_666 . ?
N1 C7 H71 108.9 3_666 . ?
C6 C7 H71 108.9 . . ?
N1 C7 H72 108.9 3_666 . ?
C6 C7 H72 108.9 . . ?
H71 C7 H72 107.8 . . ?
N1 C10 P1 106.27(17) . . ?
N1 C10 H101 110.5 . . ?
P1 C10 H101 110.5 . . ?
N1 C10 H102 110.5 . . ?
P1 C10 H102 110.5 . . ?
H101 C10 H102 108.7 . . ?
O12 P1 O11 114.37(12) . . ?
O12 P1 C10 111.15(13) . . ?
O11 P1 C10 106.56(12) . . ?
O12 P1 C11 109.4(2) . . ?
O11 P1 C11 110.74(19) . . ?
C10 P1 C11 104.06(16) . . ?
C12 C11 P1 116.3(3) . . ?
C12 C11 H111 108.2 . . ?
P1 C11 H111 108.2 . . ?
C12 C11 H112 108.2 . . ?
P1 C11 H112 108.2 . . ?
H111 C11 H112 107.4 . . ?
F122 C12 F121 105.0(4) . . ?
F122 C12 F123 107.4(3) . . ?
F121 C12 F123 104.8(3) . . ?
F122 C12 C11 110.7(4) . . ?
F121 C12 C11 115.1(4) . . ?
F123 C12 C11 113.3(4) . . ?
C21 C20 N4 113.5(2) . . ?
C21 C20 H201 108.9 . . ?
N4 C20 H201 108.9 . . ?
C21 C20 H202 108.9 . . ?
N4 C20 H202 108.9 . . ?
H201 C20 H202 107.7 . . ?
C22 C21 C26 119.3(3) . . ?
C22 C21 C20 120.6(3) . . ?
C26 C21 C20 120.1(2) . . ?
C21 C22 C23 120.2(3) . . ?
C21 C22 H221 119.9 . . ?
C23 C22 H221 119.9 . . ?
C24 C23 C22 120.1(3) . . ?
C24 C23 H231 120.0 . . ?
C22 C23 H231 120.0 . . ?
C25 C24 C23 119.7(3) . . ?
C25 C24 H241 120.2 . . ?
C23 C24 H241 120.2 . . ?
C24 C25 C26 120.4(3) . . ?
C24 C25 H251 119.8 . . ?
C26 C25 H251 119.8 . . ?
C25 C26 C21 120.3(3) . . ?
C25 C26 H261 119.8 . . ?
C21 C26 H261 119.8 . . ?
O12A C1A O11A 129.7(4) . . ?
O12A C1A C2A 117.5(5) . . ?
O11A C1A C2A 112.7(4) . . ?
C1A O11A H11A 123.7 . . ?
F22A C2A F23A 108.7(8) . . ?
F22A C2A F21A 107.9(6) . . ?
F23A C2A F21A 103.5(6) . . ?
F22A C2A C1A 113.7(5) . . ?
F23A C2A C1A 113.4(6) . . ?
F21A C2A C1A 109.0(6) . . ?
O12B C1B O11B 128.0(4) . . ?
O12B C1B C2B 118.4(4) . . ?
O11B C1B C2B 113.4(4) . . ?
C1B O11B H11B 109.3 . . ?
F26B C2B F25B 97.9(16) . . ?
F22B C2B F21B 124.9(11) . . ?
F26B C2B F24B 109.9(16) . . ?
F25B C2B F24B 103.0(14) . . ?
F22B C2B F23B 95.1(8) . . ?
F21B C2B F23B 105.7(12) . . ?
F26B C2B C1B 116.5(10) . . ?
F25B C2B C1B 121.3(9) . . ?
F22B C2B C1B 112.6(5) . . ?
F21B C2B C1B 113.6(9) . . ?
F24B C2B C1B 107.1(5) . . ?
F23B C2B C1B 99.0(8) . . ?
O12C C1C O11C 126.8(7) . . ?
O12C C1C C2C 124.0(6) . . ?
O11C C1C C2C 109.2(7) . . ?
C1C O11C H11C 99.7 . . ?
O12D C1D O11D 130.2(16) . . ?
O12D C1D C2C 125.9(11) . . ?
O11D C1D C2C 103.8(11) . . ?
C1D O11D H11C 81.7 . . ?
F23D C2C F22D 114.2(11) . . ?
F21C C2C F22C 110.9(7) . . ?
F21C C2C F23C 103.0(7) . . ?
F22C C2C F23C 108.5(8) . . ?
F23D C2C F21D 115.4(11) . . ?
F22D C2C F21D 98.9(11) . . ?
F21C C2C C1C 116.7(5) . . ?
F22C C2C C1C 112.2(5) . . ?
F23C C2C C1C 104.5(5) . . ?
F23D C2C C1D 121.8(8) . . ?
F22D C2C C1D 99.7(8) . . ?
F21D C2C C1D 103.5(7) . . ?
H11W O1W H12W 98.2 . . ?

_refine_diff_density_max         0.917
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.078



####################################################################### 
# 
# 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_cute2pf2
_database_code_depnum_ccdc_archive 'CCDC 2262041'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2023-05-10 deposited with the CCDC.	2023-06-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT602_cute2pf2            
;
PROBLEM: Solvent Accessible VOID(S) in Structure ........          ! Check
RESPONSE: no significant maxima in electron density map present
;
# Added during the CSD deposition process: Wednesday 10 May 2023 02:02 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C34 H47.40 Cu2 F6.60 N4 O8 P2, 0.5(C3 H6 O), 4(H2 O)'
_chemical_formula_sum            'C35.50 H58.40 Cu2 F6.60 N4 O12.50 P2'
_chemical_formula_weight         1055.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   36.5804(9)
_cell_length_b                   36.5804(9)
_cell_length_c                   15.8953(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     21269.9(12)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9769
_cell_measurement_theta_min      2.2270
_cell_measurement_theta_max      25.8790

_exptl_crystal_description       bar
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_F_000             8749
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.051
_exptl_absorpt_coefficient_mu    0.936
_shelx_estimated_absorpt_T_min   0.853
_shelx_estimated_absorpt_T_max   0.954
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            105574
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.227
_diffrn_reflns_theta_max         26.025
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10478
_reflns_number_gt                8168
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Instrument Service vV6.2.1'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 758)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0658P)²+89.1438P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10478
_refine_ls_number_parameters     588
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1473
_refine_ls_wR_factor_gt          0.1366
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.87858(2) 0.56729(2) 0.32125(3) 0.01869(12) Uani 1 1 d . . . . .
N1 N 0.82368(8) 0.58116(8) 0.34401(18) 0.0208(6) Uani 1 1 d . . . . .
C2 C 0.81914(10) 0.57957(11) 0.4375(2) 0.0259(8) Uani 1 1 d . . . . .
H21 H 0.8144 0.5541 0.4554 0.031 Uiso 1 1 calc R U . . .
H22 H 0.7981 0.5949 0.4549 0.031 Uiso 1 1 calc R U . . .
C3 C 0.85361(10) 0.59340(10) 0.4779(2) 0.0259(8) Uani 1 1 d . . . . .
H31 H 0.8587 0.6187 0.4588 0.031 Uiso 1 1 calc R U . . .
H32 H 0.8508 0.5937 0.5398 0.031 Uiso 1 1 calc R U . . .
N4 N 0.88436(8) 0.56905(8) 0.45407(18) 0.0212(6) Uani 1 1 d . . . . .
C5 C 0.91945(10) 0.58692(10) 0.4807(2) 0.0249(8) Uani 1 1 d . . . . .
H51 H 0.9204 0.5876 0.5430 0.030 Uiso 1 1 calc R U . . .
H52 H 0.9195 0.6125 0.4604 0.030 Uiso 1 1 calc R U . . .
C6 C 0.95344(10) 0.56800(11) 0.4486(2) 0.0264(8) Uani 1 1 d . . . . .
H61 H 0.9515 0.5415 0.4608 0.032 Uiso 1 1 calc R U . . .
H62 H 0.9749 0.5775 0.4796 0.032 Uiso 1 1 calc R U . . .
C7 C 0.95975(10) 0.57309(11) 0.3554(2) 0.0249(8) Uani 1 1 d . . . . .
H71 H 0.9589 0.5996 0.3427 0.030 Uiso 1 1 calc R U . . .
H72 H 0.9847 0.5644 0.3418 0.030 Uiso 1 1 calc R U . . .
N8 N 0.93324(8) 0.55396(8) 0.29874(18) 0.0209(6) Uani 1 1 d . . . . .
C9 C 0.94079(10) 0.56629(10) 0.2106(2) 0.0231(8) Uani 1 1 d . . . . .
H91 H 0.9673 0.5708 0.2035 0.028 Uiso 1 1 calc R U . . .
H92 H 0.9334 0.5470 0.1705 0.028 Uiso 1 1 calc R U . . .
C10 C 0.91998(10) 0.60060(11) 0.1928(2) 0.0260(8) Uani 1 1 d . . . . .
H101 H 0.9282 0.6202 0.2314 0.031 Uiso 1 1 calc R U . . .
H102 H 0.9250 0.6086 0.1344 0.031 Uiso 1 1 calc R U . . .
N11 N 0.88012(8) 0.59457(8) 0.20370(19) 0.0212(6) Uani 1 1 d . . . . .
C12 C 0.86144(11) 0.63087(10) 0.2066(2) 0.0265(8) Uani 1 1 d . . . . .
H121 H 0.8645 0.6430 0.1514 0.032 Uiso 1 1 calc R U . . .
H122 H 0.8736 0.6463 0.2494 0.032 Uiso 1 1 calc R U . . .
C13 C 0.82104(11) 0.62873(10) 0.2269(2) 0.0276(8) Uani 1 1 d . . . . .
H131 H 0.8095 0.6102 0.1899 0.033 Uiso 1 1 calc R U . . .
H132 H 0.8096 0.6526 0.2142 0.033 Uiso 1 1 calc R U . . .
C14 C 0.81325(11) 0.61891(10) 0.3178(2) 0.0270(8) Uani 1 1 d . . . . .
H141 H 0.8263 0.6365 0.3543 0.032 Uiso 1 1 calc R U . . .
