# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_mnnotpf3
_database_code_depnum_ccdc_archive 'CCDC 2327147'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2024-01-20 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C15 H24 F9 Mn N3 O6 P3), H12 Mn O6, 18(H2 O)'
_chemical_formula_sum            'C30 H96 F18 Mn3 N6 O36 P6'
_chemical_formula_weight         1809.76

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'
Mn Mn 0.3368 0.7283 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   17.3178(3)
_cell_length_b                   17.3178(3)
_cell_length_c                   21.8650(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5678.9(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9834
_cell_measurement_theta_min      2.8717
_cell_measurement_theta_max      27.4647

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_F_000             2799
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.475
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.164
_exptl_absorpt_coefficient_mu    0.747
_shelx_estimated_absorpt_T_min   0.718
_shelx_estimated_absorpt_T_max   0.887
_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  0.75
_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            12613
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.305
_diffrn_reflns_theta_max         27.488
_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             2890
_reflns_number_gt                2770
_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-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0703P)²] 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         2890
_refine_ls_number_parameters     175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.1100
_refine_ls_wR_factor_gt          0.0970
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_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
Mn1 Mn 0.666667 0.333333 0.56245(2) 0.01450(15) Uani 1 3 d S T P . .
N1 N 0.73576(12) 0.44343(13) 0.63714(8) 0.0165(4) Uani 1 1 d . . . . .
C2 C 0.80459(16) 0.42505(15) 0.66261(10) 0.0193(5) Uani 1 1 d . . . . .
H21 H 0.834657 0.465887 0.697349 0.023 Uiso 1 1 calc R U . . .
H22 H 0.850090 0.437539 0.630823 0.023 Uiso 1 1 calc R U . . .
C3 C 0.76586(16) 0.32903(16) 0.68445(10) 0.0203(5) Uani 1 1 d . . . . .
H31 H 0.815147 0.317806 0.694442 0.024 Uiso 1 1 calc R U . . .
H32 H 0.730772 0.320192 0.722173 0.024 Uiso 1 1 calc R U . . .
C4 C 0.77905(16) 0.53201(15) 0.60655(10) 0.0192(5) Uani 1 1 d . . . . .
H41 H 0.825099 0.577209 0.633822 0.023 Uiso 1 1 calc R U . . .
H42 H 0.733996 0.549953 0.598299 0.023 Uiso 1 1 calc R U . . .
P1 P 0.83064(4) 0.52717(4) 0.53439(3) 0.01723(15) Uani 1 1 d . . . . .
O11 O 0.77217(12) 0.43308(11) 0.51031(7) 0.0228(4) Uani 1 1 d . . . . .
O12 O 0.92688(12) 0.55521(14) 0.54262(8) 0.0282(4) Uani 1 1 d . . . . .
C5 C 0.81774(17) 0.60024(18) 0.48071(11) 0.0257(5) Uani 1 1 d . . . . .
H51 H 0.824350 0.583116 0.438664 0.031 Uiso 1 1 calc R U . . .
H52 H 0.756461 0.590291 0.484555 0.031 Uiso 1 1 calc R U . . .
C6 C 0.8821(2) 0.6973(2) 0.48908(14) 0.0355(6) Uani 1 1 d . . . . .
F61 F 0.88480(17) 0.72315(12) 0.54751(9) 0.0506(6) Uani 1 1 d . . . . .
F62 F 0.96511(14) 0.72002(13) 0.47258(11) 0.0541(6) Uani 1 1 d . . . . .
F63 F 0.85997(17) 0.74801(14) 0.45547(9) 0.0552(6) Uani 1 1 d . . . . .
Mn2 Mn 0.666667 0.333333 0.333333 0.01484(18) Uani 1 6 d S T P . .
O1W O 0.78380(12) 0.38574(15) 0.39148(8) 0.0267(4) Uani 1 1 d . . . . .
H11W H 0.784(2) 0.401(3) 0.4235(16) 0.031(9) Uiso 1 1 d . . . . .
H12W H 0.836(2) 0.392(2) 0.3838(15) 0.031(8) Uiso 1 1 d . . . . .
O2W O 0.94787(13) 0.40324(14) 0.36461(10) 0.0294(4) Uani 1 1 d . . . . .
H21W H 0.984(3) 0.408(3) 0.3946(18) 0.047(11) Uiso 1 1 d . . . . .
H22W H 0.946(3) 0.362(4) 0.342(2) 0.075(16) Uiso 1 1 d . . . . .
O3W O 1.06989(13) 0.61616(13) 0.46719(10) 0.0300(4) Uani 1 1 d . . . . .
H31W H 1.031(2) 0.600(2) 0.4937(14) 0.058(13) Uiso 1 1 d . . . . .
H32W H 1.100720 0.588838 0.469560 0.069 Uiso 1 1 d R U . . .
O4W O 0.91908(17) 0.24848(16) 0.31792(11) 0.0400(5) Uani 1 1 d . . . . .
H41W H 0.927654 0.251507 0.275647 0.048 Uiso 1 1 d R U . . .
H42W H 0.858(4) 0.206(4) 0.325(2) 0.075(15) 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
Mn1 O11 2.1131(16) 2_655 ?
Mn1 O11 2.1132(17) . ?
Mn1 O11 2.1132(16) 3_665 ?
Mn1 N1 2.3351(18) 3_665 ?
Mn1 N1 2.3351(18) 2_655 ?
Mn1 N1 2.3351(18) . ?
N1 C2 1.487(3) . ?
N1 C4 1.488(3) . ?
N1 C3 1.488(3) 2_655 ?
C2 C3 1.526(3) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
C4 P1 1.836(2) . ?
C4 H41 0.9900 . ?
C4 H42 0.9900 . ?
P1 O12 1.4955(18) . ?
P1 O11 1.5190(17) . ?
P1 C5 1.820(3) . ?
C5 C6 1.492(4) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 F62 1.336(4) . ?
C6 F63 1.340(4) . ?
C6 F61 1.347(4) . ?
Mn2 O1W 2.1712(17) . ?
Mn2 O1W 2.1712(17) 16_655 ?
Mn2 O1W 2.1712(17) 3_665 ?
Mn2 O1W 2.1712(17) 18_545 ?
Mn2 O1W 2.1712(17) 2_655 ?
Mn2 O1W 2.1713(17) 17 ?
O1W H11W 0.75(4) . ?
O1W H12W 0.87(4) . ?
O2W H21W 0.88(4) . ?
O2W H22W 0.86(5) . ?
O3W H31W 0.82(3) . ?
O3W H32W 0.8742 . ?
O4W H41W 0.9335 . ?
O4W H42W 0.96(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Mn1 O11 93.64(6) 2_655 . ?
O11 Mn1 O11 93.64(6) 2_655 3_665 ?
O11 Mn1 O11 93.64(6) . 3_665 ?
O11 Mn1 N1 150.07(7) 2_655 3_665 ?
O11 Mn1 N1 115.85(7) . 3_665 ?
O11 Mn1 N1 80.16(6) 3_665 3_665 ?
O11 Mn1 N1 80.17(6) 2_655 2_655 ?
O11 Mn1 N1 150.07(7) . 2_655 ?
O11 Mn1 N1 115.85(7) 3_665 2_655 ?
N1 Mn1 N1 76.49(7) 3_665 2_655 ?
O11 Mn1 N1 115.85(7) 2_655 . ?
O11 Mn1 N1 80.17(6) . . ?
O11 Mn1 N1 150.07(7) 3_665 . ?
N1 Mn1 N1 76.48(7) 3_665 . ?
N1 Mn1 N1 76.49(7) 2_655 . ?
C2 N1 C4 110.16(18) . . ?
C2 N1 C3 112.19(17) . 2_655 ?
C4 N1 C3 111.32(18) . 2_655 ?
C2 N1 Mn1 103.03(13) . . ?
C4 N1 Mn1 108.41(12) . . ?
C3 N1 Mn1 111.38(14) 2_655 . ?
N1 C2 C3 112.82(19) . . ?
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 . . ?
N1 C3 C2 111.55(17) 3_665 . ?
N1 C3 H31 109.3 3_665 . ?
C2 C3 H31 109.3 . . ?
N1 C3 H32 109.3 3_665 . ?
C2 C3 H32 109.3 . . ?
H31 C3 H32 108.0 . . ?
N1 C4 P1 110.19(14) . . ?
N1 C4 H41 109.6 . . ?
P1 C4 H41 109.6 . . ?
N1 C4 H42 109.6 . . ?
P1 C4 H42 109.6 . . ?
H41 C4 H42 108.1 . . ?
O12 P1 O11 115.28(12) . . ?
O12 P1 C5 110.87(12) . . ?
O11 P1 C5 105.94(12) . . ?
O12 P1 C4 111.75(11) . . ?
O11 P1 C4 105.56(10) . . ?
C5 P1 C4 106.90(11) . . ?
P1 O11 Mn1 122.01(9) . . ?
C6 C5 P1 114.94(19) . . ?
C6 C5 H51 108.5 . . ?
P1 C5 H51 108.5 . . ?
C6 C5 H52 108.5 . . ?
P1 C5 H52 108.5 . . ?
H51 C5 H52 107.5 . . ?
F62 C6 F63 106.1(2) . . ?
F62 C6 F61 107.8(3) . . ?
F63 C6 F61 106.0(2) . . ?
F62 C6 C5 112.8(3) . . ?
F63 C6 C5 111.9(3) . . ?
F61 C6 C5 111.9(2) . . ?
O1W Mn2 O1W 180.0 . 16_655 ?
O1W Mn2 O1W 89.18(7) . 3_665 ?
O1W Mn2 O1W 90.82(7) 16_655 3_665 ?
O1W Mn2 O1W 90.82(7) . 18_545 ?
O1W Mn2 O1W 89.18(7) 16_655 18_545 ?
O1W Mn2 O1W 180.0 3_665 18_545 ?
O1W Mn2 O1W 89.18(7) . 2_655 ?
O1W Mn2 O1W 90.82(7) 16_655 2_655 ?
O1W Mn2 O1W 89.18(7) 3_665 2_655 ?
O1W Mn2 O1W 90.82(7) 18_545 2_655 ?
O1W Mn2 O1W 90.82(7) . 17 ?
O1W Mn2 O1W 89.18(7) 16_655 17 ?
O1W Mn2 O1W 90.82(7) 3_665 17 ?
O1W Mn2 O1W 89.18(7) 18_545 17 ?
O1W Mn2 O1W 180.00(7) 2_655 17 ?
Mn2 O1W H11W 123(3) . . ?
Mn2 O1W H12W 129(2) . . ?
H11W O1W H12W 108(3) . . ?
H21W O2W H22W 104(4) . . ?
H31W O3W H32W 112.6 . . ?
H41W O4W H42W 106.8 . . ?

_refine_diff_density_max         0.312
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.070

####################################################################### 
# 
# 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_tfepin
_database_code_depnum_ccdc_archive 'CCDC 2327148'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2024-01-20 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H3 F3 O2 P, H4 N'
_chemical_formula_sum            'C2 H7 F3 N O2 P'
_chemical_formula_weight         165.06

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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   7.3490(4)
_cell_length_b                   11.7365(6)
_cell_length_c                   15.2447(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1314.88(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9832
_cell_measurement_theta_min      3.7662
_cell_measurement_theta_max      72.0772

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_F_000             672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.146
_exptl_absorpt_coefficient_mu    3.857
_shelx_estimated_absorpt_T_min   0.438
_shelx_estimated_absorpt_T_max   0.603
_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  0.50
_exptl_absorpt_correction_T_max  0.60
_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            24949
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         5.805
_diffrn_reflns_theta_max         72.128
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1287
_reflns_number_gt                1283
_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 vV6.2.14'
_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-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_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)+(0.0364P)²+0.9615P] 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         1287
_refine_ls_number_parameters     102
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0759
_refine_ls_wR_factor_gt          0.0759
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_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
P1 P 0.41107(5) 0.59238(3) 0.36954(2) 0.01779(15) Uani 1 1 d . . . . .
H1P H 0.466(3) 0.5917(16) 0.4487(13) 0.028(5) Uiso 1 1 d . . . . .
O1 O 0.43851(14) 0.70861(9) 0.33124(7) 0.0244(3) Uani 1 1 d . . . . .
O2 O 0.49047(15) 0.49234(9) 0.32187(7) 0.0252(3) Uani 1 1 d . . . . .
C1 C 0.1678(2) 0.56319(14) 0.37834(10) 0.0239(3) Uani 1 1 d . . . . .
H11 H 0.116194 0.560709 0.318371 0.029 Uiso 1 1 calc R U . . .
H12 H 0.152268 0.486482 0.404296 0.029 Uiso 1 1 calc R U . . .
C2 C 0.0590(3) 0.64564(15) 0.43116(12) 0.0323(4) Uani 1 1 d . . . . .
F1 F 0.05630(16) 0.75051(9) 0.39699(8) 0.0446(3) Uani 1 1 d . . . . .
F2 F 0.12108(19) 0.65534(11) 0.51340(7) 0.0510(4) Uani 1 1 d . . . . .
F3 F -0.11632(16) 0.61316(12) 0.43825(9) 0.0537(4) Uani 1 1 d . . . . .
N1A N 0.72511(18) 0.84421(11) 0.27808(10) 0.0212(3) Uani 1 1 d . . . . .
H1A H 0.653(3) 0.8041(19) 0.3092(14) 0.036(6) Uiso 1 1 d . . . . .
H2A H 0.659(3) 0.8907(19) 0.2446(15) 0.034(5) Uiso 1 1 d . . . . .
H3A H 0.788(3) 0.8007(19) 0.2424(14) 0.034(5) Uiso 1 1 d . . . . .
H4A H 0.805(3) 0.8866(19) 0.3098(14) 0.036(6) 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
P1 O1 1.4975(11) . ?
P1 O2 1.4992(11) . ?
P1 C1 1.8255(17) . ?
P1 H1P 1.27(2) . ?
C1 C2 1.491(2) . ?
C1 H11 0.9900 . ?
C1 H12 0.9900 . ?
C2 F1 1.337(2) . ?
C2 F2 1.339(2) . ?
C2 F3 1.348(2) . ?
N1A H1A 0.85(2) . ?
N1A H2A 0.89(2) . ?
N1A H3A 0.88(2) . ?
N1A H4A 0.91(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
O1 P1 O2 118.16(7) . . ?
O1 P1 C1 109.36(7) . . ?
O2 P1 C1 105.66(7) . . ?
O1 P1 H1P 109.5(9) . . ?
O2 P1 H1P 109.4(9) . . ?
C1 P1 H1P 103.8(10) . . ?
C2 C1 P1 116.28(12) . . ?
C2 C1 H11 108.2 . . ?
P1 C1 H11 108.2 . . ?
C2 C1 H12 108.2 . . ?
P1 C1 H12 108.2 . . ?
H11 C1 H12 107.4 . . ?
F1 C2 F2 106.96(16) . . ?
F1 C2 F3 106.11(15) . . ?
F2 C2 F3 105.94(14) . . ?
F1 C2 C1 113.27(14) . . ?
F2 C2 C1 112.22(15) . . ?
F3 C2 C1 111.84(16) . . ?
H1A N1A H2A 109(2) . . ?
H1A N1A H3A 110.5(19) . . ?
H2A N1A H3A 106.9(19) . . ?
H1A N1A H4A 114(2) . . ?
H2A N1A H4A 108.7(18) . . ?
H3A N1A H4A 108(2) . . ?

_refine_diff_density_max         0.284
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.050

####################################################################### 
# 
# 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_conotpf
_database_code_depnum_ccdc_archive 'CCDC 2327154'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2024-01-20 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H24 Co F9 N3 O6 P3, 3.5(H2 O), H4 N'
_chemical_formula_sum            'C15 H35 Co F9 N4 O9.50 P3'
_chemical_formula_weight         746.31

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'
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'
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           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                   25.658(2)
_cell_length_b                   9.3786(7)
_cell_length_c                   24.1366(19)
_cell_angle_alpha                90
_cell_angle_beta                 100.726(3)
_cell_angle_gamma                90
_cell_volume                     5706.6(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9734
_cell_measurement_theta_min      2.3170
_cell_measurement_theta_max      27.6661

_exptl_crystal_description       prism
_exptl_crystal_colour            'light violet'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_F_000             3056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.182
_exptl_absorpt_coefficient_mu    0.881
_shelx_estimated_absorpt_T_min   0.732
_shelx_estimated_absorpt_T_max   0.856
_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  0.75
_exptl_absorpt_correction_T_max  0.86
_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            40100
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.317
_diffrn_reflns_theta_max         27.666
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6587
_reflns_number_gt                6208
_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-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_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)+30.6926P] 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         6587
_refine_ls_number_parameters     477
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.1035
_refine_ls_wR_factor_gt          0.1024
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_restrained_S_all      1.161
_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
Co1 Co 0.35961(2) 0.53172(4) 0.64822(2) 0.01486(9) Uani 1 1 d . . . . .
N1 N 0.40855(10) 0.5872(2) 0.58767(9) 0.0212(5) Uani 1 1 d . . . . .
C2 C 0.37008(14) 0.6463(3) 0.53960(12) 0.0301(7) Uani 1 1 d . . . . .
H21 H 0.348602 0.567753 0.519592 0.036 Uiso 1 1 calc R U . . .
H22 H 0.389566 0.692540 0.512722 0.036 Uiso 1 1 calc R U . . .
C3 C 0.33339(14) 0.7551(3) 0.55980(12) 0.0305(7) Uani 1 1 d . . . . .
H31 H 0.353295 0.844708 0.569905 0.037 Uiso 1 1 calc R U . . .
H32 H 0.303617 0.776497 0.528492 0.037 Uiso 1 1 calc R U . . .
N4 N 0.31152(10) 0.7046(2) 0.60947(9) 0.0211(5) Uani 1 1 d . . . . .
C5 C 0.31621(12) 0.8143(3) 0.65439(12) 0.0245(6) Uani 1 1 d . . . . .
H51 H 0.297060 0.782197 0.684170 0.029 Uiso 1 1 calc R U . . .
H52 H 0.299894 0.904464 0.638383 0.029 Uiso 1 1 calc R U . . .
C6 C 0.37477(13) 0.8395(3) 0.67995(13) 0.0285(6) Uani 1 1 d . . . . .
H61 H 0.391772 0.892279 0.652539 0.034 Uiso 1 1 calc R U . . .
H62 H 0.377245 0.899196 0.714177 0.034 Uiso 1 1 calc R U . . .
N7 N 0.40366(10) 0.7041(3) 0.69496(10) 0.0228(5) Uani 1 1 d . . . . .
C8 C 0.45534(12) 0.7019(3) 0.67642(13) 0.0277(6) Uani 1 1 d . . . . .
H81 H 0.475978 0.618024 0.692932 0.033 Uiso 1 1 calc R U . . .
H82 H 0.475633 0.788711 0.690239 0.033 Uiso 1 1 calc R U . . .
C9 C 0.44804(13) 0.6955(3) 0.61255(13) 0.0298(7) Uani 1 1 d . . . . .
H91 H 0.436516 0.790199 0.596751 0.036 Uiso 1 1 calc R U . . .
H92 H 0.482542 0.673182 0.601816 0.036 Uiso 1 1 calc R U . . .
C10 C 0.43317(12) 0.4547(3) 0.57277(11) 0.0235(6) Uani 1 1 d . . . . .
H101 H 0.463571 0.477617 0.554382 0.028 Uiso 1 1 calc R U . . .
H102 H 0.407096 0.399165 0.545828 0.028 Uiso 1 1 calc R U . . .
P1 P 0.45598(3) 0.34916(7) 0.63622(3) 0.01753(14) Uani 1 1 d . . . . .
O11 O 0.41198(7) 0.3654(2) 0.66999(7) 0.0184(4) Uani 1 1 d . . . . .
O12 O 0.51092(8) 0.3868(2) 0.66419(9) 0.0258(4) Uani 1 1 d . . . . .
C11 C 0.45337(11) 0.1638(3) 0.61353(12) 0.0208(5) Uani 1 1 d . . . . .
H111 H 0.458657 0.102232 0.647435 0.025 Uiso 1 1 calc R U . . .
H112 H 0.417430 0.144067 0.591767 0.025 Uiso 1 1 calc R U . . .
C12 C 0.49294(14) 0.1228(3) 0.57845(14) 0.0325(7) Uani 1 1 d . . . . .
F121 F 0.49162(11) 0.2077(2) 0.53386(10) 0.0527(6) Uani 1 1 d . . . . .
F122 F 0.54258(8) 0.1239(3) 0.60727(11) 0.0580(7) Uani 1 1 d . . . . .
F123 F 0.48422(9) -0.0096(2) 0.55800(9) 0.0436(5) Uani 1 1 d . . . . .
C20 C 0.25647(12) 0.6534(3) 0.59404(12) 0.0252(6) Uani 1 1 d . . . . .
H201 H 0.235319 0.721191 0.567467 0.030 Uiso 1 1 calc R U . . .
H202 H 0.240328 0.647181 0.628160 0.030 Uiso 1 1 calc R U . . .
P2 P 0.25607(3) 0.47787(8) 0.56114(3) 0.02210(16) Uani 1 1 d . . . . .
O21 O 0.30661(8) 0.4094(2) 0.59347(9) 0.0248(4) Uani 1 1 d . . . . .
O22 O 0.24894(9) 0.4858(2) 0.49878(9) 0.0265(4) Uani 1 1 d . . . . .
C21 C 0.20285(12) 0.3784(3) 0.58282(13) 0.0273(6) Uani 1 1 d . . . . .
H211 H 0.207590 0.276515 0.574267 0.033 Uiso 1 1 calc R U . . .
H212 H 0.206819 0.387081 0.624269 0.033 Uiso 1 1 calc R U . . .
C22 C 0.14760(13) 0.4196(4) 0.55724(13) 0.0331(7) Uani 1 1 d . . . . .
F221 F 0.14007(9) 0.5602(3) 0.55878(11) 0.0540(6) Uani 1 1 d . . . . .
F222 F 0.13438(8) 0.3798(3) 0.50356(9) 0.0583(7) Uani 1 1 d . . . . .
F223 F 0.11159(8) 0.3604(3) 0.58376(9) 0.0466(5) Uani 1 1 d . . . . .
C30 C 0.41009(12) 0.6703(4) 0.75538(12) 0.0281(6) Uani 1 1 d . . . . .
H301 H 0.422383 0.755963 0.778041 0.034 Uiso 0.683(4) 1 calc R U P A 1
H302 H 0.437098 0.594533 0.765268 0.034 Uiso 0.683(4) 1 calc R U P A 1
H304 H 0.416833 0.758870 0.777879 0.034 Uiso 0.317(4) 1 calc R U P A 2
H305 H 0.440836 0.605926 0.766575 0.034 Uiso 0.317(4) 1 calc R U P A 2
P3A P 0.34920(15) 0.6125(3) 0.77073(17) 0.0147(5) Uani 0.683(4) 1 d . . P A 1
O32A O 0.3147(3) 0.7321(6) 0.7838(4) 0.0204(11) Uani 0.683(4) 1 d . . P A 1
C31A C 0.37340(17) 0.5164(6) 0.83578(18) 0.0206(9) Uani 0.683(4) 1 d . . P A 1
H311 H 0.401054 0.448390 0.828986 0.025 Uiso 0.683(4) 1 calc R U P A 1
H312 H 0.390461 0.585426 0.864551 0.025 Uiso 0.683(4) 1 calc R U P A 1
C32A C 0.33230(17) 0.4360(5) 0.85918(17) 0.0226(9) Uani 0.683(4) 1 d . . P A 1
F321 F 0.30764(14) 0.3392(3) 0.82356(12) 0.0442(9) Uani 0.683(4) 1 d . . P A 1
F322 F 0.29461(13) 0.5206(3) 0.87257(15) 0.0421(9) Uani 0.683(4) 1 d . . P A 1
F323 F 0.35289(14) 0.3672(4) 0.90647(12) 0.0409(8) Uani 0.683(4) 1 d . . P A 1
P3B P 0.3433(4) 0.5748(7) 0.7706(4) 0.0249(15) Uani 0.317(4) 1 d . . P A 2
O32B O 0.3080(7) 0.6900(13) 0.7860(8) 0.029(3) Uani 0.317(4) 1 d . U P A 2
C31B C 0.3585(6) 0.4460(13) 0.8269(4) 0.032(3) Uani 0.317(4) 1 d . . P A 2
H314 H 0.326133 0.389030 0.827722 0.039 Uiso 0.317(4) 1 calc R U P A 2
H315 H 0.385773 0.380046 0.817742 0.039 Uiso 0.317(4) 1 calc R U P A 2
C32B C 0.3778(6) 0.5040(14) 0.8848(4) 0.044(3) Uani 0.317(4) 1 d . . P A 2
F324 F 0.4139(3) 0.6035(9) 0.8863(3) 0.054(2) Uani 0.317(4) 1 d . . P A 2
F325 F 0.3358(4) 0.5561(9) 0.9057(3) 0.063(3) Uani 0.317(4) 1 d . . P A 2
F326 F 0.3974(4) 0.3995(10) 0.9194(3) 0.068(3) Uani 0.317(4) 1 d . . P A 2
O31 O 0.32591(8) 0.5060(2) 0.72163(8) 0.0247(4) Uani 1 1 d . . . . .
N1A N 0.20700(12) 0.7105(3) 0.79469(13) 0.0308(6) Uani 1 1 d . . . . .
H11A H 0.243921 0.711360 0.792319 0.037 Uiso 1 1 d R U . . .
H12A H 0.1929(17) 0.807(5) 0.7891(17) 0.049(12) Uiso 1 1 d . . . . .
H13A H 0.1864(16) 0.655(4) 0.7708(17) 0.037(10) Uiso 1 1 d . . . . .
H14A H 0.2013(16) 0.681(4) 0.8304(18) 0.043(11) Uiso 1 1 d . . . . .
O1W O 0.57763(9) 0.2001(3) 0.73261(11) 0.0308(5) Uani 1 1 d . . . . .
H11W H 0.5584(15) 0.252(4) 0.7109(16) 0.027(10) Uiso 1 1 d . . . . .
H12W H 0.5804(18) 0.238(5) 0.761(2) 0.049(13) Uiso 1 1 d . . . . .
O2W O 0.31510(9) 0.1232(2) 0.59753(8) 0.0248(4) Uani 1 1 d . . . . .
H21W H 0.3204(14) 0.212(4) 0.5899(14) 0.058(14) Uiso 1 1 d . . . . .
H22W H 0.297444 0.086002 0.570157 0.069 Uiso 1 1 d R U . . .
O3W O 0.33298(10) 1.0224(3) 0.79413(10) 0.0331(7) Uani 0.891(6) 1 d . . P B 1
H31W H 0.369304 1.036020 0.795946 0.040 Uiso 0.891(6) 1 d R U P B 1
H32W H 0.330986 0.923674 0.797874 0.040 Uiso 0.891(6) 1 d R U P B 1
O3V O 0.2886(9) 0.981(2) 0.7802(8) 0.032(6) Uani 0.109(6) 1 d . . P B 2
H31V H 0.294389 0.907053 0.760881 0.039 Uiso 0.109(6) 1 d R U P B 2
H32V H 0.261631 0.947797 0.790502 0.039 Uiso 0.109(6) 1 d R U P B 2
O4W O 0.500000 -0.0009(4) 0.750000 0.0372(8) Uani 1 2 d S T P . .
H41W H 0.5227(16) 0.047(5) 0.7448(19) 0.047(13) 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
Co1 O21 2.0596(19) . ?
Co1 O11 2.0621(18) . ?
Co1 O31 2.125(2) . ?
Co1 N4 2.144(2) . ?
Co1 N1 2.160(2) . ?
Co1 N7 2.165(2) . ?
N1 C10 1.468(4) . ?
N1 C9 1.481(4) . ?
N1 C2 1.484(4) . ?
C2 C3 1.528(5) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.492(4) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C20 1.473(4) . ?
N4 C5 1.483(3) . ?
C5 C6 1.533(4) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.481(4) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C30 1.472(4) . ?
N7 C8 1.476(4) . ?
C8 C9 1.519(4) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
C10 P1 1.826(3) . ?
C10 H101 0.9900 . ?
C10 H102 0.9900 . ?
P1 O12 1.488(2) . ?
P1 O11 1.5181(19) . ?
P1 C11 1.820(3) . ?
C11 C12 1.489(4) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 F122 1.333(4) . ?
C12 F121 1.334(4) . ?
C12 F123 1.339(4) . ?
C20 P2 1.827(3) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P2 O22 1.484(2) . ?
P2 O21 1.525(2) . ?
P2 C21 1.810(3) . ?
C21 C22 1.488(4) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
C22 F222 1.330(4) . ?
C22 F221 1.334(4) . ?
C22 F223 1.339(4) . ?
C30 P3A 1.757(5) . ?
C30 P3B 2.027(9) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C30 H304 0.9900 . ?
C30 H305 0.9900 . ?
P3A O32A 1.497(8) . ?
P3A O31 1.580(4) . ?
P3A C31A 1.817(6) . ?
C31A C32A 1.490(6) . ?
C31A H311 0.9900 . ?
C31A H312 0.9900 . ?
C32A F321 1.327(5) . ?
C32A F323 1.332(5) . ?
C32A F322 1.336(5) . ?
P3B O31 1.348(10) . ?
P3B O32B 1.50(2) . ?
P3B C31B 1.806(13) . ?
C31B C32B 1.494(17) . ?
C31B H314 0.9900 . ?
C31B H315 0.9900 . ?
C32B F324 1.312(17) . ?
C32B F326 1.325(12) . ?
C32B F325 1.362(13) . ?
N1A H11A 0.9597 . ?
N1A H12A 0.97(5) . ?
N1A H13A 0.88(4) . ?
N1A H14A 0.94(4) . ?
O1W H11W 0.81(4) . ?
O1W H12W 0.76(5) . ?
O2W H21W 0.87(4) . ?
O2W H22W 0.8075 . ?
O3W H31W 0.9337 . ?
O3W H32W 0.9324 . ?
O3V H31V 0.8620 . ?
O3V H32V 0.8363 . ?
O4W H41W 0.77(4) . ?
O4W H41W 0.77(4) 2_656 ?