H142 H 0.7868 0.6221 0.3282 0.032 Uiso 1 1 calc R U . . .
C15 C 0.79856(9) 0.55353(10) 0.3045(2) 0.0223(7) Uani 1 1 d . . . . .
H151 H 0.7923 0.5614 0.2467 0.027 Uiso 1 1 calc R U . . .
H152 H 0.7756 0.5521 0.3374 0.027 Uiso 1 1 calc R U . . .
P1 P 0.82001(2) 0.50821(2) 0.30084(5) 0.01861(19) Uani 1 1 d . . . . .
O11 O 0.85979(6) 0.51601(6) 0.28226(16) 0.0225(5) Uani 1 1 d . . . . .
O12 O 0.81100(7) 0.48584(7) 0.37596(15) 0.0265(6) Uani 1 1 d . . . . .
C16 C 0.80246(10) 0.48696(10) 0.2050(2) 0.0223(7) Uani 1 1 d . . . . .
H161 H 0.8014 0.5059 0.1605 0.027 Uiso 1 1 calc R U . . .
H162 H 0.8202 0.4682 0.1865 0.027 Uiso 1 1 calc R U . . .
C17 C 0.76604(12) 0.46960(12) 0.2112(2) 0.0341(10) Uani 1 1 d . . . . .
F1 F 0.74049(7) 0.49298(9) 0.23849(19) 0.0556(8) Uani 1 1 d . . . . .
F2 F 0.76504(9) 0.44089(7) 0.26322(16) 0.0529(8) Uani 1 1 d . . . . .
F3 F 0.75403(8) 0.45645(9) 0.13688(16) 0.0578(8) Uani 1 1 d . . . . .
C18 C 0.93690(9) 0.51343(10) 0.3043(2) 0.0205(7) Uani 1 1 d . . . . .
H181 H 0.9203 0.5027 0.2618 0.025 Uiso 1 1 calc R U . . .
H182 H 0.9275 0.5060 0.3602 0.025 Uiso 1 1 calc R U . . .
P2 P 0.98171(2) 0.49171(3) 0.29075(6) 0.0205(2) Uani 1 1 d . . . . .
O21 O 1.00136(7) 0.50764(7) 0.21651(16) 0.0256(6) Uani 1 1 d . . . . .
O22 O 1.00146(7) 0.49060(7) 0.37305(16) 0.0264(6) Uani 1 1 d . . . . .
C19 C 0.96571(11) 0.44535(11) 0.2648(3) 0.0300(9) Uani 1 1 d . . . . .
H191 H 0.9418 0.4415 0.2928 0.036 Uiso 1 1 calc R U . . .
H192 H 0.9615 0.4441 0.2034 0.036 Uiso 1 1 calc R U . . .
C20 C 0.99019(14) 0.41488(13) 0.2885(3) 0.0438(11) Uani 1 1 d . . . . .
F4 F 0.99191(11) 0.40881(8) 0.3706(2) 0.0714(10) Uani 1 1 d . . . . .
F5 F 1.02474(8) 0.42003(8) 0.2621(2) 0.0630(9) Uani 1 1 d . . . . .
F6 F 0.97901(10) 0.38301(8) 0.2543(2) 0.0667(9) Uani 1 1 d . . . . .
C30 C 0.88059(10) 0.53245(10) 0.4968(2) 0.0221(7) Uani 1 1 d . . . . .
H301 H 0.9019 0.5172 0.4811 0.027 Uiso 1 1 calc R U . . .
H302 H 0.8585 0.5202 0.4745 0.027 Uiso 1 1 calc R U . . .
C31 C 0.87791(10) 0.53341(10) 0.5918(2) 0.0220(7) Uani 1 1 d . . . . .
C32 C 0.84442(10) 0.53818(11) 0.6321(2) 0.0269(8) Uani 1 1 d . . . . .
H321 H 0.8230 0.5420 0.5996 0.032 Uiso 1 1 calc R U . . .
C33 C 0.84208(11) 0.53741(12) 0.7194(3) 0.0321(9) Uani 1 1 d . . . . .
H331 H 0.8192 0.5411 0.7463 0.038 Uiso 1 1 calc R U . . .
C34 C 0.87302(12) 0.53123(12) 0.7670(2) 0.0356(10) Uani 1 1 d . . . . .
H341 H 0.8714 0.5304 0.8267 0.043 Uiso 1 1 calc R U . . .
C35 C 0.90639(12) 0.52625(12) 0.7279(3) 0.0346(10) Uani 1 1 d . . . . .
H351 H 0.9277 0.5218 0.7606 0.042 Uiso 1 1 calc R U . . .
C36 C 0.90883(10) 0.52768(11) 0.6409(2) 0.0267(8) Uani 1 1 d . . . . .
H361 H 0.9319 0.5247 0.6146 0.032 Uiso 1 1 calc R U . . .
C40 C 0.86478(10) 0.57139(10) 0.1332(2) 0.0233(8) Uani 1 1 d . . . . .
H401 H 0.8775 0.5475 0.1336 0.028 Uiso 1 1 calc R U . . .
H402 H 0.8386 0.5667 0.1448 0.028 Uiso 1 1 calc R U . . .
C41 C 0.86814(11) 0.58776(10) 0.0462(2) 0.0253(8) Uani 1 1 d . . . . .
C42 C 0.84053(12) 0.60974(11) 0.0137(3) 0.0331(9) Uani 1 1 d . . . . .
H421 H 0.8195 0.6148 0.0468 0.040 Uiso 1 1 calc R U . . .
C43 C 0.84348(15) 0.62437(13) -0.0663(3) 0.0461(12) Uani 1 1 d . . . . .
H431 H 0.8247 0.6398 -0.0872 0.055 Uiso 1 1 calc R U . . .
C44 C 0.87357(16) 0.61680(14) -0.1161(3) 0.0519(13) Uani 1 1 d . . . . .
H441 H 0.8753 0.6267 -0.1712 0.062 Uiso 1 1 calc R U . . .
C45 C 0.90121(15) 0.59465(14) -0.0850(3) 0.0467(12) Uani 1 1 d . . . . .
H451 H 0.9220 0.5893 -0.1187 0.056 Uiso 1 1 calc R U . . .
C46 C 0.89838(12) 0.58037(12) -0.0046(3) 0.0348(9) Uani 1 1 d . . . . .
H461 H 0.9174 0.5652 0.0164 0.042 Uiso 1 1 calc R U . . .
Cu2 Cu 0.99975(2) 0.50260(2) 0.08395(3) 0.02743(13) Uani 1 1 d . . . . .
O11A O 0.94742(8) 0.49088(10) -0.06883(18) 0.0426(8) Uani 1 1 d . . . . .
O12A O 0.94641(7) 0.49478(8) 0.07175(17) 0.0329(6) Uani 1 1 d . . . . .
C1A C 0.93151(11) 0.48910(11) 0.0010(3) 0.0308(9) Uani 1 1 d . . . . .
C2A C 0.89160(12) 0.47915(15) -0.0002(3) 0.0449(12) Uani 1 1 d . . . . .
H21A H 0.8792 0.4910 -0.0477 0.067 Uiso 0.9 1 d R U P A 1
H22A H 0.8799 0.4866 0.0525 0.067 Uiso 0.9 1 d R U P A 1
H23A H 0.8889 0.4523 -0.0063 0.067 Uiso 0.9 1 d R U P A 1
F21A F 0.8781(7) 0.4788(7) -0.0680(17) 0.045(6) Uiso 0.1 1 d . . P B 2
F22A F 0.8773(6) 0.4810(6) 0.0664(15) 0.034(5) Uiso 0.1 1 d . . P B 2
F23A F 0.8989(7) 0.4349(7) 0.0028(17) 0.043(6) Uiso 0.1 1 d . . P B 2
O11B O 1.00453(10) 0.44882(8) 0.07996(18) 0.0439(8) Uani 1 1 d . . . . .
O12B O 1.00553(8) 0.44452(8) -0.06021(17) 0.0351(7) Uani 1 1 d . . . . .
C1B C 1.00480(11) 0.43130(12) 0.0127(3) 0.0319(9) Uani 1 1 d . . . . .
C2B C 1.00347(15) 0.39001(13) 0.0203(3) 0.0497(12) Uani 1 1 d . . . . .
H21B H 0.9774 0.3815 0.0237 0.074 Uiso 0.9 1 d R U P C 1
H22B H 1.0161 0.3815 0.0706 0.074 Uiso 0.9 1 d R U P C 1
H23B H 1.0144 0.3782 -0.0297 0.074 Uiso 0.9 1 d R U P C 1
F21B F 1.0135(5) 0.3712(5) -0.0444(12) 0.020(4) Uiso 0.1 1 d . . P D 2
F22B F 1.0160(5) 0.3757(5) 0.0893(12) 0.017(4) Uiso 0.1 1 d . . P D 2
F23B F 0.9640(6) 0.3814(6) 0.0258(15) 0.033(5) Uiso 0.1 1 d . . P D 2
O1W O 1.03882(7) 0.53461(8) 0.48574(18) 0.0367(7) Uani 1 1 d . . . . .
H11W H 1.0279 0.5297 0.5293 0.044 Uiso 1 1 d R U . . .
H12W H 1.0309 0.5212 0.4461 0.044 Uiso 1 1 d R U . . .
O2W O 1.05643(18) 0.56761(17) 0.2399(4) 0.122(2) Uani 1 1 d . . . . .
H21W H 1.0438 0.5503 0.2176 0.146 Uiso 1 1 d R U . . .
H22W H 1.0733 0.5717 0.2040 0.146 Uiso 1 1 d R U . . .
O3W O 1.04566(16) 0.60192(18) 0.3979(5) 0.093(2) Uani 0.761(6) 1 d . . P E 1
H32W H 1.0433 0.5773 0.3889 0.112 Uiso 0.761(6) 1 d R U P E 1
H31W H 1.0368 0.6121 0.4557 0.112 Uiso 1 1 d R U . . .
O3V O 1.0238(5) 0.6468(6) 0.4379(15) 0.093(2) Uani 0.239(6) 1 d . . P E 2
H32V H 0.9988 0.6637 0.4411 0.112 Uiso 0.239(6) 1 d R U P E 2
O4W O 1.0824(2) 0.6690(3) 0.3871(5) 0.102(2) Uani 0.761(6) 1 d . U P E 1
H42W H 1.0839 0.6468 0.3583 0.123 Uiso 0.761(6) 1 d R U P E 1
H41W H 1.0555 0.6745 0.4149 0.123 Uiso 1 1 d R U . . .
O4V O 1.0784(7) 0.6934(8) 0.4071(18) 0.102(2) Uani 0.239(6) 1 d . U P E 2
H42V H 1.0830 0.7082 0.4546 0.123 Uiso 0.239(6) 1 d R U P E 2
C1X C 1.0497(5) 0.6536(5) 0.1739(12) 0.112(6) Uiso 0.5 1 d . . P . .
H11X H 1.0362 0.6322 0.1941 0.168 Uiso 0.5 1 d R U P . .
H12X H 1.0334 0.6692 0.1406 0.168 Uiso 0.5 1 d R U P . .
H13X H 1.0590 0.6675 0.2221 0.168 Uiso 0.5 1 d R U P . .
C2X C 1.0794(4) 0.6419(4) 0.1238(9) 0.075(4) Uiso 0.5 1 d . . P . .
O2X O 1.0863(3) 0.6122(3) 0.1131(6) 0.081(3) Uiso 0.5 1 d . . P . .
C3X C 1.0996(5) 0.6732(5) 0.0758(11) 0.106(5) Uiso 0.5 1 d . . P . .
H31X H 1.0878 0.6774 0.0213 0.159 Uiso 0.5 1 d R U P . .
H32X H 1.1253 0.6665 0.0668 0.159 Uiso 0.5 1 d R U P . .
H33X H 1.0984 0.6957 0.1094 0.159 Uiso 0.5 1 d R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N8 2.089(3) . ?
Cu1 O11 2.092(2) . ?
Cu1 N1 2.103(3) . ?
Cu1 N11 2.119(3) . ?
Cu1 N4 2.123(3) . ?
N1 C14 1.492(5) . ?
N1 C2 1.496(4) . ?
N1 C15 1.503(4) . ?
C2 C3 1.503(5) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.484(5) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C5 1.501(4) . ?
N4 C30 1.508(5) . ?
C5 C6 1.511(5) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 C7 1.512(5) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
C7 N8 1.497(4) . ?
C7 H71 0.9900 . ?
C7 H72 0.9900 . ?
N8 C18 1.491(5) . ?
N8 C9 1.497(4) . ?
C9 C10 1.495(5) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
C10 N11 1.485(5) . ?
C10 H101 0.9900 . ?
C10 H102 0.9900 . ?
N11 C12 1.494(5) . ?
N11 C40 1.513(4) . ?
C12 C13 1.515(5) . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C13 C14 1.517(5) . ?
C13 H131 0.9900 . ?
C13 H132 0.9900 . ?
C14 H141 0.9900 . ?
C14 H142 0.9900 . ?
C15 P1 1.835(4) . ?
C15 H151 0.9900 . ?
C15 H152 0.9900 . ?
P1 O12 1.485(3) . ?
P1 O11 1.512(3) . ?
P1 C16 1.826(4) . ?
C16 C17 1.479(5) . ?
C16 H161 0.9900 . ?
C16 H162 0.9900 . ?
C17 F2 1.337(5) . ?
C17 F1 1.339(5) . ?
C17 F3 1.349(5) . ?
C18 P2 1.834(3) . ?
C18 H181 0.9900 . ?
C18 H182 0.9900 . ?
P2 O22 1.495(3) . ?
P2 O21 1.499(3) . ?
P2 C19 1.841(4) . ?
O21 Cu2 2.116(3) . ?
C19 C20 1.478(6) . ?
C19 H191 0.9900 . ?
C19 H192 0.9900 . ?
C20 F4 1.325(6) . ?
C20 F5 1.345(6) . ?
C20 F6 1.349(5) . ?
C30 C31 1.514(5) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 C36 1.391(5) . ?
C31 C32 1.393(5) . ?
C32 C33 1.391(5) . ?
C32 H321 0.9500 . ?
C33 C34 1.380(6) . ?
C33 H331 0.9500 . ?
C34 C35 1.383(6) . ?
C34 H341 0.9500 . ?
C35 C36 1.385(5) . ?
C35 H351 0.9500 . ?
C36 H361 0.9500 . ?
C40 C41 1.513(5) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C41 C42 1.390(6) . ?
C41 C46 1.396(6) . ?
C42 C43 1.384(6) . ?
C42 H421 0.9500 . ?
C43 C44 1.384(7) . ?
C43 H431 0.9500 . ?
C44 C45 1.387(7) . ?
C44 H441 0.9500 . ?
C45 C46 1.384(6) . ?
C45 H451 0.9500 . ?
C46 H461 0.9500 . ?
Cu2 O11A 1.962(3) 9_765 ?
Cu2 O11B 1.976(3) . ?
Cu2 O12B 1.980(3) 9_765 ?
Cu2 O12A 1.981(3) . ?
Cu2 Cu2 2.6757(9) 9_765 ?
O11A C1A 1.255(5) . ?
O11A Cu2 1.962(3) 9_765 ?
O12A C1A 1.267(5) . ?
C1A C2A 1.505(6) . ?
C2A F22A 1.18(2) . ?
C2A F21A 1.19(3) . ?
C2A F23A 1.64(3) . ?
C2A H21A 0.9820 . ?
C2A H22A 0.9795 . ?
C2A H23A 0.9923 . ?
O11B C1B 1.246(5) . ?
O12B C1B 1.257(5) . ?
O12B Cu2 1.980(3) 9_765 ?
C1B C2B 1.516(6) . ?
C2B F21B 1.29(2) . ?
C2B F22B 1.299(19) . ?
C2B F23B 1.48(2) . ?
C2B H21B 1.0042 . ?
C2B H22B 0.9748 . ?
C2B H23B 0.9896 . ?
O1W H11W 0.8202 . ?
O1W H12W 0.8489 . ?
O2W H21W 0.8604 . ?
O2W H22W 0.8546 . ?
O3W H32W 0.9166 . ?
O3W H31W 1.0418 . ?
O3V H31W 1.3850 . ?
O3V H32V 1.1046 . ?
O4W H42W 0.9341 . ?
O4W H41W 1.0968 . ?
O4V H41W 1.0962 . ?
O4V H42V 0.9443 . ?
C1X C2X 1.41(2) . ?
C1X H11X 0.9800 . ?
C1X H12X 0.9800 . ?
C1X H13X 0.9800 . ?
C2X O2X 1.128(15) . ?
C2X C3X 1.56(2) . ?
C3X H31X 0.9800 . ?
C3X H32X 0.9801 . ?
C3X H33X 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
N8 Cu1 O11 93.12(10) . . ?
N8 Cu1 N1 179.54(12) . . ?
O11 Cu1 N1 87.33(10) . . ?
N8 Cu1 N11 86.19(11) . . ?
O11 Cu1 N11 99.78(11) . . ?
N1 Cu1 N11 93.64(11) . . ?
N8 Cu1 N4 94.71(11) . . ?
O11 Cu1 N4 110.77(11) . . ?
N1 Cu1 N4 85.22(11) . . ?
N11 Cu1 N4 149.32(11) . . ?
C14 N1 C2 106.5(3) . . ?
C14 N1 C15 110.4(3) . . ?
C2 N1 C15 108.7(3) . . ?
C14 N1 Cu1 114.8(2) . . ?
C2 N1 Cu1 105.5(2) . . ?
C15 N1 Cu1 110.5(2) . . ?
N1 C2 C3 108.5(3) . . ?
N1 C2 H21 110.0 . . ?
C3 C2 H21 110.0 . . ?
N1 C2 H22 110.0 . . ?
C3 C2 H22 110.0 . . ?
H21 C2 H22 108.4 . . ?
N4 C3 C2 109.0(3) . . ?
N4 C3 H31 109.9 . . ?
C2 C3 H31 109.9 . . ?
N4 C3 H32 109.9 . . ?
C2 C3 H32 109.9 . . ?
H31 C3 H32 108.3 . . ?
C3 N4 C5 108.3(3) . . ?
C3 N4 C30 110.4(3) . . ?
C5 N4 C30 109.7(3) . . ?
C3 N4 Cu1 101.3(2) . . ?
C5 N4 Cu1 112.3(2) . . ?
C30 N4 Cu1 114.3(2) . . ?
N4 C5 C6 114.1(3) . . ?
N4 C5 H51 108.7 . . ?
C6 C5 H51 108.7 . . ?
N4 C5 H52 108.7 . . ?
C6 C5 H52 108.7 . . ?
H51 C5 H52 107.6 . . ?
C5 C6 C7 113.6(3) . . ?
C5 C6 H61 108.8 . . ?
C7 C6 H61 108.8 . . ?
C5 C6 H62 108.8 . . ?
C7 C6 H62 108.8 . . ?
H61 C6 H62 107.7 . . ?
N8 C7 C6 115.7(3) . . ?
N8 C7 H71 108.4 . . ?
C6 C7 H71 108.4 . . ?
N8 C7 H72 108.4 . . ?
C6 C7 H72 108.4 . . ?
H71 C7 H72 107.4 . . ?
C18 N8 C7 111.8(3) . . ?
C18 N8 C9 109.8(3) . . ?
C7 N8 C9 107.6(3) . . ?
C18 N8 Cu1 107.9(2) . . ?
C7 N8 Cu1 114.1(2) . . ?
C9 N8 Cu1 105.5(2) . . ?
C10 C9 N8 109.7(3) . . ?
C10 C9 H91 109.7 . . ?
N8 C9 H91 109.7 . . ?
C10 C9 H92 109.7 . . ?
N8 C9 H92 109.7 . . ?
H91 C9 H92 108.2 . . ?
N11 C10 C9 110.7(3) . . ?
N11 C10 H101 109.5 . . ?
C9 C10 H101 109.5 . . ?
N11 C10 H102 109.5 . . ?
C9 C10 H102 109.5 . . ?
H101 C10 H102 108.1 . . ?
C10 N11 C12 108.7(3) . . ?
C10 N11 C40 111.1(3) . . ?
C12 N11 C40 110.6(3) . . ?