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 Co1 O11 93.63(8) . . ?
O21 Co1 O31 98.59(9) . . ?
O11 Co1 O31 92.80(7) . . ?
O21 Co1 N4 83.32(8) . . ?
O11 Co1 N4 167.97(8) . . ?
O31 Co1 N4 99.16(9) . . ?
O21 Co1 N1 95.59(9) . . ?
O11 Co1 N1 85.48(8) . . ?
O31 Co1 N1 165.80(9) . . ?
N4 Co1 N1 83.25(9) . . ?
O21 Co1 N7 165.53(9) . . ?
O11 Co1 N7 100.36(8) . . ?
O31 Co1 N7 84.51(9) . . ?
N4 Co1 N7 82.23(9) . . ?
N1 Co1 N7 81.94(9) . . ?
C10 N1 C9 112.7(2) . . ?
C10 N1 C2 112.2(2) . . ?
C9 N1 C2 111.5(2) . . ?
C10 N1 Co1 107.03(16) . . ?
C9 N1 Co1 109.32(17) . . ?
C2 N1 Co1 103.47(18) . . ?
N1 C2 C3 111.1(2) . . ?
N1 C2 H21 109.4 . . ?
C3 C2 H21 109.4 . . ?
N1 C2 H22 109.4 . . ?
C3 C2 H22 109.4 . . ?
H21 C2 H22 108.0 . . ?
N4 C3 C2 113.0(2) . . ?
N4 C3 H31 109.0 . . ?
C2 C3 H31 109.0 . . ?
N4 C3 H32 109.0 . . ?
C2 C3 H32 109.0 . . ?
H31 C3 H32 107.8 . . ?
C20 N4 C5 110.8(2) . . ?
C20 N4 C3 112.7(2) . . ?
C5 N4 C3 112.1(2) . . ?
C20 N4 Co1 108.12(16) . . ?
C5 N4 Co1 104.10(16) . . ?
C3 N4 Co1 108.58(18) . . ?
N4 C5 C6 110.0(2) . . ?
N4 C5 H51 109.7 . . ?
C6 C5 H51 109.7 . . ?
N4 C5 H52 109.7 . . ?
C6 C5 H52 109.7 . . ?
H51 C5 H52 108.2 . . ?
N7 C6 C5 112.0(2) . . ?
N7 C6 H61 109.2 . . ?
C5 C6 H61 109.2 . . ?
N7 C6 H62 109.2 . . ?
C5 C6 H62 109.2 . . ?
H61 C6 H62 107.9 . . ?
C30 N7 C8 110.9(2) . . ?
C30 N7 C6 112.7(2) . . ?
C8 N7 C6 112.0(2) . . ?
C30 N7 Co1 107.86(19) . . ?
C8 N7 Co1 104.07(16) . . ?
C6 N7 Co1 108.90(16) . . ?
N7 C8 C9 111.1(2) . . ?
N7 C8 H81 109.4 . . ?
C9 C8 H81 109.4 . . ?
N7 C8 H82 109.4 . . ?
C9 C8 H82 109.4 . . ?
H81 C8 H82 108.0 . . ?
N1 C9 C8 112.6(2) . . ?
N1 C9 H91 109.1 . . ?
C8 C9 H91 109.1 . . ?
N1 C9 H92 109.1 . . ?
C8 C9 H92 109.1 . . ?
H91 C9 H92 107.8 . . ?
N1 C10 P1 109.78(18) . . ?
N1 C10 H101 109.7 . . ?
P1 C10 H101 109.7 . . ?
N1 C10 H102 109.7 . . ?
P1 C10 H102 109.7 . . ?
H101 C10 H102 108.2 . . ?
O12 P1 O11 117.97(11) . . ?
O12 P1 C11 110.00(13) . . ?
O11 P1 C11 105.55(12) . . ?
O12 P1 C10 112.35(13) . . ?
O11 P1 C10 103.99(12) . . ?
C11 P1 C10 106.11(13) . . ?
P1 O11 Co1 116.97(10) . . ?
C12 C11 P1 115.3(2) . . ?
C12 C11 H111 108.5 . . ?
P1 C11 H111 108.5 . . ?
C12 C11 H112 108.5 . . ?
P1 C11 H112 108.5 . . ?
H111 C11 H112 107.5 . . ?
F122 C12 F121 107.1(3) . . ?
F122 C12 F123 106.1(3) . . ?
F121 C12 F123 106.2(3) . . ?
F122 C12 C11 112.8(3) . . ?
F121 C12 C11 112.8(3) . . ?
F123 C12 C11 111.4(3) . . ?
N4 C20 P2 109.33(19) . . ?
N4 C20 H201 109.8 . . ?
P2 C20 H201 109.8 . . ?
N4 C20 H202 109.8 . . ?
P2 C20 H202 109.8 . . ?
H201 C20 H202 108.3 . . ?
O22 P2 O21 118.21(13) . . ?
O22 P2 C21 111.22(13) . . ?
O21 P2 C21 104.51(13) . . ?
O22 P2 C20 112.67(13) . . ?
O21 P2 C20 102.80(12) . . ?
C21 P2 C20 106.39(15) . . ?
P2 O21 Co1 119.40(11) . . ?
C22 C21 P2 117.3(2) . . ?
C22 C21 H211 108.0 . . ?
P2 C21 H211 108.0 . . ?
C22 C21 H212 108.0 . . ?
P2 C21 H212 108.0 . . ?
H211 C21 H212 107.2 . . ?
F222 C22 F221 107.0(3) . . ?
F222 C22 F223 106.0(3) . . ?
F221 C22 F223 106.3(3) . . ?
F222 C22 C21 112.4(3) . . ?
F221 C22 C21 112.1(3) . . ?
F223 C22 C21 112.5(3) . . ?
N7 C30 P3A 109.6(2) . . ?
N7 C30 P3B 109.4(3) . . ?
N7 C30 H301 109.8 . . ?
P3A C30 H301 109.8 . . ?
N7 C30 H302 109.8 . . ?
P3A C30 H302 109.8 . . ?
H301 C30 H302 108.2 . . ?
N7 C30 H304 109.8 . . ?
P3B C30 H304 109.8 . . ?
N7 C30 H305 109.8 . . ?
P3B C30 H305 109.8 . . ?
H304 C30 H305 108.2 . . ?
O32A P3A O31 118.4(4) . . ?
O32A P3A C30 113.4(3) . . ?
O31 P3A C30 105.3(3) . . ?
O32A P3A C31A 108.1(4) . . ?
O31 P3A C31A 110.8(2) . . ?
C30 P3A C31A 99.3(3) . . ?
C32A C31A P3A 115.2(3) . . ?
C32A C31A H311 108.5 . . ?
P3A C31A H311 108.5 . . ?
C32A C31A H312 108.5 . . ?
P3A C31A H312 108.5 . . ?
H311 C31A H312 107.5 . . ?
F321 C32A F323 106.8(4) . . ?
F321 C32A F322 106.5(4) . . ?
F323 C32A F322 105.7(3) . . ?
F321 C32A C31A 112.7(4) . . ?
F323 C32A C31A 112.0(4) . . ?
F322 C32A C31A 112.7(4) . . ?
O31 P3B O32B 116.4(10) . . ?
O31 P3B C31B 109.3(6) . . ?
O32B P3B C31B 110.6(10) . . ?
O31 P3B C30 101.9(6) . . ?
O32B P3B C30 107.3(6) . . ?
C31B P3B C30 111.2(7) . . ?
C32B C31B P3B 116.6(9) . . ?
C32B C31B H314 108.2 . . ?
P3B C31B H314 108.2 . . ?
C32B C31B H315 108.2 . . ?
P3B C31B H315 108.2 . . ?
H314 C31B H315 107.3 . . ?
F324 C32B F326 108.9(12) . . ?
F324 C32B F325 109.8(10) . . ?
F326 C32B F325 105.4(9) . . ?
F324 C32B C31B 113.2(9) . . ?
F326 C32B C31B 109.9(10) . . ?
F325 C32B C31B 109.3(11) . . ?
P3B O31 Co1 123.9(4) . . ?
P3A O31 Co1 113.44(18) . . ?
H11A N1A H12A 109.3 . . ?
H11A N1A H13A 116.4 . . ?
H12A N1A H13A 107(3) . . ?
H11A N1A H14A 112.4 . . ?
H12A N1A H14A 107(3) . . ?
H13A N1A H14A 104(4) . . ?
H11W O1W H12W 104(4) . . ?
H21W O2W H22W 109.1 . . ?
H31W O3W H32W 101.8 . . ?
H31V O3V H32V 95.8 . . ?
H41W O4W H41W 108(7) . 2_656 ?

_refine_diff_density_max         0.555
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.079

####################################################################### 
# 
# 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_cf3ch2ots
_database_code_depnum_ccdc_archive 'CCDC 2327151'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2024-01-20 deposited with the CCDC.	2024-03-26 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         'C9 H9 F3 O3 S'
_chemical_formula_sum            'C9 H9 F3 O3 S'
_chemical_formula_weight         254.22

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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                   8.2859(4)
_cell_length_b                   11.5440(6)
_cell_length_c                   11.0029(5)
_cell_angle_alpha                90
_cell_angle_beta                 93.944(2)
_cell_angle_gamma                90
_cell_volume                     1049.96(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9976
_cell_measurement_theta_min      2.4639
_cell_measurement_theta_max      27.4906

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_F_000             520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.136
_exptl_absorpt_coefficient_mu    0.340
_shelx_estimated_absorpt_T_min   0.931
_shelx_estimated_absorpt_T_max   0.955
_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  0.92
_exptl_absorpt_correction_T_max  0.95
_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       'Bruker D8 VENTURE'
_diffrn_measurement_device_type  'κ-geometry diffractometer'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            25026
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.464
_diffrn_reflns_theta_max         27.491
_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             2412
_reflns_number_gt                2356
_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    ?
_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)+(0.0324P)²+0.5803P] 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         2412
_refine_ls_number_parameters     170
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0748
_refine_ls_wR_factor_gt          0.0743
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.113
_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
S1 S 0.72410(3) 0.18280(3) 0.63996(3) 0.01673(10) Uani 1 1 d . . . . .
O1 O 0.72948(11) 0.32096(8) 0.65425(8) 0.01920(19) Uani 1 1 d . . . . .
O2 O 0.85940(11) 0.14878(8) 0.57487(9) 0.0230(2) Uani 1 1 d . . . . .
O3 O 0.70769(12) 0.14368(9) 0.76112(8) 0.0243(2) Uani 1 1 d . . . . .
C1 C 0.76786(17) 0.38408(11) 0.54744(12) 0.0231(3) Uani 1 1 d . . . . .
H11 H 0.6919 0.3632 0.4775 0.028 Uiso 1 1 calc R U . . .
H12 H 0.8793 0.3659 0.5263 0.028 Uiso 1 1 calc R U . . .
C2 C 0.75308(17) 0.51027(12) 0.57677(13) 0.0258(3) Uani 1 1 d . . . . .
F1 F 0.60504(11) 0.53934(9) 0.60611(9) 0.0389(2) Uani 1 1 d . . . . .
F2 F 0.85340(12) 0.54406(8) 0.66951(10) 0.0427(3) Uani 1 1 d . . . . .
F3 F 0.78620(15) 0.57263(8) 0.47965(10) 0.0490(3) Uani 1 1 d . . . . .
C3 C 0.54543(14) 0.15926(10) 0.54934(11) 0.0159(2) Uani 1 1 d . . . . .
C4 C 0.39863(15) 0.16319(11) 0.60375(11) 0.0189(2) Uani 1 1 d . . . . .
H41 H 0.3960 0.1736 0.6892 0.023 Uiso 1 1 calc R U . . .
C5 C 0.25667(15) 0.15157(11) 0.53079(12) 0.0212(3) Uani 1 1 d . . . . .
H51 H 0.1558 0.1538 0.5669 0.025 Uiso 1 1 calc R U . . .
C6 C 0.25933(15) 0.13663(11) 0.40497(12) 0.0205(3) Uani 1 1 d . . . . .
C7 C 0.40814(16) 0.12918(11) 0.35399(11) 0.0201(3) Uani 1 1 d . . . . .
H71 H 0.4112 0.1157 0.2690 0.024 Uiso 1 1 calc R U . . .
C8 C 0.55220(15) 0.14106(11) 0.42515(11) 0.0180(2) Uani 1 1 d . . . . .
H81 H 0.6533 0.1368 0.3895 0.022 Uiso 1 1 calc R U . . .
C9 C 0.10411(19) 0.12942(15) 0.32626(16) 0.0297(3) Uani 1 1 d . . . . .
H91 H 0.092(6) 0.199(4) 0.283(5) 0.032(15) Uiso 0.50(9) 1 d . . P A 1
H92 H 0.021(6) 0.116(5) 0.365(4) 0.034(14) Uiso 0.50(9) 1 d . . P A 1
H93 H 0.110(5) 0.065(5) 0.266(4) 0.031(14) Uiso 0.50(9) 1 d . . P A 1
H94 H 0.125(6) 0.116(6) 0.248(5) 0.051(16) Uiso 0.50(9) 1 d . . P A 2
H95 H 0.035(6) 0.204(4) 0.332(4) 0.028(15) Uiso 0.50(9) 1 d . . P A 2
H96 H 0.032(6) 0.071(5) 0.363(4) 0.035(15) Uiso 0.50(9) 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
S1 O3 1.4228(9) . ?
S1 O2 1.4264(9) . ?
S1 O1 1.6029(9) . ?
S1 C3 1.7483(12) . ?
O1 C1 1.4369(15) . ?
C1 C2 1.4989(19) . ?
C1 H11 0.9900 . ?
C1 H12 0.9900 . ?
C2 F2 1.3295(16) . ?
C2 F3 1.3325(17) . ?
C2 F1 1.3326(17) . ?
C3 C8 1.3875(16) . ?
C3 C4 1.3929(16) . ?
C4 C5 1.3843(18) . ?
C4 H41 0.9500 . ?
C5 C6 1.3967(18) . ?
C5 H51 0.9500 . ?
C6 C7 1.3920(18) . ?
C6 C9 1.5026(18) . ?
C7 C8 1.3886(17) . ?
C7 H71 0.9500 . ?
C8 H81 0.9500 . ?
C9 H91 0.93(5) . ?
C9 H92 0.85(5) . ?
C9 H93 1.01(5) . ?
C9 H94 0.90(6) . ?
C9 H95 1.04(5) . ?
C9 H96 1.01(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 S1 O2 120.80(6) . . ?
O3 S1 O1 103.17(5) . . ?
O2 S1 O1 107.80(5) . . ?
O3 S1 C3 110.69(6) . . ?
O2 S1 C3 109.56(6) . . ?
O1 S1 C3 103.14(5) . . ?
C1 O1 S1 115.50(8) . . ?
O1 C1 C2 106.91(10) . . ?
O1 C1 H11 110.3 . . ?
C2 C1 H11 110.3 . . ?
O1 C1 H12 110.3 . . ?
C2 C1 H12 110.3 . . ?
H11 C1 H12 108.6 . . ?
F2 C2 F3 107.74(12) . . ?
F2 C2 F1 106.11(12) . . ?
F3 C2 F1 107.58(12) . . ?
F2 C2 C1 113.22(12) . . ?
F3 C2 C1 109.15(12) . . ?
F1 C2 C1 112.77(12) . . ?
C8 C3 C4 121.59(11) . . ?
C8 C3 S1 119.68(9) . . ?
C4 C3 S1 118.69(9) . . ?
C5 C4 C3 118.69(11) . . ?
C5 C4 H41 120.7 . . ?
C3 C4 H41 120.7 . . ?
C4 C5 C6 121.06(11) . . ?
C4 C5 H51 119.5 . . ?
C6 C5 H51 119.5 . . ?
C7 C6 C5 118.81(11) . . ?
C7 C6 C9 120.74(13) . . ?
C5 C6 C9 120.45(13) . . ?
C8 C7 C6 121.17(11) . . ?
C8 C7 H71 119.4 . . ?
C6 C7 H71 119.4 . . ?
C3 C8 C7 118.61(11) . . ?
C3 C8 H81 120.7 . . ?
C7 C8 H81 120.7 . . ?
C6 C9 H91 108(2) . . ?
C6 C9 H92 114(3) . . ?
H91 C9 H92 110(4) . . ?
C6 C9 H93 110(2) . . ?
H91 C9 H93 108(3) . . ?
H92 C9 H93 106(4) . . ?
C6 C9 H94 110(3) . . ?
C6 C9 H95 112(2) . . ?
H94 C9 H95 110(4) . . ?
C6 C9 H96 108(3) . . ?
H94 C9 H96 115(4) . . ?
H95 C9 H96 101(3) . . ?