C10 N11 Cu1 101.5(2) . . ?
C12 N11 Cu1 112.3(2) . . ?
C40 N11 Cu1 112.3(2) . . ?
N11 C12 C13 114.0(3) . . ?
N11 C12 H121 108.8 . . ?
C13 C12 H121 108.8 . . ?
N11 C12 H122 108.8 . . ?
C13 C12 H122 108.8 . . ?
H121 C12 H122 107.6 . . ?
C12 C13 C14 113.5(3) . . ?
C12 C13 H131 108.9 . . ?
C14 C13 H131 108.9 . . ?
C12 C13 H132 108.9 . . ?
C14 C13 H132 108.9 . . ?
H131 C13 H132 107.7 . . ?
N1 C14 C13 115.9(3) . . ?
N1 C14 H141 108.3 . . ?
C13 C14 H141 108.3 . . ?
N1 C14 H142 108.3 . . ?
C13 C14 H142 108.3 . . ?
H141 C14 H142 107.4 . . ?
N1 C15 P1 111.0(2) . . ?
N1 C15 H151 109.4 . . ?
P1 C15 H151 109.4 . . ?
N1 C15 H152 109.4 . . ?
P1 C15 H152 109.4 . . ?
H151 C15 H152 108.0 . . ?
O12 P1 O11 118.36(15) . . ?
O12 P1 C16 110.98(16) . . ?
O11 P1 C16 104.83(15) . . ?
O12 P1 C15 112.16(16) . . ?
O11 P1 C15 104.31(15) . . ?
C16 P1 C15 105.11(17) . . ?
P1 O11 Cu1 115.33(14) . . ?
C17 C16 P1 116.4(3) . . ?
C17 C16 H161 108.2 . . ?
P1 C16 H161 108.2 . . ?
C17 C16 H162 108.2 . . ?
P1 C16 H162 108.2 . . ?
H161 C16 H162 107.3 . . ?
F2 C17 F1 106.4(3) . . ?
F2 C17 F3 104.6(3) . . ?
F1 C17 F3 106.5(4) . . ?
F2 C17 C16 113.7(4) . . ?
F1 C17 C16 112.1(3) . . ?
F3 C17 C16 112.9(3) . . ?
N8 C18 P2 120.2(2) . . ?
N8 C18 H181 107.3 . . ?
P2 C18 H181 107.3 . . ?
N8 C18 H182 107.3 . . ?
P2 C18 H182 107.3 . . ?
H181 C18 H182 106.9 . . ?
O22 P2 O21 117.89(15) . . ?
O22 P2 C18 109.91(15) . . ?
O21 P2 C18 110.65(15) . . ?
O22 P2 C19 108.93(17) . . ?
O21 P2 C19 109.51(17) . . ?
C18 P2 C19 98.12(17) . . ?
P2 O21 Cu2 137.43(17) . . ?
C20 C19 P2 116.4(3) . . ?
C20 C19 H191 108.2 . . ?
P2 C19 H191 108.2 . . ?
C20 C19 H192 108.2 . . ?
P2 C19 H192 108.2 . . ?
H191 C19 H192 107.3 . . ?
F4 C20 F5 106.6(4) . . ?
F4 C20 F6 105.4(4) . . ?
F5 C20 F6 106.3(4) . . ?
F4 C20 C19 113.9(4) . . ?
F5 C20 C19 112.6(4) . . ?
F6 C20 C19 111.5(4) . . ?
N4 C30 C31 115.7(3) . . ?
N4 C30 H301 108.3 . . ?
C31 C30 H301 108.3 . . ?
N4 C30 H302 108.3 . . ?
C31 C30 H302 108.3 . . ?
H301 C30 H302 107.4 . . ?
C36 C31 C32 118.4(3) . . ?
C36 C31 C30 120.3(3) . . ?
C32 C31 C30 121.2(3) . . ?
C33 C32 C31 120.7(4) . . ?
C33 C32 H321 119.7 . . ?
C31 C32 H321 119.7 . . ?
C34 C33 C32 120.0(4) . . ?
C34 C33 H331 120.0 . . ?
C32 C33 H331 120.0 . . ?
C33 C34 C35 119.9(4) . . ?
C33 C34 H341 120.1 . . ?
C35 C34 H341 120.1 . . ?
C34 C35 C36 120.1(4) . . ?
C34 C35 H351 120.0 . . ?
C36 C35 H351 120.0 . . ?
C35 C36 C31 120.9(4) . . ?
C35 C36 H361 119.6 . . ?
C31 C36 H361 119.6 . . ?
C41 C40 N11 115.2(3) . . ?
C41 C40 H401 108.5 . . ?
N11 C40 H401 108.5 . . ?
C41 C40 H402 108.5 . . ?
N11 C40 H402 108.5 . . ?
H401 C40 H402 107.5 . . ?
C42 C41 C46 118.2(4) . . ?
C42 C41 C40 120.6(4) . . ?
C46 C41 C40 121.1(4) . . ?
C43 C42 C41 120.5(4) . . ?
C43 C42 H421 119.7 . . ?
C41 C42 H421 119.7 . . ?
C44 C43 C42 120.7(5) . . ?
C44 C43 H431 119.6 . . ?
C42 C43 H431 119.6 . . ?
C43 C44 C45 119.5(4) . . ?
C43 C44 H441 120.2 . . ?
C45 C44 H441 120.2 . . ?
C46 C45 C44 119.7(5) . . ?
C46 C45 H451 120.2 . . ?
C44 C45 H451 120.2 . . ?
C45 C46 C41 121.4(4) . . ?
C45 C46 H461 119.3 . . ?
C41 C46 H461 119.3 . . ?
O11A Cu2 O11B 91.70(14) 9_765 . ?
O11A Cu2 O12B 87.36(13) 9_765 9_765 ?
O11B Cu2 O12B 167.16(12) . 9_765 ?
O11A Cu2 O12A 167.28(12) 9_765 . ?
O11B Cu2 O12A 86.58(13) . . ?
O12B Cu2 O12A 91.51(12) 9_765 . ?
O11A Cu2 O21 94.82(11) 9_765 . ?
O11B Cu2 O21 96.68(11) . . ?
O12B Cu2 O21 96.16(11) 9_765 . ?
O12A Cu2 O21 97.90(10) . . ?
O11A Cu2 Cu2 83.09(9) 9_765 9_765 ?
O11B Cu2 Cu2 84.06(9) . 9_765 ?
O12B Cu2 Cu2 83.11(8) 9_765 9_765 ?
O12A Cu2 Cu2 84.20(8) . 9_765 ?
O21 Cu2 Cu2 177.80(8) . 9_765 ?
C1A O11A Cu2 124.9(3) . 9_765 ?
C1A O12A Cu2 122.3(2) . . ?
O11A C1A O12A 125.2(4) . . ?
O11A C1A C2A 116.9(4) . . ?
O12A C1A C2A 117.9(4) . . ?
F22A C2A F21A 129.1(18) . . ?
F22A C2A C1A 113.9(12) . . ?
F21A C2A C1A 114.7(13) . . ?
F22A C2A F23A 95.8(15) . . ?
F21A C2A F23A 94.8(16) . . ?
C1A C2A F23A 94.6(10) . . ?
C1A C2A H21A 110.6 . . ?
C1A C2A H22A 110.3 . . ?
H21A C2A H22A 109.3 . . ?
C1A C2A H23A 109.7 . . ?
H21A C2A H23A 108.3 . . ?
H22A C2A H23A 108.5 . . ?
C1B O11B Cu2 122.7(3) . . ?
C1B O12B Cu2 123.3(3) . 9_765 ?
O11B C1B O12B 126.4(4) . . ?
O11B C1B C2B 116.3(4) . . ?
O12B C1B C2B 117.2(4) . . ?
F21B C2B F22B 111.0(12) . . ?
F21B C2B F23B 102.2(13) . . ?
F22B C2B F23B 102.1(13) . . ?
F21B C2B C1B 117.3(9) . . ?
F22B C2B C1B 117.2(9) . . ?
F23B C2B C1B 104.4(9) . . ?
C1B C2B H21B 110.2 . . ?
C1B C2B H22B 111.7 . . ?
H21B C2B H22B 107.9 . . ?
C1B C2B H23B 111.1 . . ?
H21B C2B H23B 106.7 . . ?
H22B C2B H23B 109.1 . . ?
H11W O1W H12W 109.5 . . ?
H21W O2W H22W 103.9 . . ?
H32W O3W H31W 117.3 . . ?
H31W O3V H32V 142.0 . . ?
H42W O4W H41W 114.2 . . ?
H41W O4V H42V 114.1 . . ?
C2X C1X H11X 109.3 . . ?
C2X C1X H12X 109.8 . . ?
H11X C1X H12X 109.5 . . ?
C2X C1X H13X 109.3 . . ?
H11X C1X H13X 109.5 . . ?
H12X C1X H13X 109.5 . . ?
O2X C2X C1X 123.2(15) . . ?
O2X C2X C3X 121.9(14) . . ?
C1X C2X C3X 114.6(14) . . ?
C2X C3X H31X 109.6 . . ?
C2X C3X H32X 109.8 . . ?
H31X C3X H32X 109.5 . . ?
C2X C3X H33X 109.1 . . ?
H31X C3X H33X 109.5 . . ?
H32X C3X H33X 109.5 . . ?

_refine_diff_density_max         0.971
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.093



####################################################################### 
# 
# 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_co2p6f
_database_code_depnum_ccdc_archive 'CCDC 2262044'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2023-05-10 deposited with the CCDC.	2023-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H30 Co F6 N4 O4 P2, Cl, 3(H2 O), Li'
_chemical_formula_sum            'C16 H36 Cl Co F6 Li N4 O7 P2'
_chemical_formula_weight         673.75

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

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

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

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

_cell_length_a                   21.9609(12)
_cell_length_b                   10.4910(5)
_cell_length_c                   25.9042(14)
_cell_angle_alpha                90
_cell_angle_beta                 111.540(2)
_cell_angle_gamma                90
_cell_volume                     5551.3(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9381
_cell_measurement_theta_min      2.5266
_cell_measurement_theta_max      27.5044

_exptl_crystal_description       prism
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_F_000             2776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.212
_exptl_absorpt_coefficient_mu    0.912
_shelx_estimated_absorpt_T_min   0.783
_shelx_estimated_absorpt_T_max   0.830
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            123017
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.994
_diffrn_reflns_theta_max         27.522
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12767
_reflns_number_gt                12162
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker Instrument Service vV6.2.15'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1242)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0484P)²+4.9515P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12767
_refine_ls_number_parameters     741
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0902
_refine_ls_wR_factor_gt          0.0891
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1A Co 0.20132(2) 0.26703(2) 0.56065(2) 0.01847(6) Uani 1 1 d . . . . .