_refine_diff_density_max         0.346
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.044

####################################################################### 
# 
# 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_adafepa
_database_code_depnum_ccdc_archive 'CCDC 2327149'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2024-01-20 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H18 N, C2 H3 F3 O2 P'
_chemical_formula_sum            'C12 H21 F3 N O2 P'
_chemical_formula_weight         299.27

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'

_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                   12.9012(4)
_cell_length_b                   6.5370(2)
_cell_length_c                   17.6777(6)
_cell_angle_alpha                90
_cell_angle_beta                 110.4430(10)
_cell_angle_gamma                90
_cell_volume                     1396.96(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9953
_cell_measurement_theta_min      2.4592
_cell_measurement_theta_max      27.4676

_exptl_crystal_description       bar
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_F_000             632
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.079
_exptl_absorpt_coefficient_mu    0.229
_shelx_estimated_absorpt_T_min   0.941
_shelx_estimated_absorpt_T_max   0.982
_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  0.95
_exptl_absorpt_correction_T_max  0.98
_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_reflns_number            22433
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.448
_diffrn_reflns_theta_max         27.508
_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             3214
_reflns_number_gt                2816
_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 vV6.2.4'
_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-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_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)+(0.0452P)²+0.5652P] 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         3214
_refine_ls_number_parameters     188
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0873
_refine_ls_wR_factor_gt          0.0834
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_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
P1 P 0.47140(3) 0.68725(5) 0.40224(2) 0.01389(10) Uani 1 1 d . . . . .
O1P O 0.45790(8) 0.46029(14) 0.39471(5) 0.0192(2) Uani 1 1 d . . . . .
O2P O 0.45671(8) 0.80675(14) 0.32630(6) 0.0202(2) Uani 1 1 d . . . . .
H1P H 0.5678(13) 0.734(2) 0.4531(10) 0.021(4) Uiso 1 1 d . . . . .
C1P C 0.38322(11) 0.7953(2) 0.45355(8) 0.0181(3) Uani 1 1 d . . . . .
H11P H 0.419655 0.772105 0.512249 0.022 Uiso 1 1 calc R U . . .
H12P H 0.379154 0.945073 0.444644 0.022 Uiso 1 1 calc R U . . .
C2P C 0.26826(11) 0.7148(2) 0.42902(8) 0.0205(3) Uani 1 1 d . . . . .
F1P F 0.21372(7) 0.72249(14) 0.34885(5) 0.0293(2) Uani 1 1 d . . . . .
F2P F 0.26307(8) 0.51961(14) 0.45051(6) 0.0316(2) Uani 1 1 d . . . . .
F3P F 0.20661(8) 0.82237(16) 0.46279(7) 0.0396(3) Uani 1 1 d . . . . .
N1 N 0.40844(9) 0.20282(17) 0.26493(7) 0.0146(2) Uani 1 1 d . . . . .
H11 H 0.4264(15) 0.299(3) 0.3081(11) 0.029(5) Uiso 1 1 d . . . . .
H12 H 0.4222(14) 0.076(3) 0.2866(10) 0.022(4) Uiso 1 1 d . . . . .
H13 H 0.4508(14) 0.225(3) 0.2361(10) 0.022(4) Uiso 1 1 d . . . . .
C1 C 0.28932(10) 0.22254(18) 0.21168(7) 0.0133(2) Uani 1 1 d . . . . .
C2 C 0.27214(11) 0.43253(19) 0.17088(8) 0.0160(3) Uani 1 1 d . . . . .
H21 H 0.320131 0.446300 0.138018 0.019 Uiso 1 1 calc R U . . .
H22 H 0.292056 0.541729 0.212291 0.019 Uiso 1 1 calc R U . . .
C3 C 0.26072(11) 0.05307(19) 0.14807(8) 0.0169(3) Uani 1 1 d . . . . .
H31 H 0.273266 -0.082449 0.174751 0.020 Uiso 1 1 calc R U . . .
H32 H 0.308628 0.064125 0.115050 0.020 Uiso 1 1 calc R U . . .
C4 C 0.21696(11) 0.2025(2) 0.26374(8) 0.0193(3) Uani 1 1 d . . . . .
H41 H 0.236532 0.310453 0.305667 0.023 Uiso 1 1 calc R U . . .
H42 H 0.229402 0.067773 0.291009 0.023 Uiso 1 1 calc R U . . .
C5 C 0.15013(11) 0.4536(2) 0.11672(8) 0.0197(3) Uani 1 1 d . . . . .
H51 H 0.137964 0.590379 0.089677 0.024 Uiso 1 1 calc R U . . .
C6 C 0.07710(11) 0.4342(2) 0.16856(9) 0.0241(3) Uani 1 1 d . . . . .
H61 H -0.001608 0.450419 0.134236 0.029 Uiso 1 1 calc R U . . .
H62 H 0.096135 0.543194 0.210036 0.029 Uiso 1 1 calc R U . . .
C7 C 0.09489(12) 0.2237(2) 0.20958(9) 0.0233(3) Uani 1 1 d . . . . .
H71 H 0.046936 0.210942 0.243205 0.028 Uiso 1 1 calc R U . . .
C8 C 0.06530(12) 0.0549(2) 0.14539(9) 0.0250(3) Uani 1 1 d . . . . .
H81 H 0.076476 -0.080846 0.171833 0.030 Uiso 1 1 calc R U . . .
H82 H -0.013472 0.066989 0.110651 0.030 Uiso 1 1 calc R U . . .
C9 C 0.13865(11) 0.0748(2) 0.09391(8) 0.0198(3) Uani 1 1 d . . . . .
H91 H 0.119180 -0.035206 0.051949 0.024 Uiso 1 1 calc R U . . .
C10 C 0.12080(12) 0.2847(2) 0.05260(8) 0.0218(3) Uani 1 1 d . . . . .
H101 H 0.168002 0.297264 0.019100 0.026 Uiso 1 1 calc R U . . .
H102 H 0.042622 0.298849 0.016842 0.026 Uiso 1 1 calc 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
P1 O1P 1.4943(10) . ?
P1 O2P 1.5070(10) . ?
P1 C1P 1.8266(13) . ?
P1 H1P 1.292(16) . ?
C1P C2P 1.4884(19) . ?
C1P H11P 0.9900 . ?
C1P H12P 0.9900 . ?
C2P F2P 1.3398(16) . ?
C2P F1P 1.3451(16) . ?
C2P F3P 1.3471(16) . ?
N1 C1 1.5013(16) . ?
N1 H11 0.954(19) . ?
N1 H12 0.902(18) . ?
N1 H13 0.879(18) . ?
C1 C4 1.5283(18) . ?
C1 C3 1.5290(17) . ?
C1 C2 1.5303(16) . ?
C2 C5 1.5365(17) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 C9 1.5374(18) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
C4 C7 1.5370(19) . ?
C4 H41 0.9900 . ?
C4 H42 0.9900 . ?
C5 C6 1.532(2) . ?
C5 C10 1.5325(19) . ?
C5 H51 1.0000 . ?
C6 C7 1.535(2) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
C7 C8 1.532(2) . ?
C7 H71 1.0000 . ?
C8 C9 1.530(2) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 C10 1.5334(18) . ?
C9 H91 1.0000 . ?
C10 H101 0.9900 . ?
C10 H102 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1P P1 O2P 117.44(6) . . ?
O1P P1 C1P 110.78(6) . . ?
O2P P1 C1P 109.60(6) . . ?
O1P P1 H1P 110.6(7) . . ?
O2P P1 H1P 106.8(7) . . ?
C1P P1 H1P 100.2(7) . . ?
C2P C1P P1 116.66(9) . . ?
C2P C1P H11P 108.1 . . ?
P1 C1P H11P 108.1 . . ?
C2P C1P H12P 108.1 . . ?
P1 C1P H12P 108.1 . . ?
H11P C1P H12P 107.3 . . ?
F2P C2P F1P 105.94(11) . . ?
F2P C2P F3P 106.00(11) . . ?
F1P C2P F3P 105.96(11) . . ?
F2P C2P C1P 113.42(11) . . ?
F1P C2P C1P 113.27(11) . . ?
F3P C2P C1P 111.65(12) . . ?
C1 N1 H11 110.8(11) . . ?
C1 N1 H12 110.6(11) . . ?
H11 N1 H12 108.0(15) . . ?
C1 N1 H13 109.2(11) . . ?
H11 N1 H13 109.2(15) . . ?
H12 N1 H13 109.0(15) . . ?
N1 C1 C4 108.78(10) . . ?
N1 C1 C3 109.28(10) . . ?
C4 C1 C3 109.85(10) . . ?
N1 C1 C2 108.69(10) . . ?
C4 C1 C2 110.01(10) . . ?
C3 C1 C2 110.20(10) . . ?
C1 C2 C5 108.80(10) . . ?
C1 C2 H21 109.9 . . ?
C5 C2 H21 109.9 . . ?
C1 C2 H22 109.9 . . ?
C5 C2 H22 109.9 . . ?
H21 C2 H22 108.3 . . ?
C1 C3 C9 108.83(10) . . ?
C1 C3 H31 109.9 . . ?
C9 C3 H31 109.9 . . ?
C1 C3 H32 109.9 . . ?
C9 C3 H32 109.9 . . ?
H31 C3 H32 108.3 . . ?
C1 C4 C7 109.00(11) . . ?
C1 C4 H41 109.9 . . ?
C7 C4 H41 109.9 . . ?
C1 C4 H42 109.9 . . ?
C7 C4 H42 109.9 . . ?
H41 C4 H42 108.3 . . ?
C6 C5 C10 109.76(11) . . ?
C6 C5 C2 109.28(11) . . ?
C10 C5 C2 109.31(11) . . ?
C6 C5 H51 109.5 . . ?
C10 C5 H51 109.5 . . ?
C2 C5 H51 109.5 . . ?
C5 C6 C7 109.59(11) . . ?
C5 C6 H61 109.8 . . ?
C7 C6 H61 109.8 . . ?
C5 C6 H62 109.8 . . ?
C7 C6 H62 109.8 . . ?
H61 C6 H62 108.2 . . ?
C8 C7 C6 109.76(12) . . ?
C8 C7 C4 109.42(11) . . ?
C6 C7 C4 109.07(11) . . ?
C8 C7 H71 109.5 . . ?
C6 C7 H71 109.5 . . ?
C4 C7 H71 109.5 . . ?
C9 C8 C7 109.48(11) . . ?
C9 C8 H81 109.8 . . ?
C7 C8 H81 109.8 . . ?
C9 C8 H82 109.8 . . ?
C7 C8 H82 109.8 . . ?
H81 C8 H82 108.2 . . ?
C8 C9 C10 109.74(11) . . ?
C8 C9 C3 109.48(11) . . ?
C10 C9 C3 109.26(11) . . ?
C8 C9 H91 109.4 . . ?
C10 C9 H91 109.4 . . ?
C3 C9 H91 109.4 . . ?
C5 C10 C9 109.60(11) . . ?
C5 C10 H101 109.8 . . ?
C9 C10 H101 109.8 . . ?
C5 C10 H102 109.8 . . ?
C9 C10 H102 109.8 . . ?
H101 C10 H102 108.2 . . ?

_refine_diff_density_max         0.326
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.053

####################################################################### 
# 
# 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_mnnotpf
_database_code_depnum_ccdc_archive 'CCDC 2327152'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2024-01-20 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C15 H24 F9 Mn N3 O6 P3, 2(Cl), 3(H2 O), 3(H4 N)'
_chemical_formula_sum            'C15 H42 Cl2 F9 Mn N6 O9 P3'
_chemical_formula_weight         840.29

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'
Mn Mn 0.3368 0.7283 '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                   16.6902(5)
_cell_length_b                   11.6001(4)
_cell_length_c                   17.4365(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.0700(10)
_cell_angle_gamma                90
_cell_volume                     3373.64(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9549
_cell_measurement_theta_min      2.3376
_cell_measurement_theta_max      27.5088

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_F_000             1724
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.792
_shelx_estimated_absorpt_T_min   0.821
_shelx_estimated_absorpt_T_max   0.911
_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  0.87
_exptl_absorpt_correction_T_max  0.91
_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            52478
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.109
_diffrn_reflns_theta_max         27.509
_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             7735
_reflns_number_gt                7231
_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-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_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)+(0.0384P)²+3.8790P] 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         7735
_refine_ls_number_parameters     470
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0823
_refine_ls_wR_factor_gt          0.0808
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_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
Mn1 Mn 0.24765(2) 0.26370(2) 0.45992(2) 0.01235(7) Uani 1 1 d . . . . .
N1 N 0.18747(8) 0.44380(12) 0.48324(8) 0.0150(3) Uani 1 1 d . . . . .
C2 C 0.25050(10) 0.52740(15) 0.46258(10) 0.0170(3) Uani 1 1 d . . . . .
H21 H 0.231472 0.606606 0.472677 0.020 Uiso 1 1 calc R U . . .
H22 H 0.259976 0.521025 0.407016 0.020 Uiso 1 1 calc R U . . .
C3 C 0.32903(10) 0.50701(15) 0.50761(10) 0.0171(3) Uani 1 1 d . . . . .
H31 H 0.370664 0.559436 0.488534 0.021 Uiso 1 1 calc R U . . .
H32 H 0.321751 0.524652 0.562473 0.021 Uiso 1 1 calc R U . . .
N4 N 0.35599(8) 0.38531(12) 0.49973(8) 0.0145(3) Uani 1 1 d . . . . .
C5 C 0.38241(10) 0.33375(15) 0.57457(9) 0.0170(3) Uani 1 1 d . . . . .
H51 H 0.426310 0.380926 0.597893 0.020 Uiso 1 1 calc R U . . .
H52 H 0.403650 0.255356 0.565758 0.020 Uiso 1 1 calc R U . . .
C6 C 0.31402(10) 0.32669(16) 0.62996(9) 0.0180(3) Uani 1 1 d . . . . .
H61 H 0.332001 0.282772 0.676124 0.022 Uiso 1 1 calc R U . . .
H62 H 0.299526 0.405407 0.646447 0.022 Uiso 1 1 calc R U . . .
N7 N 0.24204(9) 0.26956(13) 0.59379(8) 0.0159(3) Uani 1 1 d . . . . .
C8 C 0.16748(10) 0.33630(16) 0.60640(10) 0.0184(3) Uani 1 1 d . . . . .
H81 H 0.162190 0.348736 0.662163 0.022 Uiso 1 1 calc R U . . .
H82 H 0.120712 0.290508 0.587640 0.022 Uiso 1 1 calc R U . . .
C9 C 0.16629(10) 0.45340(15) 0.56569(9) 0.0177(3) Uani 1 1 d . . . . .
H91 H 0.112163 0.487644 0.568680 0.021 Uiso 1 1 calc R U . . .
H92 H 0.204803 0.505803 0.592539 0.021 Uiso 1 1 calc R U . . .
C10 C 0.11522(10) 0.45958(15) 0.43195(9) 0.0165(3) Uani 1 1 d . . . . .
H101 H 0.106152 0.542877 0.422817 0.020 Uiso 1 1 calc R U . . .
H102 H 0.067698 0.428231 0.457178 0.020 Uiso 1 1 calc R U . . .
P1 P 0.12720(2) 0.38631(4) 0.34001(2) 0.01454(9) Uani 1 1 d . . . . .
O11 O 0.17105(8) 0.27544(11) 0.36036(7) 0.0213(3) Uani 1 1 d . . . . .
O12 O 0.16371(8) 0.46100(12) 0.28011(7) 0.0216(3) Uani 1 1 d . . . . .
C11 C 0.02598(10) 0.34608(15) 0.30822(10) 0.0177(3) Uani 1 1 d . . . . .
H111 H 0.029315 0.280270 0.272328 0.021 Uiso 1 1 calc R U . . .
H112 H -0.003277 0.319366 0.353297 0.021 Uiso 1 1 calc R U . . .
C12 C -0.02159(11) 0.44001(17) 0.26950(11) 0.0215(4) Uani 1 1 d . . . . .
F121 F -0.01993(7) 0.53888(10) 0.31079(7) 0.0269(2) Uani 1 1 d . . . . .
F122 F 0.00493(7) 0.46687(11) 0.20017(6) 0.0300(3) Uani 1 1 d . . . . .
F123 F -0.09945(7) 0.41215(12) 0.25943(8) 0.0377(3) Uani 1 1 d . . . . .
C20 C 0.42108(10) 0.37907(15) 0.44459(10) 0.0163(3) Uani 1 1 d . . . . .
H201 H 0.472875 0.396504 0.471565 0.020 Uiso 1 1 calc R U . . .
H202 H 0.411852 0.437941 0.404124 0.020 Uiso 1 1 calc R U . . .
P2 P 0.42638(2) 0.23735(4) 0.40046(2) 0.01365(9) Uani 1 1 d . . . . .
O21 O 0.33978(7) 0.19720(10) 0.38966(7) 0.0164(2) Uani 1 1 d . . . . .
O22 O 0.48188(8) 0.15836(11) 0.44494(7) 0.0205(3) Uani 1 1 d . . . . .
C21 C 0.46215(10) 0.26346(16) 0.30471(10) 0.0182(3) Uani 1 1 d . . . . .
H211 H 0.449847 0.194845 0.272636 0.022 Uiso 1 1 calc R U . . .
H212 H 0.431850 0.329195 0.281952 0.022 Uiso 1 1 calc R U . . .
C22 C 0.54980(11) 0.28888(18) 0.30087(11) 0.0246(4) Uani 1 1 d . . . . .
F221 F 0.57409(7) 0.37007(12) 0.35184(8) 0.0352(3) Uani 1 1 d . . . . .
F222 F 0.59572(7) 0.19624(12) 0.31462(8) 0.0363(3) Uani 1 1 d . . . . .
F223 F 0.56866(8) 0.32848(14) 0.23159(7) 0.0424(3) Uani 1 1 d . . . . .
C30 C 0.23522(11) 0.15021(15) 0.62340(9) 0.0179(3) Uani 1 1 d . . . . .
H301 H 0.209309 0.151741 0.673571 0.022 Uiso 1 1 calc R U . . .
H302 H 0.289489 0.116876 0.631390 0.022 Uiso 1 1 calc R U . . .
P3 P 0.17639(3) 0.05950(4) 0.55647(2) 0.01641(9) Uani 1 1 d . . . . .
O31 O 0.20193(8) 0.09585(11) 0.47722(7) 0.0185(2) Uani 1 1 d . . . . .
O32 O 0.08806(8) 0.06409(12) 0.56907(8) 0.0241(3) Uani 1 1 d . . . . .
C31 C 0.21390(11) -0.08646(16) 0.57134(10) 0.0206(3) Uani 1 1 d . . . . .
H311 H 0.188965 -0.136388 0.531089 0.025 Uiso 1 1 calc R U . . .
H312 H 0.272345 -0.085889 0.563473 0.025 Uiso 1 1 calc R U . . .
C32 C 0.20018(12) -0.14061(18) 0.64736(11) 0.0252(4) Uani 1 1 d . . . . .
F321 F 0.23753(9) -0.08334(12) 0.70517(7) 0.0376(3) Uani 1 1 d . . . . .
F322 F 0.12255(8) -0.14630(13) 0.66482(8) 0.0428(4) Uani 1 1 d . . . . .
F323 F 0.22797(9) -0.24919(11) 0.65139(9) 0.0401(3) Uani 1 1 d . . . . .
N1A N 0.24636(11) 0.66455(15) 0.26516(9) 0.0214(3) Uani 1 1 d . . . . .
H11A H 0.2203(18) 0.599(3) 0.2670(17) 0.046(8) Uiso 1 1 d . . . . .
H12A H 0.2231(16) 0.714(2) 0.2984(15) 0.033(7) Uiso 1 1 d . . . . .
H13A H 0.298(2) 0.651(3) 0.2776(17) 0.051(8) Uiso 1 1 d . . . . .
H14A H 0.2426(19) 0.689(3) 0.216(2) 0.054(9) Uiso 1 1 d . . . . .
N2A N 0.68628(9) 0.05181(13) 0.61782(9) 0.0151(3) Uani 1 1 d . . . . .
H21A H 0.656319 0.102546 0.596588 0.018 Uiso 1 1 d R U . . .
H22A H 0.681579 -0.018101 0.602580 0.018 Uiso 1 1 d R U . . .
H23A H 0.7303(17) 0.075(2) 0.6141(15) 0.034(7) Uiso 1 1 d . . . . .
H24A H 0.6769(16) 0.051(2) 0.6634(16) 0.032(7) Uiso 1 1 d . . . . .
N3A N -0.04721(11) -0.03973(16) 0.62495(10) 0.0225(3) Uani 1 1 d . . . . .
H31A H 0.000(2) -0.023(3) 0.6101(17) 0.048(8) Uiso 1 1 d . . . . .
H32A H -0.0450(16) -0.056(2) 0.6733(17) 0.033(7) Uiso 1 1 d . . . . .
H33A H -0.079(2) 0.022(3) 0.6182(19) 0.062(10) Uiso 1 1 d . . . . .
H34A H -0.062(2) -0.089(3) 0.597(2) 0.072(12) Uiso 1 1 d . . . . .
Cl1 Cl 0.14587(2) 0.80280(4) 0.38571(2) 0.01909(9) Uani 1 1 d . . . . .
Cl2 Cl 0.42842(2) 0.59874(3) 0.30424(2) 0.01608(9) Uani 1 1 d . . . . .
O1W O 0.59645(9) 0.22912(13) 0.55500(9) 0.0292(3) Uani 1 1 d . . . . .
H11W H 0.557(2) 0.211(3) 0.524(2) 0.060(10) Uiso 1 1 d . . . . .
H12W H 0.578(2) 0.274(3) 0.592(2) 0.062(10) Uiso 1 1 d . . . . .
O2W O 0.39543(9) 0.01520(14) 0.54500(9) 0.0273(3) Uani 1 1 d . . . . .
H21W H 0.4217(18) 0.060(3) 0.5141(18) 0.046(8) Uiso 1 1 d . . . . .
H22W H 0.4266(19) -0.035(3) 0.5611(18) 0.050(9) Uiso 1 1 d . . . . .
O3W O -0.00276(11) 0.23411(15) 0.49261(9) 0.0323(3) Uani 1 1 d . . . . .
H31W H 0.0274(18) 0.184(3) 0.5197(17) 0.041(8) Uiso 1 1 d . . . . .
H32W H -0.045(2) 0.240(3) 0.5180(19) 0.052(9) 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
Mn1 O31 2.1168(12) . ?
Mn1 O11 2.1228(12) . ?
Mn1 O21 2.1438(12) . ?
Mn1 N7 2.3406(14) . ?
Mn1 N1 2.3599(14) . ?
Mn1 N4 2.3771(14) . ?
N1 C2 1.485(2) . ?
N1 C10 1.486(2) . ?
N1 C9 1.497(2) . ?
C2 C3 1.522(2) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.490(2) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C20 1.478(2) . ?
N4 C5 1.488(2) . ?
C5 C6 1.524(2) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.492(2) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C30 1.483(2) . ?
N7 C8 1.489(2) . ?
C8 C9 1.532(2) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
C10 P1 1.8318(17) . ?
C10 H101 0.9900 . ?
C10 H102 0.9900 . ?
P1 O12 1.5028(13) . ?
P1 O11 1.5155(13) . ?
P1 C11 1.8197(17) . ?
C11 C12 1.495(2) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 F122 1.339(2) . ?
C12 F123 1.345(2) . ?
C12 F121 1.354(2) . ?
C20 P2 1.8187(17) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P2 O22 1.4991(13) . ?
P2 O21 1.5238(12) . ?
P2 C21 1.8186(18) . ?
C21 C22 1.496(2) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
C22 F222 1.337(2) . ?
C22 F223 1.340(2) . ?
C22 F221 1.347(2) . ?
C30 P3 1.8304(18) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
P3 O32 1.4993(13) . ?
P3 O31 1.5204(12) . ?
P3 C31 1.8205(18) . ?
C31 C32 1.492(2) . ?
C31 H311 0.9900 . ?
C31 H312 0.9900 . ?
C32 F321 1.342(2) . ?
C32 F323 1.343(2) . ?
C32 F322 1.343(2) . ?
N1A H11A 0.88(3) . ?
N1A H12A 0.91(3) . ?
N1A H13A 0.90(3) . ?
N1A H14A 0.90(3) . ?
N2A H21A 0.8486 . ?
N2A H22A 0.8562 . ?
N2A H23A 0.79(3) . ?
N2A H24A 0.82(3) . ?
N3A H31A 0.85(3) . ?
N3A H32A 0.86(3) . ?
N3A H33A 0.90(4) . ?
N3A H34A 0.79(4) . ?
O1W H11W 0.86(4) . ?
O1W H12W 0.89(4) . ?
O2W H21W 0.87(3) . ?
O2W H22W 0.82(3) . ?
O3W H31W 0.89(3) . ?
O3W H32W 0.85(4) . ?

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
O31 Mn1 O11 88.05(5) . . ?
O31 Mn1 O21 91.16(5) . . ?
O11 Mn1 O21 88.80(5) . . ?
O31 Mn1 N7 81.78(5) . . ?
O11 Mn1 N7 140.27(5) . . ?
O21 Mn1 N7 129.48(5) . . ?
O31 Mn1 N1 129.19(5) . . ?
O11 Mn1 N1 80.59(5) . . ?
O21 Mn1 N1 137.35(5) . . ?
N7 Mn1 N1 76.69(5) . . ?
O31 Mn1 N4 141.13(5) . . ?
O11 Mn1 N4 129.05(5) . . ?
O21 Mn1 N4 80.02(5) . . ?
N7 Mn1 N4 75.46(5) . . ?
N1 Mn1 N4 75.42(5) . . ?
C2 N1 C10 109.88(13) . . ?
C2 N1 C9 112.24(13) . . ?
C10 N1 C9 110.74(13) . . ?
C2 N1 Mn1 103.10(10) . . ?
C10 N1 Mn1 110.27(10) . . ?
C9 N1 Mn1 110.37(10) . . ?
N1 C2 C3 112.20(14) . . ?
N1 C2 H21 109.2 . . ?
C3 C2 H21 109.2 . . ?
N1 C2 H22 109.2 . . ?
C3 C2 H22 109.2 . . ?
H21 C2 H22 107.9 . . ?
N4 C3 C2 110.92(13) . . ?
N4 C3 H31 109.5 . . ?
C2 C3 H31 109.5 . . ?
N4 C3 H32 109.5 . . ?
C2 C3 H32 109.5 . . ?
H31 C3 H32 108.0 . . ?
C20 N4 C5 110.44(13) . . ?
C20 N4 C3 109.76(13) . . ?
C5 N4 C3 112.40(13) . . ?
C20 N4 Mn1 110.50(10) . . ?
C5 N4 Mn1 102.46(10) . . ?
C3 N4 Mn1 111.12(10) . . ?
N4 C5 C6 111.86(13) . . ?
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 . . ?
N7 C6 C5 111.48(13) . . ?
N7 C6 H61 109.3 . . ?
C5 C6 H61 109.3 . . ?
N7 C6 H62 109.3 . . ?
C5 C6 H62 109.3 . . ?
H61 C6 H62 108.0 . . ?
C30 N7 C8 111.03(13) . . ?
C30 N7 C6 109.77(13) . . ?
C8 N7 C6 111.80(13) . . ?
C30 N7 Mn1 109.04(10) . . ?
C8 N7 Mn1 103.07(10) . . ?
C6 N7 Mn1 111.96(10) . . ?
N7 C8 C9 112.92(14) . . ?
N7 C8 H81 109.0 . . ?
C9 C8 H81 109.0 . . ?
N7 C8 H82 109.0 . . ?
C9 C8 H82 109.0 . . ?
H81 C8 H82 107.8 . . ?
N1 C9 C8 112.30(14) . . ?
N1 C9 H91 109.1 . . ?
C8 C9 H91 109.1 . . ?
N1 C9 H92 109.1 . . ?
C8 C9 H92 109.1 . . ?
H91 C9 H92 107.9 . . ?
N1 C10 P1 110.95(11) . . ?
N1 C10 H101 109.4 . . ?
P1 C10 H101 109.4 . . ?
N1 C10 H102 109.4 . . ?
P1 C10 H102 109.4 . . ?
H101 C10 H102 108.0 . . ?
O12 P1 O11 116.58(8) . . ?
O12 P1 C11 109.35(8) . . ?
O11 P1 C11 106.79(8) . . ?
O12 P1 C10 113.61(8) . . ?
O11 P1 C10 104.83(7) . . ?
C11 P1 C10 104.84(8) . . ?
P1 O11 Mn1 121.16(7) . . ?
C12 C11 P1 115.01(13) . . ?
C12 C11 H111 108.5 . . ?
P1 C11 H111 108.5 . . ?
C12 C11 H112 108.5 . . ?
P1 C11 H112 108.5 . . ?
H111 C11 H112 107.5 . . ?
F122 C12 F123 106.71(15) . . ?
F122 C12 F121 106.37(15) . . ?
F123 C12 F121 105.91(15) . . ?
F122 C12 C11 112.95(15) . . ?
F123 C12 C11 112.27(16) . . ?
F121 C12 C11 112.15(15) . . ?
N4 C20 P2 111.57(11) . . ?
N4 C20 H201 109.3 . . ?
P2 C20 H201 109.3 . . ?
N4 C20 H202 109.3 . . ?
P2 C20 H202 109.3 . . ?
H201 C20 H202 108.0 . . ?
O22 P2 O21 116.28(7) . . ?
O22 P2 C21 111.08(8) . . ?
O21 P2 C21 106.19(8) . . ?
O22 P2 C20 111.85(8) . . ?
O21 P2 C20 105.55(7) . . ?
C21 P2 C20 105.10(8) . . ?
P2 O21 Mn1 121.07(7) . . ?
C22 C21 P2 115.33(13) . . ?
C22 C21 H211 108.4 . . ?
P2 C21 H211 108.4 . . ?
C22 C21 H212 108.4 . . ?
P2 C21 H212 108.4 . . ?
H211 C21 H212 107.5 . . ?
F222 C22 F223 106.58(16) . . ?
F222 C22 F221 106.66(16) . . ?
F223 C22 F221 106.26(16) . . ?
F222 C22 C21 112.88(17) . . ?
F223 C22 C21 111.70(16) . . ?
F221 C22 C21 112.31(15) . . ?
N7 C30 P3 111.15(11) . . ?
N7 C30 H301 109.4 . . ?
P3 C30 H301 109.4 . . ?
N7 C30 H302 109.4 . . ?
P3 C30 H302 109.4 . . ?
H301 C30 H302 108.0 . . ?
O32 P3 O31 115.65(8) . . ?
O32 P3 C31 110.31(8) . . ?
O31 P3 C31 106.32(8) . . ?
O32 P3 C30 113.20(8) . . ?
O31 P3 C30 104.97(8) . . ?
C31 P3 C30 105.67(8) . . ?
P3 O31 Mn1 119.93(7) . . ?
C32 C31 P3 117.07(14) . . ?
C32 C31 H311 108.0 . . ?
P3 C31 H311 108.0 . . ?
C32 C31 H312 108.0 . . ?
P3 C31 H312 108.0 . . ?
H311 C31 H312 107.3 . . ?
F321 C32 F323 105.95(16) . . ?
F321 C32 F322 106.25(17) . . ?
F323 C32 F322 106.03(16) . . ?
F321 C32 C31 112.14(16) . . ?
F323 C32 C31 112.18(17) . . ?
F322 C32 C31 113.72(16) . . ?
H11A N1A H12A 108(2) . . ?
H11A N1A H13A 108(3) . . ?
H12A N1A H13A 113(3) . . ?
H11A N1A H14A 107(3) . . ?
H12A N1A H14A 113(3) . . ?
H13A N1A H14A 109(3) . . ?
H21A N2A H22A 118.4 . . ?
H21A N2A H23A 105.5 . . ?
H22A N2A H23A 111.8 . . ?
H21A N2A H24A 107.4 . . ?
H22A N2A H24A 106.0 . . ?
H23A N2A H24A 107(3) . . ?
H31A N3A H32A 110(3) . . ?
H31A N3A H33A 109(3) . . ?
H32A N3A H33A 108(3) . . ?
H31A N3A H34A 105(3) . . ?
H32A N3A H34A 116(3) . . ?
H33A N3A H34A 109(3) . . ?
H11W O1W H12W 108(3) . . ?
H21W O2W H22W 108(3) . . ?
H31W O3W H32W 104(3) . . ?

_refine_diff_density_max         1.088
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.066

####################################################################### 
# 
# 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_znnotptfe
_database_code_depnum_ccdc_archive 'CCDC 2327150'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2024-01-20 deposited with the CCDC.	2024-03-26 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         'C15 H24 F9 N3 O6 P3 Zn, Cl H6 O3 Zn, 2(H2 O)'
_chemical_formula_sum            'C15 H34 Cl F9 N3 O11 P3 Zn2'
_chemical_formula_weight         862.55

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'
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      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_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'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   14.7089(2)
_cell_length_b                   14.7089(2)
_cell_length_c                   14.7089(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3182.30(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9788
_cell_measurement_theta_min      2.3983
_cell_measurement_theta_max      27.4069

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_F_000             1744
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.228
_exptl_absorpt_coefficient_mu    1.848
_shelx_estimated_absorpt_T_min   0.535
_shelx_estimated_absorpt_T_max   0.678
_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  0.57
_exptl_absorpt_correction_T_max  0.68
_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            21053
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.398
_diffrn_reflns_theta_max         27.448
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2426
_reflns_number_gt                2380
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.999

_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    ?
_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)+(0.0325P)²+2.8899P] 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_abs_structure_details 
;
 Flack x determined using 1041 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(3)
_chemical_absolute_configuration .
_refine_ls_number_reflns         2426
_refine_ls_number_parameters     147
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0678
_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
Zn1 Zn 0.70758(3) 0.79242(3) 0.20758(3) 0.02775(16) Uani 1 3 d S T P . .
N1 N 0.6884(2) 0.7435(3) 0.3469(2) 0.0412(8) Uani 1 1 d . . . . .
C2 C 0.7586(3) 0.7986(4) 0.3981(3) 0.0496(11) Uani 1 1 d . . . . .
H21 H 0.7385 0.8627 0.4009 0.060 Uiso 1 1 calc R U . . .
H22 H 0.7631 0.7755 0.4611 0.060 Uiso 1 1 calc R U . . .
C3 C 0.8497(3) 0.7943(4) 0.3548(3) 0.0528(12) Uani 1 1 d . . . . .
H31 H 0.8899 0.8398 0.3839 0.063 Uiso 1 1 calc R U . . .
H32 H 0.8763 0.7335 0.3656 0.063 Uiso 1 1 calc R U . . .
C4 C 0.5957(3) 0.7670(3) 0.3769(3) 0.0420(10) Uani 1 1 d . . . . .
H41 H 0.5947 0.8305 0.3993 0.050 Uiso 1 1 calc R U . . .
H42 H 0.5776 0.7267 0.4277 0.050 Uiso 1 1 calc R U . . .
P1 P 0.51515(7) 0.75471(6) 0.28357(7) 0.0327(2) Uani 1 1 d . . . . .
O11 O 0.56845(18) 0.77777(19) 0.19810(18) 0.0353(6) Uani 1 1 d . . . . .
O12 O 0.4686(2) 0.6647(2) 0.2828(2) 0.0481(7) Uani 1 1 d . . . . .
C5 C 0.4313(3) 0.8445(3) 0.2974(4) 0.0515(12) Uani 1 1 d . . . . .
H51 H 0.4638 0.9032 0.3022 0.062 Uiso 1 1 calc R U . . .
H52 H 0.3936 0.8469 0.2416 0.062 Uiso 1 1 calc R U . . .
C6 C 0.3692(3) 0.8355(3) 0.3776(4) 0.0526(11) Uani 1 1 d . . . . .
F61 F 0.4147(2) 0.8233(3) 0.4555(2) 0.0684(9) Uani 1 1 d . . . . .
F62 F 0.3116(2) 0.7666(2) 0.3703(2) 0.0690(9) Uani 1 1 d . . . . .
F63 F 0.3165(3) 0.9085(3) 0.3872(3) 0.0885(14) Uani 1 1 d . . . . .
Zn2 Zn 0.46969(3) 0.46969(3) 0.46969(3) 0.02850(16) Uani 1 3 d S T P . .
Cl1 Cl 0.55520(6) 0.55520(6) 0.55520(6) 0.0369(3) Uani 1 3 d S T P . .
O1W O 0.45983(19) 0.50074(17) 0.33879(17) 0.0340(6) Uani 1 1 d . . . . .
H11W H 0.4586 0.5613 0.3285 0.09(2) Uiso 1 1 d R . . . .
H12W H 0.4078 0.4782 0.3173 0.10(2) Uiso 1 1 d R . . . .
O2W O 0.5225(8) 0.5629(9) 0.1228(8) 0.066(3) Uani 0.3333 1 d . . P A 1
H21W H 0.5802 0.5498 0.1005 0.080 Uiso 0.3333 1 d R U P A 1
H22W H 0.4924 0.5692 0.1763 0.080 Uiso 0.3333 1 d R U P A 1
O2V O 0.4693(9) 0.6375(9) 0.0762(8) 0.070(3) Uani 0.3333 1 d . . P B 2
H21V H 0.4145 0.6323 0.1048 0.084 Uiso 0.3333 1 d R U P B 2
H22V H 0.4724 0.5863 0.0434 0.084 Uiso 0.3333 1 d R U P B 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 O11 2.062(3) 6_566 ?
Zn1 O11 2.062(3) 12_664 ?
Zn1 O11 2.062(3) . ?
Zn1 N1 2.191(3) 12_664 ?
Zn1 N1 2.191(3) 6_566 ?
Zn1 N1 2.191(3) . ?
N1 C3 1.468(6) 12_664 ?
N1 C4 1.475(5) . ?
N1 C2 1.513(6) . ?
C2 C3 1.484(7) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N1 1.468(6) 6_566 ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
C4 P1 1.823(4) . ?
C4 H41 0.9900 . ?
C4 H42 0.9900 . ?
P1 O12 1.491(3) . ?
P1 O11 1.520(3) . ?
P1 C5 1.818(4) . ?
C5 C6 1.497(7) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 F62 1.326(6) . ?
C6 F63 1.332(6) . ?
C6 F61 1.339(6) . ?
Zn2 O1W 1.984(3) 9 ?
Zn2 O1W 1.984(3) 5 ?
Zn2 O1W 1.984(3) . ?
Zn2 Cl1 2.1785(17) . ?
O1W H11W 0.9036 . ?
O1W H12W 0.8925 . ?
O2W H21W 0.9306 . ?
O2W H22W 0.9072 . ?
O2V H21V 0.9124 . ?
O2V H22V 0.8947 . ?

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 Zn1 O11 92.51(10) 6_566 12_664 ?
O11 Zn1 O11 92.51(10) 6_566 . ?
O11 Zn1 O11 92.50(10) 12_664 . ?
O11 Zn1 N1 164.57(13) 6_566 12_664 ?
O11 Zn1 N1 84.33(12) 12_664 12_664 ?
O11 Zn1 N1 102.70(13) . 12_664 ?
O11 Zn1 N1 84.33(12) 6_566 6_566 ?
O11 Zn1 N1 102.70(13) 12_664 6_566 ?
O11 Zn1 N1 164.57(13) . 6_566 ?
N1 Zn1 N1 81.67(14) 12_664 6_566 ?
O11 Zn1 N1 102.70(13) 6_566 . ?
O11 Zn1 N1 164.57(13) 12_664 . ?
O11 Zn1 N1 84.33(12) . . ?
N1 Zn1 N1 81.67(14) 12_664 . ?
N1 Zn1 N1 81.67(14) 6_566 . ?
C3 N1 C4 112.5(4) 12_664 . ?
C3 N1 C2 113.3(4) 12_664 . ?
C4 N1 C2 110.9(4) . . ?
C3 N1 Zn1 109.1(3) 12_664 . ?
C4 N1 Zn1 108.8(2) . . ?
C2 N1 Zn1 101.6(3) . . ?
C3 C2 N1 112.4(4) . . ?
C3 C2 H21 109.1 . . ?
N1 C2 H21 109.1 . . ?
C3 C2 H22 109.1 . . ?
N1 C2 H22 109.1 . . ?
H21 C2 H22 107.9 . . ?
N1 C3 C2 112.9(4) 6_566 . ?
N1 C3 H31 109.0 6_566 . ?
C2 C3 H31 109.0 . . ?
N1 C3 H32 109.0 6_566 . ?
C2 C3 H32 109.0 . . ?
H31 C3 H32 107.8 . . ?
N1 C4 P1 110.6(3) . . ?
N1 C4 H41 109.5 . . ?
P1 C4 H41 109.5 . . ?
N1 C4 H42 109.5 . . ?
P1 C4 H42 109.5 . . ?
H41 C4 H42 108.1 . . ?
O12 P1 O11 115.41(19) . . ?
O12 P1 C5 109.5(2) . . ?
O11 P1 C5 106.26(18) . . ?
O12 P1 C4 113.08(19) . . ?
O11 P1 C4 105.42(17) . . ?
C5 P1 C4 106.6(3) . . ?
P1 O11 Zn1 118.63(15) . . ?
C6 C5 P1 115.9(3) . . ?
C6 C5 H51 108.3 . . ?
P1 C5 H51 108.3 . . ?
C6 C5 H52 108.3 . . ?
P1 C5 H52 108.3 . . ?
H51 C5 H52 107.4 . . ?
F62 C6 F63 104.6(4) . . ?
F62 C6 F61 106.6(4) . . ?
F63 C6 F61 107.9(5) . . ?
F62 C6 C5 113.2(5) . . ?
F63 C6 C5 111.6(4) . . ?
F61 C6 C5 112.4(4) . . ?
O1W Zn2 O1W 99.75(10) 9 5 ?
O1W Zn2 O1W 99.75(10) 9 . ?
O1W Zn2 O1W 99.75(10) 5 . ?
O1W Zn2 Cl1 118.00(8) 9 . ?
O1W Zn2 Cl1 118.00(8) 5 . ?
O1W Zn2 Cl1 118.00(8) . . ?
Zn2 O1W H11W 113.0 . . ?
Zn2 O1W H12W 108.7 . . ?
H11W O1W H12W 106.8 . . ?
H21W O2W H22W 140.4 . . ?
H21V O2V H22V 103.0 . . ?

_refine_diff_density_max         0.481
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.053

####################################################################### 
# 
# 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_ninotpf_mg
_database_code_depnum_ccdc_archive 'CCDC 2327155'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2024-01-20 deposited with the CCDC.	2024-03-26 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         
;
2(C15 H24 F9 N3 Ni O6 P3), H12 Mg O6, 12(H2 O)
;
_chemical_formula_sum            'C30 H84 F18 Mg N6 Ni2 O30 P6'
_chemical_formula_weight         1678.58

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'
Mg Mg 0.0486 0.0363 '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'
Ni Ni 0.3393 1.1124 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   17.5880(4)
_cell_length_b                   17.5880(4)
_cell_length_c                   18.4148(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4933.2(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9943
_cell_measurement_theta_min      2.8943
_cell_measurement_theta_max      27.4891

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_F_000             2598
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.383
_exptl_crystal_size_mid          0.344
_exptl_crystal_size_min          0.262
_exptl_absorpt_coefficient_mu    0.862
_shelx_estimated_absorpt_T_min   0.734
_shelx_estimated_absorpt_T_max   0.806
_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  0.71
_exptl_absorpt_correction_T_max  0.81
_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            22520
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.585
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2516
_reflns_number_gt                2478
_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    ?
_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)+(0.0200P)²+8.5846P] 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         2516
_refine_ls_number_parameters     165
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0197
_refine_ls_wR_factor_ref         0.0500
_refine_ls_wR_factor_gt          0.0498
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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
Ni1 Ni 0.6667 0.3333 0.59983(2) 0.00692(7) Uani 1 3 d S T P . .
N1 N 0.55944(6) 0.28364(6) 0.67166(5) 0.00940(18) Uani 1 1 d . . . . .
C2 C 0.56379(7) 0.36300(7) 0.70400(6) 0.0112(2) Uani 1 1 d . . . . .
H21 H 0.5242 0.3459 0.7465 0.013 Uiso 1 1 calc R U . . .
H22 H 0.5437 0.3909 0.6679 0.013 Uiso 1 1 calc R U . . .
C3 C 0.65778(7) 0.42871(7) 0.72764(6) 0.0120(2) Uani 1 1 d . . . . .
H31 H 0.6623 0.4861 0.7375 0.014 Uiso 1 1 calc R U . . .
H32 H 0.6710 0.4080 0.7733 0.014 Uiso 1 1 calc R U . . .
C4 C 0.47729(7) 0.23236(7) 0.62930(6) 0.0119(2) Uani 1 1 d . . . . .
H41 H 0.4596 0.2727 0.6076 0.014 Uiso 1 1 calc R U . . .
H42 H 0.4296 0.1915 0.6620 0.014 Uiso 1 1 calc R U . . .
P1 P 0.49336(2) 0.16987(2) 0.55700(2) 0.00872(7) Uani 1 1 d . . . . .
O11 O 0.59083(5) 0.22255(5) 0.53884(4) 0.00995(15) Uani 1 1 d . . . . .
O12 O 0.45723(5) 0.07515(5) 0.57587(5) 0.01533(17) Uani 1 1 d . . . . .
C5 C 0.43550(7) 0.17976(8) 0.47909(6) 0.0141(2) Uani 1 1 d . . . . .
H51 H 0.4551 0.2427 0.4719 0.017 Uiso 1 1 calc R U . . .
H52 H 0.4532 0.1595 0.4355 0.017 Uiso 1 1 calc R U . . .
C6 C 0.33757(8) 0.13039(8) 0.48346(7) 0.0191(2) Uani 1 1 d . . . . .
F61 F 0.30732(6) 0.15147(7) 0.54278(5) 0.0373(2) Uani 1 1 d . . . . .
F62 F 0.30231(5) 0.04316(5) 0.48536(5) 0.0328(2) Uani 1 1 d . . . . .
F63 F 0.30145(6) 0.14743(7) 0.42648(5) 0.0389(2) Uani 1 1 d . . . . .
Mg1 Mg 0.6667 0.3333 0.3333 0.01004(17) Uani 1 6 d S T P . .
O1W O 0.63193(6) 0.22414(6) 0.39607(5) 0.01471(17) Uani 1 1 d . . . . .
H11W H 0.6235(12) 0.2221(12) 0.4392(11) 0.030(5) Uiso 1 1 d . . . . .
H12W H 0.6392(12) 0.1847(13) 0.3856(10) 0.031(5) Uiso 1 1 d . . . . .
O2W O 0.66172(7) 0.08934(7) 0.36256(6) 0.0262(2) Uani 1 1 d . . . . .
H21W H 0.6331(14) 0.0426(15) 0.3760(12) 0.041(6) Uiso 1 1 d . . . . .
H22W H 0.6970(13) 0.0884(13) 0.3337(11) 0.035(5) Uiso 1 1 d . . . . .
O3W O 0.58070(8) 0.01808(7) 0.57996(6) 0.0281(2) Uani 1 1 d . . . . .
H31W H 0.5453(16) 0.0334(15) 0.5782(12) 0.051(6) Uiso 1 1 d . . . . .
H32W H 0.5838(14) 0.0035(14) 0.5389(13) 0.046(6) 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
Ni1 O11 2.0585(7) 3_665 ?
Ni1 O11 2.0586(7) . ?
Ni1 O11 2.0586(7) 2_655 ?
Ni1 N1 2.1028(9) 2_655 ?
Ni1 N1 2.1028(9) . ?
Ni1 N1 2.1028(9) 3_665 ?
N1 C2 1.4839(13) . ?
N1 C4 1.4853(13) . ?
N1 C3 1.4923(13) 2_655 ?
C2 C3 1.5321(15) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N1 1.4923(13) 3_665 ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
C4 P1 1.8360(11) . ?
C4 H41 0.9900 . ?
C4 H42 0.9900 . ?
P1 O12 1.4970(8) . ?
P1 O11 1.5234(8) . ?
P1 C5 1.8170(11) . ?
C5 C6 1.4937(16) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 F63 1.3359(15) . ?
C6 F62 1.3372(15) . ?
C6 F61 1.3458(15) . ?
Mg1 O1W 2.0549(8) 16_655 ?
Mg1 O1W 2.0550(8) 17 ?
Mg1 O1W 2.0550(8) . ?
Mg1 O1W 2.0550(8) 2_655 ?
Mg1 O1W 2.0550(8) 3_665 ?
Mg1 O1W 2.0551(8) 18_545 ?
O1W H11W 0.81(2) . ?
O1W H12W 0.79(2) . ?
O2W H21W 0.76(2) . ?
O2W H22W 0.82(2) . ?
O3W H31W 0.79(2) . ?
O3W H32W 0.81(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
O11 Ni1 O11 93.07(3) 3_665 . ?
O11 Ni1 O11 93.07(3) 3_665 2_655 ?
O11 Ni1 O11 93.07(3) . 2_655 ?
O11 Ni1 N1 170.24(3) 3_665 2_655 ?
O11 Ni1 N1 96.67(3) . 2_655 ?
O11 Ni1 N1 85.86(3) 2_655 2_655 ?
O11 Ni1 N1 96.68(3) 3_665 . ?
O11 Ni1 N1 85.86(3) . . ?
O11 Ni1 N1 170.24(3) 2_655 . ?
N1 Ni1 N1 84.63(4) 2_655 . ?
O11 Ni1 N1 85.86(3) 3_665 3_665 ?
O11 Ni1 N1 170.24(3) . 3_665 ?
O11 Ni1 N1 96.67(3) 2_655 3_665 ?
N1 Ni1 N1 84.63(4) 2_655 3_665 ?
N1 Ni1 N1 84.63(4) . 3_665 ?
C2 N1 C4 111.04(8) . . ?
C2 N1 C3 111.69(8) . 2_655 ?
C4 N1 C3 112.25(8) . 2_655 ?
C2 N1 Ni1 104.34(6) . . ?
C4 N1 Ni1 108.66(6) . . ?
C3 N1 Ni1 108.49(6) 2_655 . ?
N1 C2 C3 110.63(9) . . ?
N1 C2 H21 109.5 . . ?
C3 C2 H21 109.5 . . ?
N1 C2 H22 109.5 . . ?
C3 C2 H22 109.5 . . ?
H21 C2 H22 108.1 . . ?
N1 C3 C2 112.52(8) 3_665 . ?
N1 C3 H31 109.1 3_665 . ?
C2 C3 H31 109.1 . . ?
N1 C3 H32 109.1 3_665 . ?
C2 C3 H32 109.1 . . ?
H31 C3 H32 107.8 . . ?
N1 C4 P1 110.50(7) . . ?
N1 C4 H41 109.6 . . ?
P1 C4 H41 109.6 . . ?
N1 C4 H42 109.6 . . ?
P1 C4 H42 109.6 . . ?
H41 C4 H42 108.1 . . ?
O12 P1 O11 116.76(5) . . ?
O12 P1 C5 110.08(5) . . ?
O11 P1 C5 106.40(5) . . ?
O12 P1 C4 113.03(5) . . ?
O11 P1 C4 104.97(5) . . ?
C5 P1 C4 104.71(5) . . ?
P1 O11 Ni1 117.09(4) . . ?
C6 C5 P1 116.11(8) . . ?
C6 C5 H51 108.3 . . ?
P1 C5 H51 108.3 . . ?
C6 C5 H52 108.3 . . ?
P1 C5 H52 108.3 . . ?
H51 C5 H52 107.4 . . ?
F63 C6 F62 106.15(10) . . ?
F63 C6 F61 106.13(11) . . ?
F62 C6 F61 105.92(11) . . ?
F63 C6 C5 111.52(11) . . ?
F62 C6 C5 114.01(10) . . ?
F61 C6 C5 112.54(10) . . ?
O1W Mg1 O1W 91.48(4) 16_655 17 ?
O1W Mg1 O1W 180.0 16_655 . ?
O1W Mg1 O1W 88.52(4) 17 . ?
O1W Mg1 O1W 88.52(4) 16_655 2_655 ?
O1W Mg1 O1W 180.0 17 2_655 ?
O1W Mg1 O1W 91.48(4) . 2_655 ?
O1W Mg1 O1W 88.52(4) 16_655 3_665 ?
O1W Mg1 O1W 88.52(4) 17 3_665 ?
O1W Mg1 O1W 91.48(4) . 3_665 ?
O1W Mg1 O1W 91.48(4) 2_655 3_665 ?
O1W Mg1 O1W 91.48(4) 16_655 18_545 ?
O1W Mg1 O1W 91.48(4) 17 18_545 ?
O1W Mg1 O1W 88.52(4) . 18_545 ?
O1W Mg1 O1W 88.52(4) 2_655 18_545 ?
O1W Mg1 O1W 180.00(4) 3_665 18_545 ?
Mg1 O1W H11W 124.0(13) . . ?
Mg1 O1W H12W 125.4(14) . . ?
H11W O1W H12W 108.0(18) . . ?
H21W O2W H22W 107(2) . . ?
H31W O3W H32W 105(2) . . ?