N1A N 0.19136(7) 0.45586(14) 0.59197(6) 0.0236(3) Uani 1 1 d . . . . .
C2A C 0.11990(9) 0.47107(19) 0.57970(8) 0.0301(4) Uani 1 1 d . . . . .
H2A H 0.1091 0.5630 0.5771 0.036 Uiso 1 1 calc R U . . .
H2B H 0.1095 0.4352 0.6108 0.036 Uiso 1 1 calc R U . . .
C3A C 0.07774(9) 0.40590(18) 0.52624(8) 0.0294(4) Uani 1 1 d . . . . .
H3A H 0.0312 0.4101 0.5222 0.035 Uiso 1 1 calc R U . . .
H3B H 0.0824 0.4503 0.4942 0.035 Uiso 1 1 calc R U . . .
N4A N 0.09785(7) 0.27114(15) 0.52686(6) 0.0244(3) Uani 1 1 d . . . . .
H4A H 0.0828(11) 0.231(2) 0.5459(9) 0.021(5) Uiso 1 1 d . . . . .
C5A C 0.06776(9) 0.2128(2) 0.47110(8) 0.0307(4) Uani 1 1 d . . . . .
H5A H 0.0829 0.2590 0.4447 0.037 Uiso 1 1 calc R U . . .
H5B H 0.0196 0.2220 0.4582 0.037 Uiso 1 1 calc R U . . .
C6A C 0.08485(9) 0.0723(2) 0.47105(8) 0.0331(4) Uani 1 1 d . . . . .
H6A H 0.0555 0.0345 0.4356 0.040 Uiso 1 1 calc R U . . .
H6B H 0.0753 0.0297 0.5013 0.040 Uiso 1 1 calc R U . . .
C7A C 0.15551(9) 0.04184(19) 0.47806(8) 0.0309(4) Uani 1 1 d . . . . .
H7A H 0.1584 -0.0501 0.4706 0.037 Uiso 1 1 calc R U . . .
H7B H 0.1663 0.0897 0.4496 0.037 Uiso 1 1 calc R U . . .
N8A N 0.20625(7) 0.07208(14) 0.53396(6) 0.0233(3) Uani 1 1 d . . . . .
C9A C 0.19645(9) -0.00982(17) 0.57715(8) 0.0289(4) Uani 1 1 d . . . . .
H9A H 0.2141 -0.0960 0.5757 0.035 Uiso 1 1 calc R U . . .
H9B H 0.1490 -0.0183 0.5694 0.035 Uiso 1 1 calc R U . . .
C10A C 0.23001(9) 0.04535(17) 0.63469(8) 0.0273(4) Uani 1 1 d . . . . .
H10A H 0.2201 -0.0077 0.6623 0.033 Uiso 1 1 calc R U . . .
H10B H 0.2780 0.0456 0.6444 0.033 Uiso 1 1 calc R U . . .
N11A N 0.20671(7) 0.17636(15) 0.63596(6) 0.0240(3) Uani 1 1 d . . . . .
H11A H 0.1696(12) 0.173(2) 0.6370(9) 0.024(5) Uiso 1 1 d . . . . .
C12A C 0.24722(10) 0.2436(2) 0.68700(8) 0.0310(4) Uani 1 1 d . . . . .
H12A H 0.2922 0.2532 0.6874 0.037 Uiso 1 1 calc R U . . .
H12B H 0.2496 0.1919 0.7197 0.037 Uiso 1 1 calc R U . . .
C13A C 0.21981(11) 0.3745(2) 0.69139(8) 0.0333(4) Uani 1 1 d . . . . .
H13A H 0.2411 0.4050 0.7301 0.040 Uiso 1 1 calc R U . . .
H13B H 0.1725 0.3654 0.6840 0.040 Uiso 1 1 calc R U . . .
C14A C 0.22826(10) 0.47612(19) 0.65263(7) 0.0304(4) Uani 1 1 d . . . . .
H14A H 0.2147 0.5591 0.6631 0.036 Uiso 1 1 calc R U . . .
H14B H 0.2754 0.4824 0.6589 0.036 Uiso 1 1 calc R U . . .
C20A C 0.21576(9) 0.55166(16) 0.56179(7) 0.0250(3) Uani 1 1 d . . . . .
H20A H 0.2632 0.5650 0.5823 0.030 Uiso 1 1 calc R U . . .
H20B H 0.1933 0.6338 0.5612 0.030 Uiso 1 1 calc R U . . .
P1A P 0.20272(2) 0.50508(4) 0.49033(2) 0.02349(9) Uani 1 1 d . . . . .
O11A O 0.20025(6) 0.36050(12) 0.48890(5) 0.0254(3) Uani 1 1 d . . . . .
O12A O 0.14644(7) 0.57695(14) 0.45051(6) 0.0357(3) Uani 1 1 d . . . . .
C21A C 0.27802(10) 0.54648(17) 0.47944(8) 0.0285(4) Uani 1 1 d . . . . .
H21A H 0.3147 0.5005 0.5075 0.034 Uiso 1 1 calc R U . . .
H21B H 0.2743 0.5137 0.4426 0.034 Uiso 1 1 calc R U . . .
C22A C 0.29595(12) 0.6844(2) 0.48215(9) 0.0362(4) Uani 1 1 d . . . . .
F1A F 0.30197(9) 0.73697(13) 0.53100(6) 0.0553(4) Uani 1 1 d . . . . .
F2A F 0.25281(9) 0.75478(14) 0.44311(7) 0.0621(4) Uani 1 1 d . . . . .
F3A F 0.35371(9) 0.70225(15) 0.47717(8) 0.0606(4) Uani 1 1 d . . . . .
C30A C 0.27218(9) 0.05054(17) 0.53141(8) 0.0259(3) Uani 1 1 d . . . . .
H30A H 0.2697 0.0677 0.4931 0.031 Uiso 1 1 calc R U . . .
H30B H 0.2840 -0.0403 0.5395 0.031 Uiso 1 1 calc R U . . .
P2A P 0.33746(2) 0.14884(4) 0.57936(2) 0.02215(9) Uani 1 1 d . . . . .
O21A O 0.30327(6) 0.26807(12) 0.58854(5) 0.0244(2) Uani 1 1 d . . . . .
O22A O 0.38006(6) 0.07836(14) 0.62946(6) 0.0312(3) Uani 1 1 d . . . . .
C31A C 0.38735(9) 0.19998(18) 0.54001(8) 0.0286(4) Uani 1 1 d . . . . .
H31A H 0.3577 0.2252 0.5023 0.034 Uiso 1 1 calc R U . . .
H31B H 0.4123 0.2768 0.5581 0.034 Uiso 1 1 calc R U . . .
C32A C 0.43460(11) 0.1034(2) 0.53441(10) 0.0401(5) Uani 1 1 d . . . . .
F4A F 0.40581(8) -0.00804(15) 0.51486(8) 0.0617(4) Uani 1 1 d . . . . .
F5A F 0.48319(7) 0.07656(16) 0.58243(7) 0.0550(4) Uani 1 1 d . . . . .
F6A F 0.46360(8) 0.14329(17) 0.49981(7) 0.0601(4) Uani 1 1 d . . . . .
Co1X Co 0.57934(2) 0.54997(2) 0.71227(2) 0.01785(6) Uani 1 1 d . . . . .
N1X N 0.53406(7) 0.66745(15) 0.63694(6) 0.0238(3) Uani 1 1 d . . . . .
C2X C 0.58601(9) 0.7607(2) 0.63763(8) 0.0306(4) Uani 1 1 d . . . . .
H2X H 0.5649 0.8382 0.6169 0.037 Uiso 1 1 calc R U . . .
H2Y H 0.6131 0.7227 0.6184 0.037 Uiso 1 1 calc R U . . .
C3X C 0.62994(9) 0.79817(18) 0.69608(8) 0.0272(4) Uani 1 1 d . . . . .
H3X H 0.6657 0.8540 0.6948 0.033 Uiso 1 1 calc R U . . .
H3Y H 0.6044 0.8456 0.7143 0.033 Uiso 1 1 calc R U . . .
N4X N 0.65755(7) 0.68162(14) 0.72783(6) 0.0222(3) Uani 1 1 d . . . . .
H4X H 0.6864(12) 0.650(2) 0.7151(10) 0.030(6) Uiso 1 1 d . . . . .
C5X C 0.69479(8) 0.70958(17) 0.78722(7) 0.0246(3) Uani 1 1 d . . . . .
H5X H 0.6649 0.7470 0.8039 0.029 Uiso 1 1 calc R U . . .
H5YB H 0.7293 0.7731 0.7903 0.029 Uiso 1 1 calc R U . . .
C6X C 0.72618(8) 0.58969(18) 0.81904(8) 0.0274(4) Uani 1 1 d . . . . .
H6X H 0.7618 0.6156 0.8538 0.033 Uiso 1 1 calc R U . . .
H6Y H 0.7464 0.5415 0.7966 0.033 Uiso 1 1 calc R U . . .
C7X C 0.68004(9) 0.50057(18) 0.83371(7) 0.0267(4) Uani 1 1 d . . . . .
H7X H 0.7066 0.4357 0.8602 0.032 Uiso 1 1 calc R U . . .
H7Y H 0.6565 0.5507 0.8530 0.032 Uiso 1 1 calc R U . . .
N8X N 0.63037(7) 0.43305(14) 0.78544(6) 0.0228(3) Uani 1 1 d . . . . .
C9X C 0.66514(9) 0.33193(18) 0.76603(8) 0.0306(4) Uani 1 1 d . . . . .