_refine_diff_density_max         0.383
_refine_diff_density_min         -0.297
_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_cunotpf
_database_code_depnum_ccdc_archive 'CCDC 2327156'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2024-01-20 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H24 Cu F9 N3 O6 P3, Cl, 3(H2 O), 2(H4 N)'
_chemical_formula_sum            'C15 H38 Cl Cu F9 N5 O9 P3'
_chemical_formula_weight         795.40

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                   8.3574(2)
_cell_length_b                   10.8556(3)
_cell_length_c                   17.8608(4)
_cell_angle_alpha                99.8150(10)
_cell_angle_beta                 92.1580(10)
_cell_angle_gamma                110.2640(10)
_cell_volume                     1489.65(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9931
_cell_measurement_theta_min      2.5383
_cell_measurement_theta_max      27.4731

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_F_000             814
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.066
_exptl_absorpt_coefficient_mu    1.093
_shelx_estimated_absorpt_T_min   0.880
_shelx_estimated_absorpt_T_max   0.931
_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  0.88
_exptl_absorpt_correction_T_max  0.93
_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            26087
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.039
_diffrn_reflns_theta_max         27.489
_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             6824
_reflns_number_gt                6055
_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-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_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)+(0.0392P)²+1.7594P] 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         6824
_refine_ls_number_parameters     445
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0850
_refine_ls_wR_factor_gt          0.0814
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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 0.21092(3) 0.18790(2) 0.31760(2) 0.01225(7) Uani 1 1 d . . . . .
N1 N 0.0333(2) 0.01349(18) 0.25823(11) 0.0192(4) Uani 1 1 d . . . . .
C2 C -0.1242(3) 0.0057(2) 0.29698(15) 0.0250(5) Uani 1 1 d . . . . .
H21 H -0.110867 -0.013044 0.348724 0.030 Uiso 1 1 calc R U . . .
H22 H -0.224616 -0.068028 0.267467 0.030 Uiso 1 1 calc R U . . .
C3 C -0.1528(3) 0.1385(2) 0.30276(13) 0.0198(4) Uani 1 1 d . . . . .
H31 H -0.192287 0.147450 0.251693 0.024 Uiso 1 1 calc R U . . .
H32 H -0.242238 0.140961 0.337178 0.024 Uiso 1 1 calc R U . . .
N4 N 0.0118(2) 0.25134(16) 0.33330(9) 0.0135(3) Uani 1 1 d . . . . .
C5 C 0.0469(3) 0.3634(2) 0.29053(11) 0.0155(4) Uani 1 1 d . . . . .
H51 H 0.147946 0.440157 0.317101 0.019 Uiso 1 1 calc R U . . .
H52 H -0.052616 0.392974 0.290222 0.019 Uiso 1 1 calc R U . . .
C6 C 0.0806(3) 0.3217(2) 0.20815(11) 0.0165(4) Uani 1 1 d . . . . .
H61 H -0.027705 0.258730 0.178422 0.020 Uiso 1 1 calc R U . . .
H62 H 0.121499 0.401659 0.184450 0.020 Uiso 1 1 calc R U . . .
N7 N 0.2111(2) 0.25648(17) 0.20535(9) 0.0138(3) Uani 1 1 d . . . . .
C8 C 0.1572(3) 0.1271(2) 0.15062(12) 0.0172(4) Uani 1 1 d . . . . .
H81 H 0.255482 0.096240 0.145906 0.021 Uiso 1 1 calc R U . . .
H82 H 0.122958 0.140055 0.099722 0.021 Uiso 1 1 calc R U . . .
C9 C 0.0077(3) 0.0200(2) 0.17579(13) 0.0223(5) Uani 1 1 d . . . . .
H91 H -0.098564 0.038612 0.166731 0.027 Uiso 1 1 calc R U . . .
H92 H -0.007869 -0.068320 0.144037 0.027 Uiso 1 1 calc R U . . .
C10 C 0.0945(3) -0.0965(2) 0.26965(15) 0.0254(5) Uani 1 1 d . . . . .
H101 H 0.038230 -0.176120 0.228694 0.031 Uiso 1 1 calc R U . . .
H102 H 0.064044 -0.121965 0.319325 0.031 Uiso 1 1 calc R U . . .
P1 P 0.32599(7) -0.04025(5) 0.26778(3) 0.01575(11) Uani 1 1 d . . . . .
O11 O 0.38803(18) 0.10594(14) 0.30892(8) 0.0168(3) Uani 1 1 d . . . . .
O12 O 0.38109(19) -0.06979(14) 0.19032(8) 0.0182(3) Uani 1 1 d . . . . .
C11 C 0.3969(3) -0.1314(2) 0.33049(12) 0.0214(4) Uani 1 1 d . . . . .
H111 H 0.518326 -0.079997 0.350354 0.026 Uiso 1 1 calc R U . . .
H112 H 0.328417 -0.137678 0.374667 0.026 Uiso 1 1 calc R U . . .
C12 C 0.3810(3) -0.2694(2) 0.29230(13) 0.0202(4) Uani 1 1 d . . . . .
F121 F 0.22438(18) -0.34071(14) 0.25636(10) 0.0338(3) Uani 1 1 d . . . . .
F122 F 0.49138(18) -0.26945(14) 0.23925(8) 0.0267(3) Uani 1 1 d . . . . .
F123 F 0.41278(19) -0.33976(14) 0.34173(8) 0.0294(3) Uani 1 1 d . . . . .
C20 C 0.0175(2) 0.3008(2) 0.41701(11) 0.0150(4) Uani 1 1 d . . . . .
H201 H -0.033298 0.224292 0.442679 0.018 Uiso 1 1 calc R U . . .
H202 H -0.049281 0.360505 0.425982 0.018 Uiso 1 1 calc R U . . .
P2 P 0.24237(6) 0.39263(5) 0.45593(3) 0.01302(11) Uani 1 1 d . . . . .
O21 O 0.34292(17) 0.33107(14) 0.40129(8) 0.0159(3) Uani 1 1 d . . . . .
O22 O 0.28499(19) 0.53962(15) 0.46829(8) 0.0190(3) Uani 1 1 d . . . . .
C21 C 0.2732(3) 0.3419(2) 0.54565(12) 0.0177(4) Uani 1 1 d . . . . .
H211 H 0.225823 0.242901 0.536758 0.021 Uiso 1 1 calc R U . . .
H212 H 0.398067 0.370585 0.560209 0.021 Uiso 1 1 calc R U . . .
C22 C 0.1951(3) 0.3943(2) 0.61178(12) 0.0213(4) Uani 1 1 d . . . . .
F221 F 0.02637(17) 0.36711(16) 0.59634(8) 0.0331(3) Uani 1 1 d . . . . .
F222 F 0.26727(19) 0.52707(14) 0.63565(8) 0.0282(3) Uani 1 1 d . . . . .
F223 F 0.2109(2) 0.33975(16) 0.67287(8) 0.0333(3) Uani 1 1 d . . . . .
C30 C 0.3854(2) 0.3463(2) 0.19612(11) 0.0142(4) Uani 1 1 d . . . . .
H301 H 0.468179 0.306538 0.212023 0.017 Uiso 1 1 calc R U . . .
H302 H 0.410099 0.432586 0.231917 0.017 Uiso 1 1 calc R U . . .
P3 P 0.42670(6) 0.38236(5) 0.09982(3) 0.01317(11) Uani 1 1 d . . . . .
O31 O 0.45513(19) 0.26545(14) 0.05033(8) 0.0168(3) Uani 1 1 d . . . . .
O32 O 0.29328(19) 0.43092(15) 0.06994(8) 0.0173(3) Uani 1 1 d . . . . .
C31 C 0.6306(3) 0.5257(2) 0.11610(12) 0.0166(4) Uani 1 1 d . . . . .
H311 H 0.647754 0.562897 0.068875 0.020 Uiso 1 1 calc R U . . .
H312 H 0.620088 0.595845 0.156868 0.020 Uiso 1 1 calc R U . . .
C32 C 0.7874(3) 0.4981(2) 0.13798(11) 0.0175(4) Uani 1 1 d . . . . .
F321 F 0.76971(18) 0.43430(15) 0.19665(8) 0.0303(3) Uani 1 1 d . . . . .
F322 F 0.83224(18) 0.42343(16) 0.08136(8) 0.0313(3) Uani 1 1 d . . . . .
F323 F 0.92546(17) 0.61058(14) 0.15958(9) 0.0309(3) Uani 1 1 d . . . . .
N1A N 0.6899(3) 0.2968(2) -0.06804(11) 0.0169(3) Uani 1 1 d . . . . .
H11A H 0.788(4) 0.298(3) -0.0515(17) 0.032(8) Uiso 1 1 d . . . . .
H12A H 0.619(4) 0.279(3) -0.0331(17) 0.028(7) Uiso 1 1 d . . . . .
H13A H 0.709(3) 0.377(3) -0.0742(15) 0.021(7) Uiso 1 1 d . . . . .
H14A H 0.657(4) 0.236(3) -0.1103(18) 0.027(7) Uiso 1 1 d . . . . .
N2A N 0.4337(2) 0.79895(19) 0.53619(11) 0.0175(4) Uani 1 1 d . . . . .
H21A H 0.394149 0.721758 0.516040 0.041(9) Uiso 1 1 d R . . . .
H22A H 0.368500 0.836987 0.530267 0.036(8) Uiso 1 1 d R . . . .
H23A H 0.521(5) 0.835(4) 0.515(2) 0.049(10) Uiso 1 1 d . . . . .
H24A H 0.467(4) 0.800(3) 0.577(2) 0.036(9) Uiso 1 1 d . . . . .
Cl1A Cl 0.77025(11) 1.01305(8) 0.49770(5) 0.03589(18) Uani 0.82 1 d . . P A 1
Cl1B Cl 0.6655(11) 0.9842(8) 0.4621(5) 0.0450(16) Uiso 0.1 1 d . . P B 2
Cl1C Cl 0.9090(15) 0.9988(12) 0.5743(7) 0.057(3) Uiso 0.08 1 d . . P C 3
O1W O 0.6199(2) 0.11854(17) 0.12511(10) 0.0225(3) Uani 1 1 d . . . . .
H11W H 0.552(3) 0.061(2) 0.1445(13) 0.032(8) Uiso 1 1 d . . . . .
H12W H 0.574802 0.158808 0.104221 0.036(9) Uiso 1 1 d R . . . .
O2W O 0.7810(2) 0.0075(2) 0.01742(11) 0.0317(4) Uani 1 1 d . . . . .
H21W H 0.723(4) 0.036(3) 0.046(2) 0.044(9) Uiso 1 1 d . . . . .
H22W H 0.721(5) -0.065(4) -0.002(2) 0.051(11) Uiso 1 1 d . . . . .
O3W O 0.9840(3) 0.2460(2) -0.02531(10) 0.0251(4) Uani 1 1 d . . . . .
H31W H 1.056(5) 0.288(4) 0.002(2) 0.039(10) Uiso 1 1 d . . . . .
H32W H 0.946(5) 0.179(4) -0.010(2) 0.047(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
Cu1 O21 1.9398(14) . ?
Cu1 O11 1.9721(14) . ?
Cu1 N4 2.0212(17) . ?
Cu1 N1 2.0402(18) . ?
Cu1 N7 2.2543(17) . ?
N1 C10 1.492(3) . ?
N1 C2 1.494(3) . ?
N1 C9 1.497(3) . ?
C2 C3 1.528(3) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.496(2) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C20 1.493(2) . ?
N4 C5 1.495(3) . ?
C5 C6 1.530(3) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.490(2) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C30 1.479(3) . ?
N7 C8 1.480(3) . ?
C8 C9 1.527(3) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
C10 P1 1.820(2) . ?
C10 H101 0.9900 . ?
C10 H102 0.9900 . ?
P1 O12 1.4927(15) . ?
P1 O11 1.5267(15) . ?
P1 C11 1.822(2) . ?
C11 C12 1.494(3) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 F123 1.337(2) . ?
C12 F121 1.338(3) . ?
C12 F122 1.347(3) . ?
C20 P2 1.837(2) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P2 O22 1.4839(15) . ?
P2 O21 1.5277(14) . ?
P2 C21 1.818(2) . ?
C21 C22 1.494(3) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
C22 F222 1.338(3) . ?
C22 F221 1.344(3) . ?
C22 F223 1.350(3) . ?
C30 P3 1.847(2) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
P3 O32 1.5047(15) . ?
P3 O31 1.5135(15) . ?
P3 C31 1.839(2) . ?
C31 C32 1.494(3) . ?
C31 H311 0.9900 . ?
C31 H312 0.9900 . ?
C32 F322 1.334(2) . ?
C32 F321 1.337(2) . ?
C32 F323 1.342(2) . ?
N1A H11A 0.85(3) . ?
N1A H12A 0.88(3) . ?
N1A H13A 0.85(3) . ?
N1A H14A 0.88(3) . ?
N2A H21A 0.7983 . ?
N2A H22A 0.8030 . ?
N2A H23A 0.84(4) . ?
N2A H24A 0.78(3) . ?
O1W H11W 0.82(3) . ?
O1W H12W 0.7945 . ?
O2W H21W 0.81(4) . ?
O2W H22W 0.78(4) . ?
O3W H31W 0.72(4) . ?
O3W H32W 0.78(4) . ?

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 Cu1 O11 93.71(6) . . ?
O21 Cu1 N4 88.27(6) . . ?
O11 Cu1 N4 172.28(6) . . ?
O21 Cu1 N1 161.44(7) . . ?
O11 Cu1 N1 89.93(7) . . ?
N4 Cu1 N1 85.89(7) . . ?
O21 Cu1 N7 112.86(6) . . ?
O11 Cu1 N7 101.71(6) . . ?
N4 Cu1 N7 84.33(6) . . ?
N1 Cu1 N7 84.09(7) . . ?
C10 N1 C2 111.56(17) . . ?
C10 N1 C9 112.85(18) . . ?
C2 N1 C9 111.34(18) . . ?
C10 N1 Cu1 106.99(14) . . ?
C2 N1 Cu1 102.66(13) . . ?
C9 N1 Cu1 110.89(13) . . ?
N1 C2 C3 109.38(18) . . ?
N1 C2 H21 109.8 . . ?
C3 C2 H21 109.8 . . ?
N1 C2 H22 109.8 . . ?
C3 C2 H22 109.8 . . ?
H21 C2 H22 108.2 . . ?
N4 C3 C2 109.20(17) . . ?
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 . . ?
C20 N4 C5 111.14(15) . . ?
C20 N4 C3 111.60(15) . . ?
C5 N4 C3 112.42(16) . . ?
C20 N4 Cu1 107.33(12) . . ?
C5 N4 Cu1 104.31(12) . . ?
C3 N4 Cu1 109.66(12) . . ?
N4 C5 C6 111.90(16) . . ?
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 . . ?
N7 C6 C5 111.10(16) . . ?
N7 C6 H61 109.4 . . ?
C5 C6 H61 109.4 . . ?
N7 C6 H62 109.4 . . ?
C5 C6 H62 109.4 . . ?
H61 C6 H62 108.0 . . ?
C30 N7 C8 112.29(15) . . ?
C30 N7 C6 113.89(16) . . ?
C8 N7 C6 113.54(15) . . ?
C30 N7 Cu1 110.13(11) . . ?
C8 N7 Cu1 101.07(12) . . ?
C6 N7 Cu1 104.81(12) . . ?
N7 C8 C9 111.91(17) . . ?
N7 C8 H81 109.2 . . ?
C9 C8 H81 109.2 . . ?
N7 C8 H82 109.2 . . ?
C9 C8 H82 109.2 . . ?
H81 C8 H82 107.9 . . ?
N1 C9 C8 113.04(17) . . ?
N1 C9 H91 109.0 . . ?
C8 C9 H91 109.0 . . ?
N1 C9 H92 109.0 . . ?
C8 C9 H92 109.0 . . ?
H91 C9 H92 107.8 . . ?
N1 C10 P1 109.41(14) . . ?
N1 C10 H101 109.8 . . ?
P1 C10 H101 109.8 . . ?
N1 C10 H102 109.8 . . ?
P1 C10 H102 109.8 . . ?
H101 C10 H102 108.2 . . ?
O12 P1 O11 117.53(9) . . ?
O12 P1 C10 113.95(11) . . ?
O11 P1 C10 103.62(9) . . ?
O12 P1 C11 109.25(9) . . ?
O11 P1 C11 106.83(10) . . ?
C10 P1 C11 104.67(11) . . ?
P1 O11 Cu1 115.51(8) . . ?
C12 C11 P1 113.66(15) . . ?
C12 C11 H111 108.8 . . ?
P1 C11 H111 108.8 . . ?
C12 C11 H112 108.8 . . ?
P1 C11 H112 108.8 . . ?
H111 C11 H112 107.7 . . ?
F123 C12 F121 106.73(17) . . ?
F123 C12 F122 105.82(17) . . ?
F121 C12 F122 106.14(18) . . ?
F123 C12 C11 112.27(18) . . ?
F121 C12 C11 112.55(19) . . ?
F122 C12 C11 112.81(18) . . ?
N4 C20 P2 108.58(13) . . ?
N4 C20 H201 110.0 . . ?
P2 C20 H201 110.0 . . ?
N4 C20 H202 110.0 . . ?
P2 C20 H202 110.0 . . ?
H201 C20 H202 108.4 . . ?
O22 P2 O21 118.10(9) . . ?
O22 P2 C21 110.53(9) . . ?
O21 P2 C21 104.81(9) . . ?
O22 P2 C20 111.54(9) . . ?
O21 P2 C20 103.83(9) . . ?
C21 P2 C20 107.27(10) . . ?
P2 O21 Cu1 117.00(8) . . ?
C22 C21 P2 116.69(15) . . ?
C22 C21 H211 108.1 . . ?
P2 C21 H211 108.1 . . ?
C22 C21 H212 108.1 . . ?
P2 C21 H212 108.1 . . ?
H211 C21 H212 107.3 . . ?
F222 C22 F221 106.46(18) . . ?
F222 C22 F223 106.17(18) . . ?
F221 C22 F223 106.02(18) . . ?
F222 C22 C21 113.25(18) . . ?
F221 C22 C21 112.85(18) . . ?
F223 C22 C21 111.56(18) . . ?
N7 C30 P3 117.16(13) . . ?
N7 C30 H301 108.0 . . ?
P3 C30 H301 108.0 . . ?
N7 C30 H302 108.0 . . ?
P3 C30 H302 108.0 . . ?
H301 C30 H302 107.3 . . ?
O32 P3 O31 117.86(8) . . ?
O32 P3 C31 106.45(9) . . ?
O31 P3 C31 107.87(9) . . ?
O32 P3 C30 110.03(9) . . ?
O31 P3 C30 109.64(9) . . ?
C31 P3 C30 104.03(9) . . ?
C32 C31 P3 116.44(14) . . ?
C32 C31 H311 108.2 . . ?
P3 C31 H311 108.2 . . ?
C32 C31 H312 108.2 . . ?
P3 C31 H312 108.2 . . ?
H311 C31 H312 107.3 . . ?
F322 C32 F321 106.29(18) . . ?
F322 C32 F323 105.56(17) . . ?
F321 C32 F323 105.81(17) . . ?
F322 C32 C31 113.40(17) . . ?
F321 C32 C31 112.72(17) . . ?
F323 C32 C31 112.43(18) . . ?
H11A N1A H12A 109(3) . . ?
H11A N1A H13A 104(3) . . ?
H12A N1A H13A 109(3) . . ?
H11A N1A H14A 106(3) . . ?
H12A N1A H14A 113(3) . . ?
H13A N1A H14A 115(3) . . ?
H21A N2A H22A 111.7 . . ?
H21A N2A H23A 107.5 . . ?
H22A N2A H23A 107.0 . . ?
H21A N2A H24A 105.5 . . ?
H22A N2A H24A 118.7 . . ?
H23A N2A H24A 106(3) . . ?
H11W O1W H12W 113.0 . . ?
H21W O2W H22W 105(4) . . ?
H31W O3W H32W 106(4) . . ?

_refine_diff_density_max         0.910
_refine_diff_density_min         -0.957
_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_conotpf4
_database_code_depnum_ccdc_archive 'CCDC 2327157'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2024-01-20 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_conotpf4            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.938 Why?
RESPONSE: low data quality
;
# Added during the CSD deposition process: Saturday 20 January 2024 01:38 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H54 Co2 F18 N6 Na3 O13 P6, 2(C3 H6 O), Br'
_chemical_formula_sum            'C39 H66 Br Co2 F18 N6 Na3 O15 P6'
_chemical_formula_weight         1653.53

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'
Co Co -2.3653 3.6143 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 '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                   13.7602(6)
_cell_length_b                   14.0687(6)
_cell_length_c                   32.8775(13)
_cell_angle_alpha                90
_cell_angle_beta                 93.802(2)
_cell_angle_gamma                90
_cell_volume                     6350.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    7494
_cell_measurement_theta_min      3.4182
_cell_measurement_theta_max      72.3900

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless-pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_F_000             3344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    7.521
_shelx_estimated_absorpt_T_min   0.245
_shelx_estimated_absorpt_T_max   0.621
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Sevvana, M., Ruf, M., Usón, I., Sheldrick, G. M., and Herbst-Irmer, R. (2019)
"Non-merohedral twinning: from minerals to proteins"
Acta. Cryst. D75, 1040-1050.
doi:10.1107/S2059798319010179
;
_exptl_absorpt_correction_T_min  0.22
_exptl_absorpt_correction_T_max  0.59
_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       'Bruker D8 VENTURE'
_diffrn_measurement_device_type  'κ-geometry diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_reflns_number            15764
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         3.219
_diffrn_reflns_theta_max         72.386
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measured_fraction_theta_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_point_group_measured_fraction_full 0.938
_reflns_number_total             15764
_reflns_number_gt                13905
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1194P)²+39.2142P] 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         15764
_refine_ls_number_parameters     847
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0945
_refine_ls_wR_factor_ref         0.2617
_refine_ls_wR_factor_gt          0.2563
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.113
_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
Co1A Co 0.57450(11) 0.54648(11) 0.18550(4) 0.0235(3) Uani 1 1 d . . . . .
N1A N 0.5281(6) 0.4584(6) 0.2342(2) 0.0271(17) Uani 1 1 d . . . . .
C2A C 0.4384(7) 0.5078(7) 0.2459(3) 0.0280(19) Uani 1 1 d . . . . .
H21 H 0.456395 0.569367 0.258897 0.034 Uiso 1 1 calc R U . . .
H22 H 0.405884 0.468658 0.266017 0.034 Uiso 1 1 calc R U . . .
C3A C 0.3681(7) 0.5251(7) 0.2087(3) 0.031(2) Uani 1 1 d . . . . .
H31 H 0.339246 0.463919 0.199211 0.038 Uiso 1 1 calc R U . . .
H32 H 0.314644 0.567174 0.216378 0.038 Uiso 1 1 calc R U . . .
N4A N 0.4194(6) 0.5695(6) 0.1754(2) 0.0260(16) Uani 1 1 d . . . . .
C5A C 0.3952(7) 0.5239(7) 0.1357(3) 0.032(2) Uani 1 1 d . . . . .
H51 H 0.423424 0.561683 0.113994 0.038 Uiso 1 1 calc R U . . .
H52 H 0.323629 0.523065 0.130248 0.038 Uiso 1 1 calc R U . . .
C6A C 0.4343(7) 0.4217(7) 0.1346(3) 0.029(2) Uani 1 1 d . . . . .
H61 H 0.395520 0.380033 0.151560 0.034 Uiso 1 1 calc R U . . .
H62 H 0.428197 0.397482 0.106234 0.034 Uiso 1 1 calc R U . . .
N7A N 0.5399(6) 0.4196(6) 0.1504(2) 0.0272(16) Uani 1 1 d . . . . .
C8A C 0.5616(8) 0.3417(7) 0.1800(3) 0.033(2) Uani 1 1 d . . . . .
H81 H 0.632858 0.337249 0.186177 0.039 Uiso 1 1 calc R U . . .
H82 H 0.538682 0.280517 0.167990 0.039 Uiso 1 1 calc R U . . .
C9A C 0.5104(7) 0.3609(7) 0.2198(3) 0.0284(19) Uani 1 1 d . . . . .
H91 H 0.439487 0.350466 0.214779 0.034 Uiso 1 1 calc R U . . .
H92 H 0.535021 0.315536 0.241082 0.034 Uiso 1 1 calc R U . . .
C10A C 0.6064(7) 0.4598(7) 0.2683(3) 0.0280(19) Uani 1 1 d . . . . .
H101 H 0.654907 0.409717 0.263523 0.034 Uiso 1 1 calc R U . . .
H102 H 0.577137 0.445307 0.294308 0.034 Uiso 1 1 calc R U . . .
P1A P 0.66742(17) 0.57469(18) 0.27239(6) 0.0249(5) Uani 1 1 d . . . . .
O1A O 0.6310(5) 0.6310(4) 0.23445(18) 0.0249(13) Uani 1 1 d . . . . .
O1B O 0.7763(5) 0.5600(4) 0.27779(18) 0.0257(13) Uani 1 1 d . . . . .
C11A C 0.6274(7) 0.6404(7) 0.3157(3) 0.029(2) Uani 1 1 d . . . . .
H111 H 0.653123 0.705905 0.313857 0.035 Uiso 1 1 calc R U . . .
H112 H 0.555501 0.645070 0.312289 0.035 Uiso 1 1 calc R U . . .
C12A C 0.6525(8) 0.6062(8) 0.3573(3) 0.037(2) Uani 1 1 d . . . . .
F1A F 0.6080(6) 0.5241(5) 0.36487(19) 0.0515(18) Uani 1 1 d . . . . .
F1B F 0.7494(5) 0.5885(6) 0.36400(18) 0.0478(17) Uani 1 1 d . . . . .
F1C F 0.6296(5) 0.6672(6) 0.38607(18) 0.0481(17) Uani 1 1 d . . . . .
C20A C 0.4012(7) 0.6739(7) 0.1726(3) 0.029(2) Uani 1 1 d . . . . .
H201 H 0.394129 0.699591 0.200295 0.035 Uiso 1 1 calc R U . . .
H202 H 0.339416 0.685414 0.156211 0.035 Uiso 1 1 calc R U . . .
P2A P 0.50056(17) 0.73709(18) 0.14926(7) 0.0252(5) Uani 1 1 d . . . . .
O2A O 0.5859(5) 0.6671(4) 0.14832(19) 0.0260(13) Uani 1 1 d . . . . .
O2B O 0.5200(5) 0.8273(5) 0.17208(19) 0.0318(15) Uani 1 1 d . . . . .
C21A C 0.4662(8) 0.7640(8) 0.0953(3) 0.036(2) Uani 1 1 d . . . . .
H211 H 0.507791 0.817043 0.086970 0.043 Uiso 1 1 calc R U . . .
H212 H 0.482549 0.707852 0.078963 0.043 Uiso 1 1 calc R U . . .
C22A C 0.3646(9) 0.7895(10) 0.0841(4) 0.047(3) Uani 1 1 d . . . . .
F2A F 0.3048(5) 0.7122(6) 0.0823(2) 0.0567(19) Uani 1 1 d . . . . .
F2B F 0.3257(6) 0.8496(6) 0.1102(3) 0.062(2) Uani 1 1 d . . . . .
F2C F 0.3544(7) 0.8298(8) 0.0467(3) 0.080(3) Uani 1 1 d . . . . .
C30A C 0.6050(7) 0.4161(7) 0.1171(3) 0.0278(19) Uani 1 1 d . . . . .
H301 H 0.576067 0.453116 0.093734 0.033 Uiso 1 1 calc R U . . .
H302 H 0.611606 0.349386 0.108145 0.033 Uiso 1 1 calc R U . . .
P3A P 0.72666(18) 0.46420(17) 0.13237(7) 0.0258(5) Uani 1 1 d . . . . .
O3A O 0.7166(5) 0.5060(5) 0.17430(19) 0.0267(13) Uani 1 1 d . . . . .
O3B O 0.7598(5) 0.5284(5) 0.09984(19) 0.0313(15) Uani 1 1 d . . . . .
C31A C 0.8124(7) 0.3646(6) 0.1402(3) 0.0235(18) Uani 1 1 d . . . . .
H311 H 0.873928 0.389237 0.153482 0.028 Uiso 1 1 calc R U . . .
H312 H 0.784912 0.318769 0.159213 0.028 Uiso 1 1 calc R U . . .
C32A C 0.8353(8) 0.3125(7) 0.1024(3) 0.032(2) Uani 1 1 d . . . . .
F3A F 0.7586(5) 0.2871(5) 0.0787(2) 0.0508(18) Uani 1 1 d . . . . .
F3B F 0.8932(5) 0.3608(5) 0.07933(18) 0.0415(14) Uani 1 1 d . . . . .
F3C F 0.8830(6) 0.2308(5) 0.1124(2) 0.0479(17) Uani 1 1 d . . . . .
Co1D Co 0.90705(11) 0.83314(11) 0.18140(4) 0.0223(3) Uani 1 1 d . . . . .
N1D N 0.9688(6) 0.9224(5) 0.2295(2) 0.0231(15) Uani 1 1 d . . . . .
C2D C 1.0636(7) 0.8746(7) 0.2414(3) 0.0254(18) Uani 1 1 d . . . . .
H25 H 1.051104 0.814187 0.255578 0.030 Uiso 1 1 calc R U . . .
H26 H 1.102881 0.915913 0.260578 0.030 Uiso 1 1 calc R U . . .
C3D C 1.1202(7) 0.8546(8) 0.2044(3) 0.030(2) Uani 1 1 d . . . . .
H35 H 1.146651 0.915009 0.194320 0.035 Uiso 1 1 calc R U . . .
H36 H 1.175827 0.812424 0.212322 0.035 Uiso 1 1 calc R U . . .
N4D N 1.0579(6) 0.8085(6) 0.1707(2) 0.0252(16) Uani 1 1 d . . . . .
C5D C 1.0678(7) 0.8567(7) 0.1309(3) 0.0268(19) Uani 1 1 d . . . . .
H55 H 1.032458 0.819254 0.109112 0.032 Uiso 1 1 calc R U . . .
H56 H 1.137431 0.858035 0.125038 0.032 Uiso 1 1 calc R U . . .
C6D C 1.0291(7) 0.9565(8) 0.1298(3) 0.031(2) Uani 1 1 d . . . . .
H65 H 1.073220 0.998295 0.146754 0.037 Uiso 1 1 calc R U . . .
H66 H 1.025732 0.980768 0.101486 0.037 Uiso 1 1 calc R U . . .
N7D N 0.9296(6) 0.9576(6) 0.1457(2) 0.0256(16) Uani 1 1 d . . . . .
C8D C 0.9195(7) 1.0368(7) 0.1742(3) 0.0265(18) Uani 1 1 d . . . . .
H85 H 0.850285 1.042830 0.180391 0.032 Uiso 1 1 calc R U . . .
H86 H 0.938816 1.096656 0.161106 0.032 Uiso 1 1 calc R U . . .
C9D C 0.9815(7) 1.0232(7) 0.2138(3) 0.0263(19) Uani 1 1 d . . . . .
H95 H 0.961656 1.069432 0.234342 0.032 Uiso 1 1 calc R U . . .
H96 H 1.050796 1.034594 0.209033 0.032 Uiso 1 1 calc R U . . .
C10D C 0.9003(7) 0.9248(7) 0.2627(3) 0.0268(19) Uani 1 1 d . . . . .
H105 H 0.850475 0.974439 0.256510 0.032 Uiso 1 1 calc R U . . .
H106 H 0.936623 0.941929 0.288628 0.032 Uiso 1 1 calc R U . . .
P1D P 0.84004(17) 0.81064(18) 0.26858(6) 0.0239(4) Uani 1 1 d . . . . .
O1D O 0.8660(5) 0.7519(5) 0.23205(16) 0.0246(13) Uani 1 1 d . . . . .
O1E O 0.7336(5) 0.8249(5) 0.27329(18) 0.0283(14) Uani 1 1 d . . . . .
C11D C 0.8938(7) 0.7506(7) 0.3144(3) 0.0259(18) Uani 1 1 d . . . . .
H115 H 0.869455 0.684407 0.314150 0.031 Uiso 1 1 calc R U . . .
H116 H 0.965176 0.747558 0.312202 0.031 Uiso 1 1 calc R U . . .
C12D C 0.8760(8) 0.7925(9) 0.3544(3) 0.037(2) Uani 1 1 d . . . . .
F1D F 0.9155(7) 0.8802(6) 0.3595(2) 0.059(2) Uani 1 1 d . . . . .
F1E F 0.7788(5) 0.8060(5) 0.35961(18) 0.0439(15) Uani 1 1 d . . . . .
F1F F 0.9097(5) 0.7409(6) 0.38521(17) 0.0494(18) Uani 1 1 d . . . . .
C20D C 1.0778(7) 0.7051(7) 0.1680(3) 0.030(2) Uani 1 1 d . . . . .
H205 H 1.100630 0.680816 0.195220 0.036 Uiso 1 1 calc R U . . .
H206 H 1.130302 0.694434 0.149297 0.036 Uiso 1 1 calc R U . . .
P2D P 0.96859(17) 0.63889(17) 0.14932(7) 0.0250(5) Uani 1 1 d . . . . .
O2D O 0.8868(5) 0.7105(4) 0.1436(2) 0.0284(14) Uani 1 1 d . . . . .
O2E O 0.9559(5) 0.5589(6) 0.1774(2) 0.0338(15) Uani 1 1 d . . . . .
C21D C 0.9885(7) 0.5810(7) 0.1002(3) 0.0292(19) Uani 1 1 d . . . . .
H215 H 1.047329 0.540753 0.104590 0.035 Uiso 1 1 calc R U . . .
H216 H 0.932961 0.537477 0.094099 0.035 Uiso 1 1 calc R U . . .
C22D C 1.0005(10) 0.6370(10) 0.0635(3) 0.048(3) Uani 1 1 d . . . . .
F2D F 0.9282(7) 0.7023(5) 0.0554(2) 0.060(2) Uani 1 1 d . . . . .
F2E F 1.0836(6) 0.6866(6) 0.0652(2) 0.059(2) Uani 1 1 d . . . . .
F2F F 1.0003(6) 0.5841(5) 0.02996(19) 0.0535(19) Uani 1 1 d . . . . .
C30D C 0.8525(8) 0.9624(7) 0.1118(3) 0.033(2) Uani 1 1 d . . . . .
H305 H 0.873296 0.925830 0.088166 0.040 Uiso 1 1 calc R U . . .
H306 H 0.842614 1.029328 0.103182 0.040 Uiso 1 1 calc R U . . .
P3D P 0.73685(18) 0.91330(18) 0.12825(7) 0.0257(5) Uani 1 1 d . . . . .
O3D O 0.7615(5) 0.8728(5) 0.17093(19) 0.0282(14) Uani 1 1 d . . . . .
O3E O 0.6941(5) 0.8479(5) 0.0965(2) 0.0327(15) Uani 1 1 d . . . . .
C31D C 0.6558(7) 1.0130(7) 0.1356(3) 0.030(2) Uani 1 1 d . . . . .
H315 H 0.600326 0.990466 0.150764 0.036 Uiso 1 1 calc R U . . .
H316 H 0.691335 1.061224 0.152773 0.036 Uiso 1 1 calc R U . . .
C32D C 0.6165(9) 1.0597(9) 0.0969(3) 0.040(3) Uani 1 1 d . . . . .
F3D F 0.6856(5) 1.0806(6) 0.0715(2) 0.0512(18) Uani 1 1 d . . . . .
F3E F 0.5487(5) 1.0088(5) 0.07527(18) 0.0436(15) Uani 1 1 d . . . . .
F3F F 0.5717(5) 1.1442(5) 0.1051(2) 0.0467(16) Uani 1 1 d . . . . .
Na1 Na 0.6636(3) 0.7824(3) 0.20962(10) 0.0298(8) Uani 1 1 d . . . . .
Na2 Na 0.7264(3) 0.6872(3) 0.10218(11) 0.0326(8) Uani 1 1 d . . . . .
Na3 Na 0.8256(3) 0.5963(3) 0.21377(10) 0.0278(7) Uani 1 1 d . . . . .
Br1 Br 0.74988(9) 0.18921(8) 0.22411(3) 0.0351(2) Uani 1 1 d . . . . .
C1S C 0.5433(15) 0.760(2) -0.0165(5) 0.110(8) Uani 1 1 d D . . . .
H1S1 H 0.493318 0.718127 -0.006072 0.165 Uiso 1 1 calc R U . . .
H1S2 H 0.552643 0.743114 -0.044937 0.165 Uiso 1 1 calc R U . . .
H1S3 H 0.522463 0.825945 -0.014885 0.165 Uiso 1 1 calc R U . . .
C2S C 0.6374(11) 0.7463(13) 0.0087(4) 0.062(4) Uani 1 1 d D . . . .
O2S O 0.6471(8) 0.6880(7) 0.0355(3) 0.064(3) Uani 1 1 d D . . . .
C3S C 0.7154(19) 0.8169(19) -0.0008(6) 0.124(10) Uani 1 1 d D . . . .
H3S1 H 0.745254 0.797648 -0.025731 0.186 Uiso 1 1 calc R U . . .
H3S2 H 0.765232 0.818943 0.021905 0.186 Uiso 1 1 calc R U . . .
H3S3 H 0.686150 0.880088 -0.004664 0.186 Uiso 1 1 calc R U . . .
C1T C 0.9933(15) 0.6611(13) 0.4701(5) 0.079(5) Uani 1 1 d . . . . .
H1T1 H 0.987618 0.615016 0.447741 0.119 Uiso 1 1 calc R U . . .
H1T2 H 1.035704 0.713534 0.462818 0.119 Uiso 1 1 calc R U . . .
H1T3 H 0.928608 0.686072 0.475043 0.119 Uiso 1 1 calc R U . . .
C2T C 1.0347(12) 0.6148(10) 0.5068(4) 0.056(3) Uani 1 1 d . . . . .
O2T O 0.9883(8) 0.5851(7) 0.5333(2) 0.057(2) Uani 1 1 d . . . . .
C3T C 1.1414(12) 0.6018(17) 0.5091(6) 0.097(7) Uani 1 1 d . . . . .
H3T1 H 1.173384 0.664116 0.510553 0.145 Uiso 1 1 calc R U . . .
H3T2 H 1.160210 0.567900 0.484812 0.145 Uiso 1 1 calc R U . . .
H3T3 H 1.161569 0.564885 0.533505 0.145 Uiso 1 1 calc R U . . .
C1U C 0.227(2) 0.436(2) 0.0394(9) 0.080(9) Uani 0.60(2) 1 d . U P A 1
H1U1 H 0.251122 0.398001 0.063020 0.120 Uiso 0.60(2) 1 d R U P A 1
H1U2 H 0.198894 0.393677 0.018094 0.120 Uiso 0.60(2) 1 d R U P A 1
H1U3 H 0.177861 0.480740 0.047581 0.120 Uiso 0.60(2) 1 d R U P A 1
C2U C 0.312(3) 0.490(5) 0.0258(16) 0.071(5) Uani 0.60(2) 1 d . U P A 1
O2U O 0.3885(15) 0.4802(18) 0.0429(6) 0.075(6) Uani 0.60(2) 1 d . U P A 1
C3U C 0.266(3) 0.560(3) -0.0059(11) 0.113(14) Uani 0.60(2) 1 d . U P A 1
H3U1 H 0.207786 0.592180 0.002710 0.169 Uiso 0.60(2) 1 d R U P A 1
H3U2 H 0.251941 0.531016 -0.032729 0.169 Uiso 0.60(2) 1 d R U P A 1
H3U3 H 0.318875 0.606591 -0.007587 0.169 Uiso 0.60(2) 1 d R U P A 1
C1V C 0.202(3) 0.484(4) 0.0021(14) 0.095(17) Uani 0.40(2) 1 d D U P A 2
H1V1 H 0.205263 0.472175 -0.027097 0.142 Uiso 0.40(2) 1 d R U P A 2
H1V2 H 0.162407 0.541125 0.006042 0.142 Uiso 0.40(2) 1 d R U P A 2
H1V3 H 0.172384 0.429618 0.014992 0.142 Uiso 0.40(2) 1 d R U P A 2
C2V C 0.301(4) 0.497(7) 0.023(2) 0.071(5) Uani 0.40(2) 1 d D U P A 2
O2V O 0.329(3) 0.447(3) 0.0516(10) 0.099(12) Uani 0.40(2) 1 d D U P A 2
C3V C 0.367(3) 0.558(3) -0.0009(13) 0.077(13) Uani 0.40(2) 1 d D U P A 2
H3V1 H 0.431069 0.568073 0.013119 0.116 Uiso 0.40(2) 1 d R U P A 2
H3V2 H 0.335306 0.619484 -0.006450 0.116 Uiso 0.40(2) 1 d R U P A 2
H3V3 H 0.374116 0.524374 -0.026592 0.116 Uiso 0.40(2) 1 d R U 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
Co1A O3A 2.093(7) . ?
Co1A O2A 2.104(6) . ?
Co1A O1A 2.108(6) . ?
Co1A N1A 2.154(8) . ?
Co1A N7A 2.162(8) . ?
Co1A N4A 2.163(8) . ?
N1A C9A 1.467(12) . ?
N1A C2A 1.489(11) . ?
N1A C10A 1.503(12) . ?
C2A C3A 1.527(13) . ?
C2A H21 0.9900 . ?
C2A H22 0.9900 . ?
C3A N4A 1.480(12) . ?
C3A H31 0.9900 . ?
C3A H32 0.9900 . ?
N4A C5A 1.472(12) . ?
N4A C20A 1.492(11) . ?
C5A C6A 1.537(14) . ?
C5A H51 0.9900 . ?
C5A H52 0.9900 . ?
C6A N7A 1.510(12) . ?
C6A H61 0.9900 . ?
C6A H62 0.9900 . ?
N7A C30A 1.459(11) . ?
N7A C8A 1.483(13) . ?