H9X H 0.6706 0.2555 0.7897 0.037 Uiso 1 1 calc R U . . .
H9Y H 0.7094 0.3631 0.7705 0.037 Uiso 1 1 calc R U . . .
C10X C 0.62935(9) 0.29448(17) 0.70615(8) 0.0287(4) Uani 1 1 d . . . . .
H10X H 0.6567 0.2355 0.6941 0.034 Uiso 1 1 calc R U . . .
H10Y H 0.5880 0.2503 0.7022 0.034 Uiso 1 1 calc R U . . .
N11X N 0.61503(7) 0.40996(15) 0.67143(6) 0.0253(3) Uani 1 1 d . . . . .
H11X H 0.6536(12) 0.439(2) 0.6710(9) 0.027(5) Uiso 1 1 d . . . . .
C12X C 0.57192(10) 0.3824(2) 0.61342(8) 0.0347(4) Uani 1 1 d . . . . .
H12X H 0.5292 0.3507 0.6128 0.042 Uiso 1 1 calc R U . . .
H12Y H 0.5919 0.3146 0.5983 0.042 Uiso 1 1 calc R U . . .
C13X C 0.56094(11) 0.5000(2) 0.57694(8) 0.0376(5) Uani 1 1 d . . . . .
H13X H 0.5457 0.4723 0.5377 0.045 Uiso 1 1 calc R U . . .
H13Y H 0.6035 0.5437 0.5855 0.045 Uiso 1 1 calc R U . . .
C14X C 0.51168(10) 0.5962(2) 0.58316(7) 0.0322(4) Uani 1 1 d . . . . .
H14X H 0.5012 0.6587 0.5525 0.039 Uiso 1 1 calc R U . . .
H14Y H 0.4708 0.5504 0.5791 0.039 Uiso 1 1 calc R U . . .
C20X C 0.47629(8) 0.73425(17) 0.64144(7) 0.0232(3) Uani 1 1 d . . . . .
H20X H 0.4369 0.6810 0.6237 0.028 Uiso 1 1 calc R U . . .
H20Y H 0.4696 0.8156 0.6207 0.028 Uiso 1 1 calc R U . . .
P1X P 0.48467(2) 0.76804(4) 0.71324(2) 0.01916(9) Uani 1 1 d . . . . .
O11X O 0.53806(6) 0.68108(11) 0.75018(5) 0.0212(2) Uani 1 1 d . . . . .
O12X O 0.49230(6) 0.90806(11) 0.72522(5) 0.0268(3) Uani 1 1 d . . . . .
C21X C 0.41007(8) 0.71086(16) 0.72083(7) 0.0227(3) Uani 1 1 d . . . . .
H21X H 0.3997 0.6257 0.7033 0.027 Uiso 1 1 calc R U . . .
H21Y H 0.4190 0.6998 0.7609 0.027 Uiso 1 1 calc R U . . .
C22X C 0.35125(9) 0.79315(18) 0.69683(7) 0.0259(3) Uani 1 1 d . . . . .
F1X F 0.33533(6) 0.81344(12) 0.64227(4) 0.0344(3) Uani 1 1 d . . . . .
F2X F 0.35871(6) 0.90835(10) 0.72135(5) 0.0304(2) Uani 1 1 d . . . . .
F3X F 0.29804(6) 0.74137(12) 0.70259(6) 0.0397(3) Uani 1 1 d . . . . .
C30X C 0.58002(9) 0.37626(17) 0.80453(7) 0.0268(3) Uani 1 1 d . . . . .
H30X H 0.5700 0.4376 0.8294 0.032 Uiso 1 1 calc R U . . .
H30Y H 0.5982 0.2984 0.8263 0.032 Uiso 1 1 calc R U . . .
P2X P 0.50408(2) 0.33519(4) 0.74725(2) 0.02316(9) Uani 1 1 d . . . . .
O21X O 0.49828(6) 0.43099(12) 0.70192(5) 0.0249(2) Uani 1 1 d . . . . .
O22X O 0.50139(7) 0.19706(13) 0.73308(7) 0.0354(3) Uani 1 1 d . . . . .
C31X C 0.43677(9) 0.37123(18) 0.77055(8) 0.0282(4) Uani 1 1 d . . . . .
H31X H 0.4470 0.4520 0.7918 0.034 Uiso 1 1 calc R U . . .
H31Y H 0.3967 0.3856 0.7374 0.034 Uiso 1 1 calc R U . . .
C32X C 0.42233(10) 0.2716(2) 0.80574(9) 0.0344(4) Uani 1 1 d . . . . .
F4X F 0.47524(7) 0.24167(15) 0.85013(6) 0.0519(4) Uani 1 1 d . . . . .
F5X F 0.40030(7) 0.16194(12) 0.77869(6) 0.0436(3) Uani 1 1 d . . . . .
F6X F 0.37553(8) 0.30983(16) 0.82426(7) 0.0560(4) Uani 1 1 d . . . . .
Li1 Li 0.09018(17) 0.6007(4) 0.37784(15) 0.0359(7) Uani 1 1 d . . . . .
Li2 Li 0.45220(15) 0.0622(3) 0.69376(13) 0.0279(6) Uani 1 1 d . . . . .
Cl1 Cl -0.05357(2) 0.84970(5) 0.37147(2) 0.03125(10) Uani 1 1 d . . . . .
Cl2 Cl 0.25061(2) 0.45947(4) 0.33058(2) 0.02927(10) Uani 1 1 d . . . . .
O1W O 0.08177(7) 0.78748(15) 0.36274(6) 0.0334(3) Uani 1 1 d . . . . .
H11W H 0.0676(15) 0.791(3) 0.3228(14) 0.061(9) Uiso 1 1 d . . . . .
H12W H 0.0421(16) 0.807(3) 0.3709(13) 0.060(9) Uiso 1 1 d . . . . .
O2W O 0.10604(9) 0.5012(2) 0.32239(7) 0.0465(4) Uani 1 1 d . . . . .
H21W H 0.1418(16) 0.481(3) 0.3220(12) 0.051(8) Uiso 1 1 d . . . . .
H22W H 0.075(2) 0.486(4) 0.2915(19) 0.105(15) Uiso 1 1 d . . . . .
O3W O -0.00504(9) 0.5666(2) 0.35857(11) 0.0566(5) Uani 1 1 d . . . . .
H31W H -0.019(2) 0.652(5) 0.3587(18) 0.109(15) Uiso 1 1 d . . . . .
H32W H -0.020(2) 0.511(5) 0.3374(19) 0.108(17) Uiso 1 1 d . . . . .
O4W O 0.37922(7) 0.48140(14) 0.61962(7) 0.0392(4) Uani 1 1 d . . . . .
H41W H 0.3558(15) 0.410(3) 0.6137(12) 0.055(8) Uiso 1 1 d . . . . .
H42W H 0.4194(15) 0.457(3) 0.6451(12) 0.047(7) Uiso 1 1 d . . . . .
O5W O 0.26186(9) 0.24544(15) 0.42227(7) 0.0421(4) Uani 1 1 d . . . . .
H51W H 0.2623(18) 0.298(4) 0.3967(16) 0.079(11) Uiso 1 1 d . . . . .
H52W H 0.2330(17) 0.283(3) 0.4405(15) 0.072(10) Uiso 1 1 d . . . . .
O6W O 0.07239(11) 0.7507(2) 0.49042(9) 0.0627(5) Uani 1 1 d . . . . .
H61W H 0.0969 0.7093 0.4712 0.094 Uiso 1 1 d R U . . .
H62W H 0.0358 0.7818 0.4654 0.094 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1A O21A 2.0850(12) . ?
Co1A O11A 2.0940(12) . ?
Co1A N4A 2.1145(15) . ?
Co1A N11A 2.1343(15) . ?
Co1A N8A 2.1743(15) . ?
Co1A N1A 2.1820(15) . ?
N1A C20A 1.489(2) . ?
N1A C2A 1.491(2) . ?
N1A C14A 1.495(2) . ?
C2A C3A 1.517(3) . ?
C2A H2A 0.9900 . ?
C2A H2B 0.9900 . ?
C3A N4A 1.479(2) . ?
C3A H3A 0.9900 . ?
C3A H3B 0.9900 . ?
N4A C5A 1.482(2) . ?
N4A H4A 0.81(2) . ?
C5A C6A 1.521(3) . ?
C5A H5A 0.9900 . ?
C5A H5B 0.9900 . ?
C6A C7A 1.528(3) . ?
C6A H6A 0.9900 . ?
C6A H6B 0.9900 . ?
C7A N8A 1.501(2) . ?
C7A H7A 0.9900 . ?
C7A H7B 0.9900 . ?
N8A C9A 1.488(2) . ?
N8A C30A 1.491(2) . ?
C9A C10A 1.514(3) . ?
C9A H9A 0.9900 . ?
C9A H9B 0.9900 . ?
C10A N11A 1.471(2) . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
N11A C12A 1.474(2) . ?
N11A H11A 0.83(2) . ?
C12A C13A 1.520(3) . ?
C12A H12A 0.9900 . ?
C12A H12B 0.9900 . ?
C13A C14A 1.522(3) . ?
C13A H13A 0.9900 . ?
C13A H13B 0.9900 . ?
C14A H14A 0.9900 . ?
C14A H14B 0.9900 . ?
C20A P1A 1.8326(18) . ?
C20A H20A 0.9900 . ?
C20A H20B 0.9900 . ?
P1A O12A 1.4913(14) . ?
P1A O11A 1.5178(13) . ?
P1A C21A 1.829(2) . ?
O12A Li1 1.851(4) . ?
C21A C22A 1.494(3) . ?
C21A H21A 0.9900 . ?
C21A H21B 0.9900 . ?
C22A F2A 1.327(3) . ?
C22A F3A 1.335(3) . ?
C22A F1A 1.342(2) . ?
C30A P2A 1.8314(18) . ?
C30A H30A 0.9900 . ?
C30A H30B 0.9900 . ?
P2A O22A 1.4882(13) . ?
P2A O21A 1.5218(13) . ?
P2A C31A 1.8298(19) . ?
O22A Li2 1.837(3) . ?
C31A C32A 1.495(3) . ?
C31A H31A 0.9900 . ?
C31A H31B 0.9900 . ?