C8A C9A 1.550(13) . ?
C8A H81 0.9900 . ?
C8A H82 0.9900 . ?
C9A H91 0.9900 . ?
C9A H92 0.9900 . ?
C10A P1A 1.823(10) . ?
C10A H101 0.9900 . ?
C10A H102 0.9900 . ?
P1A O1B 1.510(7) . ?
P1A O1A 1.533(7) . ?
P1A C11A 1.814(9) . ?
O1A Na1 2.336(7) . ?
O1A Na3 2.848(7) . ?
O1B Na3 2.311(7) . ?
C11A C12A 1.470(14) . ?
C11A H111 0.9900 . ?
C11A H112 0.9900 . ?
C12A F1C 1.330(12) . ?
C12A F1A 1.339(12) . ?
C12A F1B 1.360(13) . ?
C20A P2A 1.840(10) . ?
C20A H201 0.9900 . ?
C20A H202 0.9900 . ?
P2A O2B 1.489(7) . ?
P2A O2A 1.534(7) . ?
P2A C21A 1.844(10) . ?
O2A Na2 2.551(8) . ?
O2A Na1 2.748(7) . ?
O2B Na1 2.346(8) . ?
C21A C22A 1.467(16) . ?
C21A H211 0.9900 . ?
C21A H212 0.9900 . ?
C22A F2B 1.341(16) . ?
C22A F2C 1.353(14) . ?
C22A F2A 1.362(14) . ?
C30A P3A 1.844(10) . ?
C30A H301 0.9900 . ?
C30A H302 0.9900 . ?
P3A O3B 1.494(7) . ?
P3A O3A 1.513(6) . ?
P3A C31A 1.839(9) . ?
O3A Na3 2.300(7) . ?
O3B Na2 2.282(8) . ?
C31A C32A 1.493(12) . ?
C31A H311 0.9900 . ?
C31A H312 0.9900 . ?
C32A F3A 1.319(12) . ?
C32A F3B 1.324(12) . ?
C32A F3C 1.353(12) . ?
Co1D O3D 2.086(7) . ?
Co1D O1D 2.127(6) . ?
Co1D O2D 2.133(6) . ?
Co1D N7D 2.141(8) . ?
Co1D N1D 2.149(7) . ?
Co1D N4D 2.156(8) . ?
N1D C10D 1.489(12) . ?
N1D C2D 1.497(11) . ?
N1D C9D 1.523(11) . ?
C2D C3D 1.514(13) . ?
C2D H25 0.9900 . ?
C2D H26 0.9900 . ?
C3D N4D 1.500(12) . ?
C3D H35 0.9900 . ?
C3D H36 0.9900 . ?
N4D C20D 1.485(12) . ?
N4D C5D 1.490(11) . ?
C5D C6D 1.501(14) . ?
C5D H55 0.9900 . ?
C5D H56 0.9900 . ?
C6D N7D 1.498(12) . ?
C6D H65 0.9900 . ?
C6D H66 0.9900 . ?
N7D C8D 1.469(12) . ?
N7D C30D 1.489(12) . ?
C8D C9D 1.519(12) . ?
C8D H85 0.9900 . ?
C8D H86 0.9900 . ?
C9D H95 0.9900 . ?
C9D H96 0.9900 . ?
C10D P1D 1.824(10) . ?
C10D H105 0.9900 . ?
C10D H106 0.9900 . ?
P1D O1E 1.497(7) . ?
P1D O1D 1.520(6) . ?
P1D C11D 1.839(9) . ?
O1D Na3 2.327(7) . ?
O1D Na1 2.865(7) . ?
O1E Na1 2.324(7) . ?
C11D C12D 1.476(13) . ?
C11D H115 0.9900 . ?
C11D H116 0.9900 . ?
C12D F1F 1.307(12) . ?
C12D F1D 1.354(13) . ?
C12D F1E 1.372(13) . ?
C20D P2D 1.838(10) . ?
C20D H205 0.9900 . ?
C20D H206 0.9900 . ?
P2D O2E 1.472(7) . ?
P2D O2D 1.513(7) . ?
P2D C21D 1.845(9) . ?
O2D Na2 2.537(8) . ?
O2D Na3 2.978(8) . ?
O2E Na3 2.283(8) . ?
C21D C22D 1.461(15) . ?
C21D H215 0.9900 . ?
C21D H216 0.9900 . ?
C22D F2F 1.330(14) . ?
C22D F2E 1.338(16) . ?
C22D F2D 1.366(15) . ?
C30D P3D 1.848(11) . ?
C30D H305 0.9900 . ?
C30D H306 0.9900 . ?
P3D O3E 1.485(7) . ?
P3D O3D 1.532(7) . ?
P3D C31D 1.819(10) . ?
O3D Na1 2.297(7) . ?
O3E Na2 2.309(8) . ?
C31D C32D 1.500(14) . ?
C31D H315 0.9900 . ?
C31D H316 0.9900 . ?
C32D F3D 1.339(13) . ?
C32D F3E 1.342(14) . ?
C32D F3F 1.374(13) . ?
Na2 O2S 2.382(9) . ?
C1S C2S 1.50(2) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
C2S O2S 1.206(18) . ?
C2S C3S 1.51(3) . ?
C3S H3S1 0.9800 . ?
C3S H3S2 0.9800 . ?
C3S H3S3 0.9800 . ?
C1T C2T 1.45(2) . ?
C1T H1T1 0.9800 . ?
C1T H1T2 0.9800 . ?
C1T H1T3 0.9800 . ?
C2T O2T 1.190(16) . ?
C2T C3T 1.48(2) . ?
C3T H3T1 0.9800 . ?
C3T H3T2 0.9800 . ?
C3T H3T3 0.9800 . ?
C1U C2U 1.48(5) . ?
C1U H1U1 0.9800 . ?
C1U H1U2 0.9800 . ?
C1U H1U3 0.9800 . ?
C2U O2U 1.17(4) . ?
C2U C3U 1.54(5) . ?
C3U H3U1 0.9800 . ?
C3U H3U2 0.9800 . ?
C3U H3U3 0.9800 . ?
C1V C2V 1.50(3) . ?
C1V H1V1 0.9800 . ?
C1V H1V2 0.9800 . ?
C1V H1V3 0.9800 . ?
C2V O2V 1.20(3) . ?
C2V C3V 1.51(3) . ?
C3V H3V1 0.9800 . ?
C3V H3V2 0.9800 . ?
C3V H3V3 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
O3A Co1A O2A 90.6(3) . . ?
O3A Co1A O1A 89.2(3) . . ?
O2A Co1A O1A 87.2(3) . . ?
O3A Co1A N1A 107.5(3) . . ?
O2A Co1A N1A 158.9(3) . . ?
O1A Co1A N1A 82.5(3) . . ?
O3A Co1A N7A 81.8(3) . . ?
O2A Co1A N7A 112.2(3) . . ?
O1A Co1A N7A 158.6(3) . . ?
N1A Co1A N7A 81.7(3) . . ?
O3A Co1A N4A 159.7(3) . . ?
O2A Co1A N4A 84.3(3) . . ?
O1A Co1A N4A 110.0(3) . . ?
N1A Co1A N4A 82.1(3) . . ?
N7A Co1A N4A 82.0(3) . . ?
C9A N1A C2A 113.4(8) . . ?
C9A N1A C10A 110.4(7) . . ?
C2A N1A C10A 111.5(7) . . ?
C9A N1A Co1A 110.4(6) . . ?
C2A N1A Co1A 102.4(6) . . ?
C10A N1A Co1A 108.3(6) . . ?
N1A C2A C3A 111.0(7) . . ?
N1A C2A H21 109.4 . . ?
C3A C2A H21 109.4 . . ?
N1A C2A H22 109.4 . . ?
C3A C2A H22 109.4 . . ?
H21 C2A H22 108.0 . . ?
N4A C3A C2A 110.6(8) . . ?
N4A C3A H31 109.5 . . ?
C2A C3A H31 109.5 . . ?
N4A C3A H32 109.5 . . ?
C2A C3A H32 109.5 . . ?
H31 C3A H32 108.1 . . ?
C5A N4A C3A 112.4(8) . . ?
C5A N4A C20A 110.3(7) . . ?
C3A N4A C20A 112.1(7) . . ?
C5A N4A Co1A 103.5(6) . . ?
C3A N4A Co1A 109.7(6) . . ?
C20A N4A Co1A 108.4(6) . . ?
N4A C5A C6A 111.8(8) . . ?
N4A C5A H51 109.3 . . ?
C6A C5A H51 109.3 . . ?
N4A C5A H52 109.3 . . ?
C6A C5A H52 109.3 . . ?
H51 C5A H52 107.9 . . ?
N7A C6A C5A 109.8(8) . . ?
N7A C6A H61 109.7 . . ?
C5A C6A H61 109.7 . . ?
N7A C6A H62 109.7 . . ?
C5A C6A H62 109.7 . . ?
H61 C6A H62 108.2 . . ?
C30A N7A C8A 111.1(8) . . ?
C30A N7A C6A 111.6(7) . . ?
C8A N7A C6A 112.8(8) . . ?
C30A N7A Co1A 107.7(6) . . ?
C8A N7A Co1A 103.4(6) . . ?
C6A N7A Co1A 109.9(6) . . ?
N7A C8A C9A 110.0(8) . . ?
N7A C8A H81 109.7 . . ?
C9A C8A H81 109.7 . . ?
N7A C8A H82 109.7 . . ?
C9A C8A H82 109.7 . . ?
H81 C8A H82 108.2 . . ?
N1A C9A C8A 111.1(8) . . ?
N1A C9A H91 109.4 . . ?
C8A C9A H91 109.4 . . ?
N1A C9A H92 109.4 . . ?
C8A C9A H92 109.4 . . ?
H91 C9A H92 108.0 . . ?
N1A C10A P1A 111.7(6) . . ?
N1A C10A H101 109.3 . . ?
P1A C10A H101 109.3 . . ?
N1A C10A H102 109.3 . . ?
P1A C10A H102 109.3 . . ?
H101 C10A H102 107.9 . . ?
O1B P1A O1A 115.7(4) . . ?
O1B P1A C11A 109.1(4) . . ?
O1A P1A C11A 106.0(4) . . ?
O1B P1A C10A 109.6(4) . . ?
O1A P1A C10A 105.9(4) . . ?
C11A P1A C10A 110.4(4) . . ?
P1A O1A Co1A 114.5(4) . . ?
P1A O1A Na1 134.1(4) . . ?
Co1A O1A Na1 108.5(3) . . ?
P1A O1A Na3 81.0(3) . . ?
Co1A O1A Na3 91.5(2) . . ?
Na1 O1A Na3 82.4(2) . . ?
P1A O1B Na3 102.2(3) . . ?
C12A C11A P1A 119.9(8) . . ?
C12A C11A H111 107.3 . . ?
P1A C11A H111 107.3 . . ?
C12A C11A H112 107.3 . . ?
P1A C11A H112 107.3 . . ?
H111 C11A H112 106.9 . . ?
F1C C12A F1A 107.0(8) . . ?
F1C C12A F1B 106.2(9) . . ?
F1A C12A F1B 105.5(10) . . ?
F1C C12A C11A 113.5(10) . . ?
F1A C12A C11A 111.9(9) . . ?
F1B C12A C11A 112.2(8) . . ?
N4A C20A P2A 112.1(6) . . ?
N4A C20A H201 109.2 . . ?
P2A C20A H201 109.2 . . ?
N4A C20A H202 109.2 . . ?
P2A C20A H202 109.2 . . ?
H201 C20A H202 107.9 . . ?
O2B P2A O2A 116.4(4) . . ?
O2B P2A C20A 108.3(4) . . ?
O2A P2A C20A 106.8(4) . . ?
O2B P2A C21A 109.6(5) . . ?
O2A P2A C21A 105.1(4) . . ?
C20A P2A C21A 110.5(5) . . ?
P2A O2A Co1A 114.8(4) . . ?
P2A O2A Na2 123.5(3) . . ?
Co1A O2A Na2 121.6(3) . . ?
P2A O2A Na1 82.4(3) . . ?
Co1A O2A Na1 95.2(2) . . ?
Na2 O2A Na1 95.6(2) . . ?
P2A O2B Na1 98.8(4) . . ?
C22A C21A P2A 118.1(8) . . ?
C22A C21A H211 107.8 . . ?
P2A C21A H211 107.8 . . ?
C22A C21A H212 107.8 . . ?
P2A C21A H212 107.8 . . ?
H211 C21A H212 107.1 . . ?
F2B C22A F2C 107.1(12) . . ?
F2B C22A F2A 105.4(10) . . ?
F2C C22A F2A 105.6(10) . . ?
F2B C22A C21A 114.1(10) . . ?
F2C C22A C21A 111.7(10) . . ?
F2A C22A C21A 112.3(11) . . ?
N7A C30A P3A 112.1(6) . . ?
N7A C30A H301 109.2 . . ?
P3A C30A H301 109.2 . . ?
N7A C30A H302 109.2 . . ?
P3A C30A H302 109.2 . . ?
H301 C30A H302 107.9 . . ?
O3B P3A O3A 117.9(4) . . ?
O3B P3A C31A 109.7(4) . . ?
O3A P3A C31A 105.4(4) . . ?
O3B P3A C30A 110.0(4) . . ?
O3A P3A C30A 104.7(4) . . ?
C31A P3A C30A 108.7(4) . . ?
P3A O3A Co1A 114.1(4) . . ?
P3A O3A Na3 129.3(4) . . ?
Co1A O3A Na3 109.4(3) . . ?
P3A O3B Na2 119.7(4) . . ?
C32A C31A P3A 115.3(6) . . ?
C32A C31A H311 108.5 . . ?
P3A C31A H311 108.5 . . ?
C32A C31A H312 108.5 . . ?
P3A C31A H312 108.5 . . ?
H311 C31A H312 107.5 . . ?
F3A C32A F3B 106.8(8) . . ?
F3A C32A F3C 105.6(8) . . ?
F3B C32A F3C 106.0(8) . . ?
F3A C32A C31A 114.8(9) . . ?
F3B C32A C31A 113.2(8) . . ?
F3C C32A C31A 109.9(8) . . ?
O3D Co1D O1D 88.3(3) . . ?
O3D Co1D O2D 91.9(3) . . ?
O1D Co1D O2D 89.4(3) . . ?
O3D Co1D N7D 82.1(3) . . ?
O1D Co1D N7D 157.5(3) . . ?
O2D Co1D N7D 111.1(3) . . ?
O3D Co1D N1D 107.1(3) . . ?
O1D Co1D N1D 81.4(3) . . ?
O2D Co1D N1D 158.5(3) . . ?
N7D Co1D N1D 82.0(3) . . ?
O3D Co1D N4D 160.2(3) . . ?
O1D Co1D N4D 110.5(3) . . ?
O2D Co1D N4D 82.3(3) . . ?
N7D Co1D N4D 82.3(3) . . ?
N1D Co1D N4D 82.8(3) . . ?
C10D N1D C2D 113.6(7) . . ?
C10D N1D C9D 108.6(7) . . ?
C2D N1D C9D 112.9(7) . . ?
C10D N1D Co1D 108.3(5) . . ?
C2D N1D Co1D 103.1(5) . . ?
C9D N1D Co1D 110.1(5) . . ?
N1D C2D C3D 111.0(7) . . ?
N1D C2D H25 109.4 . . ?
C3D C2D H25 109.4 . . ?
N1D C2D H26 109.4 . . ?
C3D C2D H26 109.4 . . ?
H25 C2D H26 108.0 . . ?
N4D C3D C2D 112.0(7) . . ?
N4D C3D H35 109.2 . . ?
C2D C3D H35 109.2 . . ?
N4D C3D H36 109.2 . . ?
C2D C3D H36 109.2 . . ?
H35 C3D H36 107.9 . . ?
C20D N4D C5D 111.4(7) . . ?
C20D N4D C3D 111.7(7) . . ?
C5D N4D C3D 111.8(7) . . ?
C20D N4D Co1D 110.5(6) . . ?
C5D N4D Co1D 102.4(5) . . ?
C3D N4D Co1D 108.6(5) . . ?
N4D C5D C6D 113.2(8) . . ?
N4D C5D H55 108.9 . . ?
C6D C5D H55 108.9 . . ?
N4D C5D H56 108.9 . . ?
C6D C5D H56 108.9 . . ?
H55 C5D H56 107.8 . . ?
N7D C6D C5D 109.4(8) . . ?
N7D C6D H65 109.8 . . ?
C5D C6D H65 109.8 . . ?
N7D C6D H66 109.8 . . ?
C5D C6D H66 109.8 . . ?
H65 C6D H66 108.2 . . ?
C8D N7D C30D 110.5(7) . . ?
C8D N7D C6D 110.9(7) . . ?
C30D N7D C6D 111.2(7) . . ?
C8D N7D Co1D 104.4(5) . . ?
C30D N7D Co1D 109.0(6) . . ?
C6D N7D Co1D 110.6(6) . . ?
N7D C8D C9D 112.2(8) . . ?
N7D C8D H85 109.2 . . ?
C9D C8D H85 109.2 . . ?
N7D C8D H86 109.2 . . ?
C9D C8D H86 109.2 . . ?
H85 C8D H86 107.9 . . ?
C8D C9D N1D 109.7(7) . . ?
C8D C9D H95 109.7 . . ?
N1D C9D H95 109.7 . . ?
C8D C9D H96 109.7 . . ?
N1D C9D H96 109.7 . . ?
H95 C9D H96 108.2 . . ?
N1D C10D P1D 111.9(6) . . ?
N1D C10D H105 109.2 . . ?
P1D C10D H105 109.2 . . ?
N1D C10D H106 109.2 . . ?
P1D C10D H106 109.2 . . ?
H105 C10D H106 107.9 . . ?
O1E P1D O1D 115.9(4) . . ?
O1E P1D C10D 110.3(4) . . ?
O1D P1D C10D 105.2(4) . . ?
O1E P1D C11D 108.7(4) . . ?
O1D P1D C11D 107.1(4) . . ?
C10D P1D C11D 109.3(4) . . ?
P1D O1D Co1D 114.5(4) . . ?
P1D O1D Na3 130.6(4) . . ?
Co1D O1D Na3 112.0(3) . . ?
P1D O1D Na1 81.2(3) . . ?
Co1D O1D Na1 91.3(2) . . ?
Na3 O1D Na1 82.1(2) . . ?
P1D O1E Na1 102.8(3) . . ?
C12D C11D P1D 117.7(7) . . ?
C12D C11D H115 107.9 . . ?
P1D C11D H115 107.9 . . ?
C12D C11D H116 107.9 . . ?
P1D C11D H116 107.9 . . ?
H115 C11D H116 107.2 . . ?
F1F C12D F1D 106.9(8) . . ?
F1F C12D F1E 106.2(8) . . ?
F1D C12D F1E 104.2(10) . . ?
F1F C12D C11D 113.4(10) . . ?
F1D C12D C11D 112.7(8) . . ?
F1E C12D C11D 112.8(8) . . ?
N4D C20D P2D 111.5(6) . . ?
N4D C20D H205 109.3 . . ?
P2D C20D H205 109.3 . . ?
N4D C20D H206 109.3 . . ?
P2D C20D H206 109.3 . . ?
H205 C20D H206 108.0 . . ?
O2E P2D O2D 118.0(4) . . ?
O2E P2D C20D 107.8(4) . . ?
O2D P2D C20D 106.8(4) . . ?
O2E P2D C21D 103.9(4) . . ?
O2D P2D C21D 109.8(4) . . ?
C20D P2D C21D 110.5(5) . . ?
P2D O2D Co1D 113.5(4) . . ?
P2D O2D Na2 126.4(4) . . ?
Co1D O2D Na2 119.5(3) . . ?
P2D O2D Na3 77.9(3) . . ?
Co1D O2D Na3 91.0(2) . . ?
Na2 O2D Na3 93.7(2) . . ?
P2D O2E Na3 106.4(4) . . ?
C22D C21D P2D 121.1(8) . . ?
C22D C21D H215 107.0 . . ?
P2D C21D H215 107.0 . . ?
C22D C21D H216 107.0 . . ?
P2D C21D H216 107.0 . . ?
H215 C21D H216 106.8 . . ?
F2F C22D F2E 106.3(10) . . ?
F2F C22D F2D 104.7(9) . . ?
F2E C22D F2D 105.5(11) . . ?
F2F C22D C21D 112.9(11) . . ?
F2E C22D C21D 112.9(10) . . ?
F2D C22D C21D 113.8(10) . . ?
N7D C30D P3D 110.4(6) . . ?
N7D C30D H305 109.6 . . ?
P3D C30D H305 109.6 . . ?
N7D C30D H306 109.6 . . ?
P3D C30D H306 109.6 . . ?
H305 C30D H306 108.1 . . ?
O3E P3D O3D 117.9(4) . . ?
O3E P3D C31D 110.8(4) . . ?
O3D P3D C31D 105.4(4) . . ?
O3E P3D C30D 109.5(4) . . ?
O3D P3D C30D 105.4(4) . . ?
C31D P3D C30D 107.4(5) . . ?
P3D O3D Co1D 113.7(4) . . ?
P3D O3D Na1 127.7(4) . . ?
Co1D O3D Na1 110.6(3) . . ?
P3D O3E Na2 119.0(4) . . ?
C32D C31D P3D 114.5(7) . . ?
C32D C31D H315 108.6 . . ?
P3D C31D H315 108.6 . . ?
C32D C31D H316 108.6 . . ?
P3D C31D H316 108.6 . . ?
H315 C31D H316 107.6 . . ?
F3D C32D F3E 106.5(9) . . ?
F3D C32D F3F 106.1(10) . . ?
F3E C32D F3F 105.2(9) . . ?
F3D C32D C31D 113.2(9) . . ?
F3E C32D C31D 114.6(10) . . ?
F3F C32D C31D 110.7(9) . . ?
O3D Na1 O1E 97.7(3) . . ?
O3D Na1 O1A 146.3(3) . . ?
O1E Na1 O1A 89.9(3) . . ?
O3D Na1 O2B 93.7(3) . . ?
O1E Na1 O2B 133.5(3) . . ?
O1A Na1 O2B 104.8(3) . . ?
O3D Na1 O2A 97.7(2) . . ?
O1E Na1 O2A 158.5(3) . . ?
O1A Na1 O2A 69.1(2) . . ?
O2B Na1 O2A 60.0(2) . . ?
O3D Na1 O1D 68.3(2) . . ?
O1E Na1 O1D 57.9(2) . . ?
O1A Na1 O1D 88.8(2) . . ?
O2B Na1 O1D 161.1(3) . . ?
O2A Na1 O1D 115.1(2) . . ?
O3B Na2 O3E 173.3(3) . . ?
O3B Na2 O2S 93.1(3) . . ?
O3E Na2 O2S 81.1(3) . . ?
O3B Na2 O2D 88.6(3) . . ?
O3E Na2 O2D 94.2(3) . . ?
O2S Na2 O2D 145.3(4) . . ?
O3B Na2 O2A 94.2(3) . . ?
O3E Na2 O2A 90.4(3) . . ?
O2S Na2 O2A 103.2(4) . . ?
O2D Na2 O2A 111.2(2) . . ?
O2E Na3 O3A 94.7(3) . . ?
O2E Na3 O1B 135.7(3) . . ?
O3A Na3 O1B 99.9(3) . . ?
O2E Na3 O1D 99.8(3) . . ?
O3A Na3 O1D 143.2(3) . . ?
O1B Na3 O1D 93.0(2) . . ?
O2E Na3 O1A 161.5(3) . . ?
O3A Na3 O1A 69.0(2) . . ?
O1B Na3 O1A 58.9(2) . . ?
O1D Na3 O1A 89.4(2) . . ?
O2E Na3 O2D 56.3(2) . . ?
O3A Na3 O2D 93.9(2) . . ?
O1B Na3 O2D 160.0(3) . . ?
O1D Na3 O2D 67.5(2) . . ?
O1A Na3 O2D 114.3(2) . . ?
C2S C1S H1S1 109.5 . . ?
C2S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
C2S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
O2S C2S C1S 122.5(17) . . ?
O2S C2S C3S 123.6(15) . . ?
C1S C2S C3S 113.8(16) . . ?
C2S O2S Na2 134.3(11) . . ?
C2S C3S H3S1 109.5 . . ?
C2S C3S H3S2 109.5 . . ?
H3S1 C3S H3S2 109.5 . . ?
C2S C3S H3S3 109.5 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?
C2T C1T H1T1 109.5 . . ?
C2T C1T H1T2 109.5 . . ?
H1T1 C1T H1T2 109.5 . . ?
C2T C1T H1T3 109.5 . . ?
H1T1 C1T H1T3 109.5 . . ?
H1T2 C1T H1T3 109.5 . . ?
O2T C2T C1T 124.4(17) . . ?
O2T C2T C3T 120.0(16) . . ?
C1T C2T C3T 115.6(15) . . ?
C2T C3T H3T1 109.5 . . ?
C2T C3T H3T2 109.5 . . ?
H3T1 C3T H3T2 109.5 . . ?
C2T C3T H3T3 109.5 . . ?
H3T1 C3T H3T3 109.5 . . ?
H3T2 C3T H3T3 109.5 . . ?
C2U C1U H1U1 107.1 . . ?
C2U C1U H1U2 112.4 . . ?
H1U1 C1U H1U2 109.5 . . ?
C2U C1U H1U3 108.9 . . ?
H1U1 C1U H1U3 109.5 . . ?
H1U2 C1U H1U3 109.5 . . ?
O2U C2U C1U 119(3) . . ?
O2U C2U C3U 136(4) . . ?
C1U C2U C3U 104(3) . . ?
C2U C3U H3U1 113.8 . . ?
C2U C3U H3U2 113.0 . . ?
H3U1 C3U H3U2 109.5 . . ?
C2U C3U H3U3 101.3 . . ?
H3U1 C3U H3U3 109.5 . . ?
H3U2 C3U H3U3 109.5 . . ?
C2V C1V H1V1 112.2 . . ?
C2V C1V H1V2 109.9 . . ?
H1V1 C1V H1V2 109.5 . . ?
C2V C1V H1V3 106.3 . . ?
H1V1 C1V H1V3 109.5 . . ?
H1V2 C1V H1V3 109.5 . . ?
O2V C2V C1V 122(4) . . ?
O2V C2V C3V 125(4) . . ?
C1V C2V C3V 112(3) . . ?
C2V C3V H3V1 112.7 . . ?
C2V C3V H3V2 109.4 . . ?
H3V1 C3V H3V2 109.5 . . ?
C2V C3V H3V3 106.3 . . ?
H3V1 C3V H3V3 109.5 . . ?
H3V2 C3V H3V3 109.5 . . ?