C32A F4A 1.337(3) . ?
C32A F5A 1.338(3) . ?
C32A F6A 1.343(3) . ?
Co1X O11X 2.0814(12) . ?
Co1X O21X 2.1093(13) . ?
Co1X N11X 2.1213(15) . ?
Co1X N4X 2.1240(15) . ?
Co1X N8X 2.1894(14) . ?
Co1X N1X 2.2115(15) . ?
N1X C20X 1.491(2) . ?
N1X C14X 1.496(2) . ?
N1X C2X 1.498(2) . ?
C2X C3X 1.518(3) . ?
C2X H2X 0.9900 . ?
C2X H2Y 0.9900 . ?
C3X N4X 1.474(2) . ?
C3X H3X 0.9900 . ?
C3X H3Y 0.9900 . ?
N4X C5X 1.482(2) . ?
N4X H4X 0.88(2) . ?
C5X C6X 1.523(3) . ?
C5X H5X 0.9900 . ?
C5X H5YB 0.9900 . ?
C6X C7X 1.526(3) . ?
C6X H6X 0.9900 . ?
C6X H6Y 0.9900 . ?
C7X N8X 1.501(2) . ?
C7X H7X 0.9900 . ?
C7X H7Y 0.9900 . ?
N8X C30X 1.491(2) . ?
N8X C9X 1.498(2) . ?
C9X C10X 1.511(3) . ?
C9X H9X 0.9900 . ?
C9X H9Y 0.9900 . ?
C10X N11X 1.472(2) . ?
C10X H10X 0.9900 . ?
C10X H10Y 0.9900 . ?
N11X C12X 1.481(2) . ?
N11X H11X 0.90(2) . ?
C12X C13X 1.518(3) . ?
C12X H12X 0.9900 . ?
C12X H12Y 0.9900 . ?
C13X C14X 1.530(3) . ?
C13X H13X 0.9900 . ?
C13X H13Y 0.9900 . ?
C14X H14X 0.9900 . ?
C14X H14Y 0.9900 . ?
C20X P1X 1.8351(18) . ?
C20X H20X 0.9900 . ?
C20X H20Y 0.9900 . ?
P1X O12X 1.4980(12) . ?
P1X O11X 1.5162(12) . ?
P1X C21X 1.8218(18) . ?
O12X Li2 1.878(3) 1_565 ?
C21X C22X 1.487(2) . ?
C21X H21X 0.9900 . ?
C21X H21Y 0.9900 . ?
C22X F1X 1.343(2) . ?
C22X F3X 1.346(2) . ?
C22X F2X 1.347(2) . ?
C30X P2X 1.8308(18) . ?
C30X H30X 0.9900 . ?
C30X H30Y 0.9900 . ?
P2X O22X 1.4909(14) . ?
P2X O21X 1.5150(14) . ?
P2X C31X 1.8294(19) . ?
O22X Li2 1.844(3) . ?
C31X C32X 1.496(3) . ?
C31X H31X 0.9900 . ?
C31X H31Y 0.9900 . ?
C32X F4X 1.338(2) . ?
C32X F5X 1.341(2) . ?
C32X F6X 1.345(3) . ?
Li1 O2W 1.908(4) . ?
Li1 O1W 1.994(4) . ?
Li1 O3W 1.996(4) . ?
Li1 H31W 2.33(5) . ?
Li2 O12X 1.878(3) 1_545 ?
O1W H11W 0.96(3) . ?
O1W H12W 0.99(3) . ?
O2W H21W 0.82(3) . ?
O2W H22W 0.85(5) . ?
O3W H31W 0.95(5) . ?
O3W H32W 0.78(5) . ?
O4W H41W 0.89(3) . ?
O4W H42W 0.92(3) . ?
O5W H51W 0.87(4) . ?
O5W H52W 1.00(4) . ?
O6W H61W 0.9604 . ?
O6W H62W 0.8895 . ?

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
O21A Co1A O11A 88.04(5) . . ?
O21A Co1A N4A 175.88(6) . . ?
O11A Co1A N4A 87.87(6) . . ?
O21A Co1A N11A 89.62(5) . . ?
O11A Co1A N11A 177.25(6) . . ?
N4A Co1A N11A 94.47(6) . . ?
O21A Co1A N8A 86.71(5) . . ?
O11A Co1A N8A 98.27(5) . . ?
N4A Co1A N8A 93.38(6) . . ?
N11A Co1A N8A 83.05(6) . . ?
O21A Co1A N1A 96.19(5) . . ?
O11A Co1A N1A 86.27(5) . . ?
N4A Co1A N1A 84.04(6) . . ?
N11A Co1A N1A 92.53(6) . . ?
N8A Co1A N1A 174.71(6) . . ?
C20A N1A C2A 111.68(14) . . ?
C20A N1A C14A 107.17(14) . . ?
C2A N1A C14A 109.32(14) . . ?
C20A N1A Co1A 108.24(10) . . ?
C2A N1A Co1A 105.03(11) . . ?
C14A N1A Co1A 115.48(11) . . ?
N1A C2A C3A 112.85(15) . . ?
N1A C2A H2A 109.0 . . ?
C3A C2A H2A 109.0 . . ?
N1A C2A H2B 109.0 . . ?
C3A C2A H2B 109.0 . . ?
H2A C2A H2B 107.8 . . ?
N4A C3A C2A 109.95(15) . . ?
N4A C3A H3A 109.7 . . ?
C2A C3A H3A 109.7 . . ?
N4A C3A H3B 109.7 . . ?
C2A C3A H3B 109.7 . . ?
H3A C3A H3B 108.2 . . ?
C3A N4A C5A 111.08(14) . . ?
C3A N4A Co1A 107.16(11) . . ?
C5A N4A Co1A 114.94(12) . . ?
C3A N4A H4A 108.3(15) . . ?
C5A N4A H4A 104.3(16) . . ?
Co1A N4A H4A 110.9(16) . . ?
N4A C5A C6A 112.29(15) . . ?
N4A C5A H5A 109.1 . . ?
C6A C5A H5A 109.1 . . ?
N4A C5A H5B 109.1 . . ?
C6A C5A H5B 109.1 . . ?
H5A C5A H5B 107.9 . . ?
C5A C6A C7A 116.28(17) . . ?
C5A C6A H6A 108.2 . . ?
C7A C6A H6A 108.2 . . ?
C5A C6A H6B 108.2 . . ?
C7A C6A H6B 108.2 . . ?
H6A C6A H6B 107.4 . . ?
N8A C7A C6A 115.61(16) . . ?
N8A C7A H7A 108.4 . . ?
C6A C7A H7A 108.4 . . ?
N8A C7A H7B 108.4 . . ?
C6A C7A H7B 108.4 . . ?
H7A C7A H7B 107.4 . . ?
C9A N8A C30A 110.91(14) . . ?
C9A N8A C7A 110.01(14) . . ?
C30A N8A C7A 108.32(14) . . ?
C9A N8A Co1A 105.44(11) . . ?
C30A N8A Co1A 108.62(10) . . ?
C7A N8A Co1A 113.54(11) . . ?
N8A C9A C10A 111.52(14) . . ?
N8A C9A H9A 109.3 . . ?
C10A C9A H9A 109.3 . . ?
N8A C9A H9B 109.3 . . ?
C10A C9A H9B 109.3 . . ?
H9A C9A H9B 108.0 . . ?
N11A C10A C9A 109.36(14) . . ?
N11A C10A H10A 109.8 . . ?
C9A C10A H10A 109.8 . . ?
N11A C10A H10B 109.8 . . ?
C9A C10A H10B 109.8 . . ?
H10A C10A H10B 108.2 . . ?
C10A N11A C12A 111.53(14) . . ?
C10A N11A Co1A 107.39(11) . . ?
C12A N11A Co1A 114.77(12) . . ?
C10A N11A H11A 108.3(16) . . ?
C12A N11A H11A 105.7(16) . . ?
Co1A N11A H11A 109.0(15) . . ?
N11A C12A C13A 111.99(15) . . ?
N11A C12A H12A 109.2 . . ?
C13A C12A H12A 109.2 . . ?
N11A C12A H12B 109.2 . . ?
C13A C12A H12B 109.2 . . ?
H12A C12A H12B 107.9 . . ?
C12A C13A C14A 115.83(16) . . ?
C12A C13A H13A 108.3 . . ?
C14A C13A H13A 108.3 . . ?
C12A C13A H13B 108.3 . . ?
C14A C13A H13B 108.3 . . ?
H13A C13A H13B 107.4 . . ?
N1A C14A C13A 116.32(16) . . ?
N1A C14A H14A 108.2 . . ?
C13A C14A H14A 108.2 . . ?
N1A C14A H14B 108.2 . . ?
C13A C14A H14B 108.2 . . ?
H14A C14A H14B 107.4 . . ?
N1A C20A P1A 113.43(12) . . ?
N1A C20A H20A 108.9 . . ?
P1A C20A H20A 108.9 . . ?
N1A C20A H20B 108.9 . . ?
P1A C20A H20B 108.9 . . ?
H20A C20A H20B 107.7 . . ?
O12A P1A O11A 118.38(8) . . ?
O12A P1A C21A 109.88(9) . . ?
O11A P1A C21A 105.06(8) . . ?
O12A P1A C20A 110.25(9) . . ?
O11A P1A C20A 106.38(7) . . ?
C21A P1A C20A 106.12(9) . . ?
P1A O11A Co1A 117.24(7) . . ?
P1A O12A Li1 147.76(15) . . ?
C22A C21A P1A 117.40(14) . . ?
C22A C21A H21A 108.0 . . ?
P1A C21A H21A 108.0 . . ?
C22A C21A H21B 108.0 . . ?
P1A C21A H21B 108.0 . . ?
H21A C21A H21B 107.2 . . ?
F2A C22A F3A 106.62(18) . . ?
F2A C22A F1A 106.58(19) . . ?
F3A C22A F1A 105.39(19) . . ?
F2A C22A C21A 113.63(19) . . ?
F3A C22A C21A 112.02(18) . . ?
F1A C22A C21A 112.06(16) . . ?
N8A C30A P2A 114.56(12) . . ?
N8A C30A H30A 108.6 . . ?
P2A C30A H30A 108.6 . . ?
N8A C30A H30B 108.6 . . ?
P2A C30A H30B 108.6 . . ?
H30A C30A H30B 107.6 . . ?
O22A P2A O21A 117.41(8) . . ?
O22A P2A C31A 108.56(8) . . ?
O21A P2A C31A 106.06(8) . . ?
O22A P2A C30A 113.37(9) . . ?
O21A P2A C30A 105.11(8) . . ?
C31A P2A C30A 105.48(9) . . ?
P2A O21A Co1A 118.04(7) . . ?
P2A O22A Li2 153.29(14) . . ?
C32A C31A P2A 115.73(14) . . ?
C32A C31A H31A 108.3 . . ?
P2A C31A H31A 108.3 . . ?
C32A C31A H31B 108.3 . . ?
P2A C31A H31B 108.3 . . ?
H31A C31A H31B 107.4 . . ?
F4A C32A F5A 105.9(2) . . ?
F4A C32A F6A 107.1(2) . . ?
F5A C32A F6A 105.92(18) . . ?
F4A C32A C31A 112.39(18) . . ?
F5A C32A C31A 113.41(19) . . ?
F6A C32A C31A 111.68(19) . . ?
O11X Co1X O21X 87.56(5) . . ?
O11X Co1X N11X 176.04(5) . . ?
O21X Co1X N11X 88.62(6) . . ?
O11X Co1X N4X 86.71(5) . . ?
O21X Co1X N4X 174.20(5) . . ?
N11X Co1X N4X 97.11(6) . . ?
O11X Co1X N8X 97.75(5) . . ?
O21X Co1X N8X 85.31(5) . . ?
N11X Co1X N8X 83.02(6) . . ?
N4X Co1X N8X 94.52(6) . . ?
O11X Co1X N1X 85.15(5) . . ?
O21X Co1X N1X 97.62(5) . . ?
N11X Co1X N1X 94.28(6) . . ?
N4X Co1X N1X 82.84(6) . . ?
N8X Co1X N1X 175.99(6) . . ?
C20X N1X C14X 108.04(13) . . ?
C20X N1X C2X 110.99(15) . . ?
C14X N1X C2X 109.01(15) . . ?
C20X N1X Co1X 108.23(10) . . ?
C14X N1X Co1X 115.52(12) . . ?
C2X N1X Co1X 105.05(10) . . ?
N1X C2X C3X 112.54(15) . . ?
N1X C2X H2X 109.1 . . ?
C3X C2X H2X 109.1 . . ?
N1X C2X H2Y 109.1 . . ?
C3X C2X H2Y 109.1 . . ?
H2X C2X H2Y 107.8 . . ?
N4X C3X C2X 108.81(15) . . ?
N4X C3X H3X 109.9 . . ?
C2X C3X H3X 109.9 . . ?
N4X C3X H3Y 109.9 . . ?
C2X C3X H3Y 109.9 . . ?
H3X C3X H3Y 108.3 . . ?
C3X N4X C5X 111.85(14) . . ?
C3X N4X Co1X 107.17(10) . . ?
C5X N4X Co1X 115.16(11) . . ?
C3X N4X H4X 107.9(16) . . ?
C5X N4X H4X 105.3(15) . . ?
Co1X N4X H4X 109.2(16) . . ?
N4X C5X C6X 111.46(14) . . ?
N4X C5X H5X 109.3 . . ?
C6X C5X H5X 109.3 . . ?
N4X C5X H5YB 109.3 . . ?
C6X C5X H5YB 109.3 . . ?
H5X C5X H5YB 108.0 . . ?
C5X C6X C7X 115.53(15) . . ?
C5X C6X H6X 108.4 . . ?
C7X C6X H6X 108.4 . . ?
C5X C6X H6Y 108.4 . . ?
C7X C6X H6Y 108.4 . . ?
H6X C6X H6Y 107.5 . . ?
N8X C7X C6X 115.31(15) . . ?
N8X C7X H7X 108.4 . . ?
C6X C7X H7X 108.4 . . ?
N8X C7X H7Y 108.4 . . ?
C6X C7X H7Y 108.4 . . ?
H7X C7X H7Y 107.5 . . ?
C30X N8X C9X 111.09(14) . . ?
C30X N8X C7X 108.22(14) . . ?
C9X N8X C7X 108.04(14) . . ?
C30X N8X Co1X 107.75(10) . . ?
C9X N8X Co1X 105.56(11) . . ?
C7X N8X Co1X 116.18(11) . . ?
N8X C9X C10X 113.05(14) . . ?
N8X C9X H9X 109.0 . . ?
C10X C9X H9X 109.0 . . ?
N8X C9X H9Y 109.0 . . ?
C10X C9X H9Y 109.0 . . ?
H9X C9X H9Y 107.8 . . ?
N11X C10X C9X 109.10(15) . . ?
N11X C10X H10X 109.9 . . ?
C9X C10X H10X 109.9 . . ?
N11X C10X H10Y 109.9 . . ?
C9X C10X H10Y 109.9 . . ?
H10X C10X H10Y 108.3 . . ?
C10X N11X C12X 111.89(15) . . ?
C10X N11X Co1X 107.48(11) . . ?
C12X N11X Co1X 115.18(12) . . ?
C10X N11X H11X 107.1(14) . . ?
C12X N11X H11X 107.8(14) . . ?
Co1X N11X H11X 107.0(14) . . ?
N11X C12X C13X 111.67(17) . . ?
N11X C12X H12X 109.3 . . ?
C13X C12X H12X 109.3 . . ?
N11X C12X H12Y 109.3 . . ?
C13X C12X H12Y 109.3 . . ?
H12X C12X H12Y 107.9 . . ?
C12X C13X C14X 115.29(17) . . ?
C12X C13X H13X 108.5 . . ?
C14X C13X H13X 108.5 . . ?
C12X C13X H13Y 108.5 . . ?
C14X C13X H13Y 108.5 . . ?
H13X C13X H13Y 107.5 . . ?
N1X C14X C13X 115.10(15) . . ?
N1X C14X H14X 108.5 . . ?
C13X C14X H14X 108.5 . . ?
N1X C14X H14Y 108.5 . . ?
C13X C14X H14Y 108.5 . . ?
H14X C14X H14Y 107.5 . . ?
N1X C20X P1X 113.49(11) . . ?
N1X C20X H20X 108.9 . . ?
P1X C20X H20X 108.9 . . ?
N1X C20X H20Y 108.9 . . ?
P1X C20X H20Y 108.9 . . ?
H20X C20X H20Y 107.7 . . ?
O12X P1X O11X 117.23(7) . . ?
O12X P1X C21X 109.71(8) . . ?
O11X P1X C21X 104.56(8) . . ?
O12X P1X C20X 111.18(8) . . ?
O11X P1X C20X 106.85(7) . . ?
C21X P1X C20X 106.63(8) . . ?
P1X O11X Co1X 118.01(7) . . ?
P1X O12X Li2 139.06(13) . 1_565 ?
C22X C21X P1X 116.19(13) . . ?
C22X C21X H21X 108.2 . . ?
P1X C21X H21X 108.2 . . ?
C22X C21X H21Y 108.2 . . ?
P1X C21X H21Y 108.2 . . ?
H21X C21X H21Y 107.4 . . ?
F1X C22X F3X 106.23(15) . . ?
F1X C22X F2X 107.08(15) . . ?
F3X C22X F2X 105.68(14) . . ?
F1X C22X C21X 112.50(14) . . ?
F3X C22X C21X 112.07(15) . . ?
F2X C22X C21X 112.78(15) . . ?
N8X C30X P2X 113.02(12) . . ?
N8X C30X H30X 109.0 . . ?
P2X C30X H30X 109.0 . . ?
N8X C30X H30Y 109.0 . . ?
P2X C30X H30Y 109.0 . . ?
H30X C30X H30Y 107.8 . . ?
O22X P2X O21X 118.00(9) . . ?
O22X P2X C31X 108.57(9) . . ?
O21X P2X C31X 105.69(8) . . ?
O22X P2X C30X 111.73(9) . . ?
O21X P2X C30X 105.33(8) . . ?
C31X P2X C30X 106.86(9) . . ?
P2X O21X Co1X 117.86(7) . . ?
P2X O22X Li2 147.61(14) . . ?
C32X C31X P2X 115.75(14) . . ?
C32X C31X H31X 108.3 . . ?
P2X C31X H31X 108.3 . . ?
C32X C31X H31Y 108.3 . . ?
P2X C31X H31Y 108.3 . . ?
H31X C31X H31Y 107.4 . . ?
F4X C32X F5X 106.32(18) . . ?
F4X C32X F6X 107.43(18) . . ?
F5X C32X F6X 105.43(17) . . ?
F4X C32X C31X 112.09(17) . . ?
F5X C32X C31X 113.43(17) . . ?
F6X C32X C31X 111.68(18) . . ?
O12A Li1 O2W 117.0(2) . . ?
O12A Li1 O1W 108.1(2) . . ?
O2W Li1 O1W 114.80(19) . . ?
O12A Li1 O3W 118.5(2) . . ?
O2W Li1 O3W 100.23(19) . . ?
O1W Li1 O3W 96.55(17) . . ?
O12A Li1 H31W 119.9(11) . . ?
O2W Li1 H31W 115.2(12) . . ?
O1W Li1 H31W 73.6(12) . . ?
O3W Li1 H31W 23.8(12) . . ?
O22A Li2 O22X 124.41(18) . . ?
O22A Li2 O12X 125.73(18) . 1_545 ?
O22X Li2 O12X 109.56(16) . 1_545 ?
Li1 O1W H11W 102.8(19) . . ?
Li1 O1W H12W 101.0(19) . . ?
H11W O1W H12W 105(3) . . ?
Li1 O2W H21W 126(2) . . ?
Li1 O2W H22W 121(3) . . ?
H21W O2W H22W 112(4) . . ?
Li1 O3W H31W 98(3) . . ?
Li1 O3W H32W 115(4) . . ?
H31W O3W H32W 131(4) . . ?
H41W O4W H42W 104(3) . . ?
H51W O5W H52W 107(3) . . ?
H61W O6W H62W 108.4 . . ?

_refine_diff_density_max         0.822
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.065