_refine_diff_density_max         1.116
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.165

####################################################################### 
# 
# 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_cunotptfe
_database_code_depnum_ccdc_archive 'CCDC 2327153'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2024-01-20 deposited with the CCDC.	2024-03-26 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         'C15 H24 Cu F9 N3 O6 P3, 3.5(H2 O), H4 N'
_chemical_formula_sum            'C15 H35 Cu F9 N4 O9.50 P3'
_chemical_formula_weight         750.92

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'
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      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                   25.5776(10)
_cell_length_b                   9.4016(3)
_cell_length_c                   24.4262(8)
_cell_angle_alpha                90
_cell_angle_beta                 101.0720(10)
_cell_angle_gamma                90
_cell_volume                     5764.4(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9866
_cell_measurement_theta_min      2.4101
_cell_measurement_theta_max      27.4673

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_F_000             3072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.270
_exptl_absorpt_coefficient_mu    1.035
_shelx_estimated_absorpt_T_min   0.737
_shelx_estimated_absorpt_T_max   0.768
_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  0.65
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180(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            22140
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.410
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6568
_reflns_number_gt                6169
_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 vV6.2.14'
_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    ?
_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)+(0.0401P)²+6.5614P] 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         6568
_refine_ls_number_parameters     484
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0753
_refine_ls_wR_factor_gt          0.0739
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.061
_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 0.35849(2) 0.46887(2) 0.64421(2) 0.02083(6) Uani 1 1 d . . . . .
N1 N 0.41233(6) 0.40171(14) 0.58603(5) 0.0294(3) Uani 1 1 d . . . . .
C2 C 0.37225(8) 0.34380(19) 0.53992(7) 0.0369(4) Uani 1 1 d . . . . .
H21 H 0.3904 0.2903 0.5141 0.044 Uiso 1 1 calc R U . . .
H22 H 0.3523 0.4231 0.5189 0.044 Uiso 1 1 calc R U . . .
C3 C 0.33331(8) 0.24535(18) 0.56177(7) 0.0372(4) Uani 1 1 d . . . . .
H31 H 0.3032 0.2239 0.5308 0.045 Uiso 1 1 calc R U . . .
H32 H 0.3516 0.1546 0.5736 0.045 Uiso 1 1 calc R U . . .
N4 N 0.31144(5) 0.30494(13) 0.60976(5) 0.0279(3) Uani 1 1 d . . . . .
C5 C 0.31384(7) 0.19871(16) 0.65541(7) 0.0319(3) Uani 1 1 d . . . . .
H51 H 0.2969 0.1088 0.6401 0.038 Uiso 1 1 calc R U . . .
H52 H 0.2941 0.2349 0.6836 0.038 Uiso 1 1 calc R U . . .
C6 C 0.37166(7) 0.17123(17) 0.68259(8) 0.0362(4) Uani 1 1 d . . . . .
H61 H 0.3730 0.1183 0.7179 0.043 Uiso 1 1 calc R U . . .
H62 H 0.3888 0.1119 0.6575 0.043 Uiso 1 1 calc R U . . .
N7 N 0.40164(5) 0.30843(15) 0.69441(6) 0.0301(3) Uani 1 1 d . . . . .
C8 C 0.45474(7) 0.29994(19) 0.67792(8) 0.0362(4) Uani 1 1 d . . . . .
H81 H 0.4736 0.2139 0.6947 0.043 Uiso 1 1 calc R U . . .
H82 H 0.4762 0.3840 0.6927 0.043 Uiso 1 1 calc R U . . .
C9 C 0.44980(8) 0.29414(19) 0.61486(8) 0.0380(4) Uani 1 1 d . . . . .
H91 H 0.4853 0.3098 0.6054 0.046 Uiso 1 1 calc R U . . .
H92 H 0.4374 0.1983 0.6014 0.046 Uiso 1 1 calc R U . . .
C10 C 0.43829(7) 0.53269(17) 0.57244(7) 0.0313(3) Uani 1 1 d . . . . .
H101 H 0.4138 0.5862 0.5434 0.038 Uiso 1 1 calc R U . . .
H102 H 0.4706 0.5087 0.5576 0.038 Uiso 1 1 calc R U . . .
P1 P 0.45661(2) 0.64312(4) 0.63531(2) 0.02239(9) Uani 1 1 d . . . . .
O11 O 0.41036(4) 0.62602(11) 0.66618(4) 0.0237(2) Uani 1 1 d . . . . .
O12 O 0.51106(4) 0.61022(13) 0.66702(5) 0.0326(3) Uani 1 1 d . . . . .
C11 C 0.45402(6) 0.82740(17) 0.61236(6) 0.0269(3) Uani 1 1 d . . . . .
H111 H 0.4184 0.8454 0.5892 0.032 Uiso 1 1 calc R U . . .
H112 H 0.4576 0.8893 0.6457 0.032 Uiso 1 1 calc R U . . .
C12 C 0.49527(8) 0.8707(2) 0.57980(8) 0.0419(4) Uani 1 1 d . . . . .
F121 F 0.49572(7) 0.78599(15) 0.53611(6) 0.0727(5) Uani 1 1 d . . . . .
F122 F 0.54431(5) 0.8706(2) 0.61044(8) 0.0820(5) Uani 1 1 d . . . . .
F123 F 0.48681(6) 1.00192(13) 0.55910(6) 0.0601(4) Uani 1 1 d . . . . .
C20 C 0.25600(7) 0.35867(17) 0.59224(7) 0.0319(3) Uani 1 1 d . . . . .
H201 H 0.2390 0.3680 0.6252 0.038 Uiso 1 1 calc R U . . .
H202 H 0.2348 0.2909 0.5659 0.038 Uiso 1 1 calc R U . . .
P2 P 0.25798(2) 0.53185(4) 0.55864(2) 0.02670(9) Uani 1 1 d . . . . .
O21 O 0.30959(4) 0.59537(11) 0.59141(5) 0.0291(2) Uani 1 1 d . . . . .
O22 O 0.25125(5) 0.52171(13) 0.49708(5) 0.0349(3) Uani 1 1 d . . . . .
C21 C 0.20520(7) 0.63752(19) 0.57892(7) 0.0347(4) Uani 1 1 d . . . . .
H211 H 0.2095 0.6333 0.6200 0.042 Uiso 1 1 calc R U . . .
H212 H 0.2103 0.7378 0.5688 0.042 Uiso 1 1 calc R U . . .
C22 C 0.14948(7) 0.5958(2) 0.55422(8) 0.0433(4) Uani 1 1 d . . . . .
F221 F 0.14118(6) 0.45637(17) 0.55748(9) 0.0809(5) Uani 1 1 d . . . . .
F222 F 0.13590(5) 0.6316(3) 0.50115(6) 0.0924(7) Uani 1 1 d . U . . .
F223 F 0.11361(5) 0.65766(19) 0.57956(6) 0.0695(4) Uani 1 1 d . . . . .
C30 C 0.40853(7) 0.3485(2) 0.75377(7) 0.0366(4) Uani 1 1 d . . . . .
H301 H 0.4343 0.4280 0.7615 0.044 Uiso 0.670(2) 1 calc R U P A 1
H302 H 0.4234 0.2667 0.7772 0.044 Uiso 0.670(2) 1 calc R U P A 1
H303 H 0.4378 0.4186 0.7629 0.044 Uiso 0.330(2) 1 calc R U P A 2
H304 H 0.4183 0.2633 0.7774 0.044 Uiso 0.330(2) 1 calc R U P A 2
P3A P 0.34884(7) 0.39908(17) 0.77122(8) 0.0205(2) Uani 0.670(2) 1 d . . P A 1
P3B P 0.33858(15) 0.4356(3) 0.77069(17) 0.0246(6) Uani 0.330(2) 1 d . . P A 2
O31 O 0.32070(5) 0.50457(13) 0.72400(5) 0.0334(3) Uani 1 1 d . . . . .
O32A O 0.31653(16) 0.2747(4) 0.78423(19) 0.0295(6) Uani 0.670(2) 1 d . . P A 1
C31A C 0.37450(10) 0.4928(4) 0.83610(10) 0.0279(5) Uani 0.670(2) 1 d . . P A 1
H311 H 0.3925 0.4231 0.8638 0.033 Uiso 0.670(2) 1 calc R U P A 1
H312 H 0.4017 0.5618 0.8292 0.033 Uiso 0.670(2) 1 calc R U P A 1
C32A C 0.33404(10) 0.5704(3) 0.86092(10) 0.0311(5) Uani 0.670(2) 1 d . . P A 1
F321 F 0.30976(10) 0.6732(2) 0.82746(8) 0.0630(6) Uani 0.670(2) 1 d . . P A 1
F322 F 0.29531(9) 0.4879(2) 0.87228(11) 0.0552(6) Uani 0.670(2) 1 d . . P A 1
F323 F 0.35472(10) 0.6362(3) 0.90852(9) 0.0579(6) Uani 0.670(2) 1 d . . P A 1
O32B O 0.3057(3) 0.3168(7) 0.7881(4) 0.0309(14) Uani 0.330(2) 1 d . . P A 2
C31B C 0.3553(3) 0.5643(8) 0.8275(3) 0.0396(14) Uani 0.330(2) 1 d . . P A 2
H313 H 0.3846 0.6248 0.8196 0.048 Uiso 0.330(2) 1 calc R U P A 2
H314 H 0.3240 0.6268 0.8266 0.048 Uiso 0.330(2) 1 calc R U P A 2
C32B C 0.3708(4) 0.5104(8) 0.8834(3) 0.0572(18) Uani 0.330(2) 1 d . U P A 2
F324 F 0.4089(2) 0.4078(6) 0.88754(18) 0.0799(16) Uani 0.330(2) 1 d . U P A 2
F325 F 0.3320(3) 0.4539(6) 0.9049(2) 0.0800(18) Uani 0.330(2) 1 d . U P A 2
F326 F 0.3929(3) 0.6125(7) 0.9195(2) 0.095(2) Uani 0.330(2) 1 d . U P A 2
N1A N 0.29461(8) 0.7981(2) 0.70832(8) 0.0418(4) Uani 1 1 d . . . . .
H1A H 0.3119(9) 0.853(3) 0.7340(11) 0.047(6) Uiso 1 1 d . . . . .
H2A H 0.3062(11) 0.711(3) 0.7122(11) 0.066(8) Uiso 1 1 d . . . . .
H3A H 0.2581(12) 0.794(3) 0.7086(11) 0.065(8) Uiso 1 1 d . . . . .
H4A H 0.3007(10) 0.832(3) 0.6755(11) 0.053(7) Uiso 1 1 d . . . . .
O1W O 0.31607(5) 0.88451(14) 0.60086(5) 0.0321(3) Uani 1 1 d . . . . .
H11W H 0.3180(9) 0.803(3) 0.5937(10) 0.046(6) Uiso 1 1 d . . . . .
H12W H 0.2974(10) 0.913(3) 0.5760(11) 0.051(7) Uiso 1 1 d . . . . .
O2W O 0.57779(5) 0.79495(15) 0.73742(6) 0.0382(3) Uani 1 1 d . . . . .
H21W H 0.5590(10) 0.740(3) 0.7158(10) 0.044(6) Uiso 1 1 d . . . . .
H22W H 0.5823(10) 0.743(3) 0.7659(12) 0.057(7) Uiso 1 1 d . . . . .
O3W O 0.5000 1.0011(2) 0.7500 0.0527(6) Uani 1 2 d S T P . .
H31W H 0.4752(11) 0.951(3) 0.7503(14) 0.075(10) Uiso 1 1 d . . . . .
O4W O 0.33477(10) -0.0156(2) 0.79772(9) 0.0479(6) Uani 0.670(2) 1 d . . P A 1
H41W H 0.3323 0.0798 0.7952 0.057 Uiso 0.670(2) 1 d R U P A 1
H42W H 0.3705 -0.0417 0.8062 0.057 Uiso 0.670(2) 1 d R U P A 1
O4V O 0.29225(16) 0.0167(4) 0.78675(16) 0.0350(9) Uani 0.330(2) 1 d . . P A 2
H41V H 0.2960 0.1096 0.7898 0.042 Uiso 0.330(2) 1 d R U P A 2
H42V H 0.3089 -0.0294 0.8175 0.042 Uiso 0.330(2) 1 d R U 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
Cu1 O11 1.9894(10) . ?
Cu1 O21 2.0056(10) . ?
Cu1 N4 2.0353(13) . ?
Cu1 N7 2.1160(13) . ?
Cu1 N1 2.2510(14) . ?
Cu1 O31 2.3597(12) . ?
N1 C10 1.467(2) . ?
N1 C2 1.474(2) . ?
N1 C9 1.476(2) . ?
C2 C3 1.529(3) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.501(2) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C20 1.489(2) . ?
N4 C5 1.489(2) . ?
C5 C6 1.522(2) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.500(2) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C30 1.475(2) . ?
N7 C8 1.491(2) . ?
C8 C9 1.522(3) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
C10 P1 1.8384(17) . ?
C10 H101 0.9900 . ?
C10 H102 0.9900 . ?
P1 O12 1.4901(11) . ?
P1 O11 1.5286(11) . ?
P1 C11 1.8183(16) . ?
C11 C12 1.495(2) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 F122 1.332(3) . ?
C12 F121 1.333(2) . ?
C12 F123 1.335(2) . ?
C20 P2 1.8284(17) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P2 O22 1.4834(13) . ?
P2 O21 1.5278(11) . ?
P2 C21 1.8197(18) . ?
C21 C22 1.490(2) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
C22 F222 1.320(2) . ?
C22 F221 1.333(3) . ?
C22 F223 1.334(2) . ?
C30 P3A 1.729(3) . ?
C30 P3B 2.080(4) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C30 H303 0.9900 . ?
C30 H304 0.9900 . ?
P3A O32A 1.501(5) . ?
P3A O31 1.585(2) . ?
P3A C31A 1.822(3) . ?
P3B O31 1.315(4) . ?
P3B O32B 1.508(9) . ?
P3B C31B 1.829(7) . ?
C31A C32A 1.487(4) . ?
C31A H311 0.9900 . ?
C31A H312 0.9900 . ?
C32A F322 1.328(3) . ?
C32A F323 1.334(3) . ?
C32A F321 1.339(3) . ?
C31B C32B 1.438(11) . ?
C31B H313 0.9900 . ?
C31B H314 0.9900 . ?
C32B F325 1.323(8) . ?
C32B F326 1.352(8) . ?
C32B F324 1.360(10) . ?
N1A H1A 0.87(3) . ?
N1A H2A 0.87(3) . ?
N1A H3A 0.94(3) . ?
N1A H4A 0.90(3) . ?
O1W H11W 0.79(3) . ?
O1W H12W 0.75(3) . ?
O2W H21W 0.82(3) . ?
O2W H22W 0.84(3) . ?
O3W H31W 0.79(3) . ?
O4W H41W 0.9011 . ?
O4W H42W 0.9312 . ?
O4V H41V 0.8799 . ?
O4V H42V 0.9008 . ?

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 Cu1 O21 91.97(4) . . ?
O11 Cu1 N4 169.93(5) . . ?
O21 Cu1 N4 86.39(5) . . ?
O11 Cu1 N7 97.26(5) . . ?
O21 Cu1 N7 170.69(5) . . ?
N4 Cu1 N7 84.32(5) . . ?
O11 Cu1 N1 85.50(5) . . ?
O21 Cu1 N1 98.16(5) . . ?
N4 Cu1 N1 84.91(5) . . ?
N7 Cu1 N1 81.46(5) . . ?
O11 Cu1 O31 91.68(4) . . ?
O21 Cu1 O31 98.22(5) . . ?
N4 Cu1 O31 98.38(5) . . ?
N7 Cu1 O31 82.74(5) . . ?
N1 Cu1 O31 163.46(5) . . ?
C10 N1 C2 114.57(13) . . ?
C10 N1 C9 113.73(14) . . ?
C2 N1 C9 113.84(14) . . ?
C10 N1 Cu1 105.41(9) . . ?
C2 N1 Cu1 99.56(10) . . ?
C9 N1 Cu1 108.12(10) . . ?
N1 C2 C3 111.16(14) . . ?
N1 C2 H21 109.4 . . ?
C3 C2 H21 109.4 . . ?
N1 C2 H22 109.4 . . ?
C3 C2 H22 109.4 . . ?
H21 C2 H22 108.0 . . ?
N4 C3 C2 114.34(13) . . ?
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 . . ?
C20 N4 C5 110.04(13) . . ?
C20 N4 C3 112.30(13) . . ?
C5 N4 C3 111.50(13) . . ?
C20 N4 Cu1 108.47(9) . . ?
C5 N4 Cu1 105.20(9) . . ?
C3 N4 Cu1 109.04(10) . . ?
N4 C5 C6 109.70(14) . . ?
N4 C5 H51 109.7 . . ?
C6 C5 H51 109.7 . . ?
N4 C5 H52 109.7 . . ?
C6 C5 H52 109.7 . . ?
H51 C5 H52 108.2 . . ?
N7 C6 C5 110.85(13) . . ?
N7 C6 H61 109.5 . . ?
C5 C6 H61 109.5 . . ?
N7 C6 H62 109.5 . . ?
C5 C6 H62 109.5 . . ?
H61 C6 H62 108.1 . . ?
C30 N7 C8 109.64(13) . . ?
C30 N7 C6 111.63(13) . . ?
C8 N7 C6 111.13(14) . . ?
C30 N7 Cu1 109.77(11) . . ?
C8 N7 Cu1 106.41(10) . . ?
C6 N7 Cu1 108.12(9) . . ?
N7 C8 C9 111.88(13) . . ?
N7 C8 H81 109.2 . . ?
C9 C8 H81 109.2 . . ?
N7 C8 H82 109.2 . . ?
C9 C8 H82 109.2 . . ?
H81 C8 H82 107.9 . . ?
N1 C9 C8 112.23(14) . . ?
N1 C9 H91 109.2 . . ?
C8 C9 H91 109.2 . . ?
N1 C9 H92 109.2 . . ?
C8 C9 H92 109.2 . . ?
H91 C9 H92 107.9 . . ?
N1 C10 P1 109.81(11) . . ?
N1 C10 H101 109.7 . . ?
P1 C10 H101 109.7 . . ?
N1 C10 H102 109.7 . . ?
P1 C10 H102 109.7 . . ?
H101 C10 H102 108.2 . . ?
O12 P1 O11 117.15(6) . . ?
O12 P1 C11 109.46(7) . . ?
O11 P1 C11 105.45(7) . . ?
O12 P1 C10 112.32(8) . . ?
O11 P1 C10 104.80(7) . . ?
C11 P1 C10 106.99(7) . . ?
P1 O11 Cu1 118.96(6) . . ?
C12 C11 P1 115.83(12) . . ?
C12 C11 H111 108.3 . . ?
P1 C11 H111 108.3 . . ?
C12 C11 H112 108.3 . . ?
P1 C11 H112 108.3 . . ?
H111 C11 H112 107.4 . . ?
F122 C12 F121 107.32(19) . . ?
F122 C12 F123 106.26(18) . . ?
F121 C12 F123 105.93(16) . . ?
F122 C12 C11 112.69(16) . . ?
F121 C12 C11 112.26(17) . . ?
F123 C12 C11 111.92(16) . . ?
N4 C20 P2 108.92(11) . . ?
N4 C20 H201 109.9 . . ?
P2 C20 H201 109.9 . . ?
N4 C20 H202 109.9 . . ?
P2 C20 H202 109.9 . . ?
H201 C20 H202 108.3 . . ?
O22 P2 O21 118.45(8) . . ?
O22 P2 C21 111.31(8) . . ?
O21 P2 C21 104.80(7) . . ?
O22 P2 C20 112.95(8) . . ?
O21 P2 C20 102.04(6) . . ?
C21 P2 C20 106.15(9) . . ?
P2 O21 Cu1 118.32(6) . . ?
C22 C21 P2 116.63(14) . . ?
C22 C21 H211 108.1 . . ?
P2 C21 H211 108.1 . . ?
C22 C21 H212 108.1 . . ?
P2 C21 H212 108.1 . . ?
H211 C21 H212 107.3 . . ?
F222 C22 F221 107.1(2) . . ?
F222 C22 F223 105.67(17) . . ?
F221 C22 F223 105.62(18) . . ?
F222 C22 C21 112.45(17) . . ?
F221 C22 C21 112.67(17) . . ?
F223 C22 C21 112.77(17) . . ?
N7 C30 P3A 111.59(13) . . ?
N7 C30 P3B 110.53(16) . . ?
N7 C30 H301 109.3 . . ?
P3A C30 H301 109.3 . . ?
N7 C30 H302 109.3 . . ?
P3A C30 H302 109.3 . . ?
H301 C30 H302 108.0 . . ?
N7 C30 H303 109.5 . . ?
P3B C30 H303 109.5 . . ?
N7 C30 H304 109.5 . . ?
P3B C30 H304 109.5 . . ?
H303 C30 H304 108.1 . . ?
O32A P3A O31 116.7(2) . . ?
O32A P3A C30 112.70(14) . . ?
O31 P3A C30 106.97(13) . . ?
O32A P3A C31A 108.3(2) . . ?
O31 P3A C31A 111.57(14) . . ?
C30 P3A C31A 99.21(14) . . ?
O31 P3B O32B 119.3(4) . . ?
O31 P3B C31B 108.9(3) . . ?
O32B P3B C31B 109.7(4) . . ?
O31 P3B C30 101.0(2) . . ?
O32B P3B C30 108.2(3) . . ?
C31B P3B C30 109.1(3) . . ?
P3B O31 Cu1 121.11(16) . . ?
P3A O31 Cu1 108.13(9) . . ?
C32A C31A P3A 115.42(19) . . ?
C32A C31A H311 108.4 . . ?
P3A C31A H311 108.4 . . ?
C32A C31A H312 108.4 . . ?
P3A C31A H312 108.4 . . ?
H311 C31A H312 107.5 . . ?
F322 C32A F323 106.0(2) . . ?
F322 C32A F321 105.8(2) . . ?
F323 C32A F321 104.9(2) . . ?
F322 C32A C31A 113.9(2) . . ?
F323 C32A C31A 113.1(2) . . ?
F321 C32A C31A 112.5(2) . . ?
C32B C31B P3B 117.9(6) . . ?
C32B C31B H313 107.8 . . ?
P3B C31B H313 107.8 . . ?
C32B C31B H314 107.8 . . ?
P3B C31B H314 107.8 . . ?
H313 C31B H314 107.2 . . ?
F325 C32B F326 106.0(6) . . ?
F325 C32B F324 105.5(7) . . ?
F326 C32B F324 104.6(7) . . ?
F325 C32B C31B 115.3(7) . . ?
F326 C32B C31B 112.0(6) . . ?
F324 C32B C31B 112.7(6) . . ?
H1A N1A H2A 111(2) . . ?
H1A N1A H3A 113(2) . . ?
H2A N1A H3A 106(2) . . ?
H1A N1A H4A 106(2) . . ?
H2A N1A H4A 108(2) . . ?
H3A N1A H4A 111(2) . . ?
H11W O1W H12W 103(3) . . ?
H21W O2W H22W 98(2) . . ?
H41W O4W H42W 109.3 . . ?
H41V O4V H42V 112.4 . . ?

_refine_diff_density_max         0.446
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.051

####################################################################### 
# 
# 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_conotpf2
_database_code_depnum_ccdc_archive 'CCDC 2327158'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2024-01-20 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
2(C15 H24 Co F9 N3 O6 P3), Co H12 O6, 0.75(C H4 O), 14.25(H2 O)
;
_chemical_formula_sum            'C30.75 H91.50 Co3 F18 N6 O33 P6'
_chemical_formula_weight         1778.20

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'
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'
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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   34.3841(8)
_cell_length_b                   34.3841(8)
_cell_length_c                   40.9610(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     41939(2)
_cell_formula_units_Z            24
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9941
_cell_measurement_theta_min      2.5158
_cell_measurement_theta_max      27.4618

_exptl_crystal_description       prism
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_F_000             21960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.137
_exptl_absorpt_coefficient_mu    0.974
_shelx_estimated_absorpt_T_min   0.779
_shelx_estimated_absorpt_T_max   0.878
_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  0.82
_exptl_absorpt_correction_T_max  0.88
_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            88634
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_theta_min         1.905
_diffrn_reflns_theta_max         27.492
_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             21382
_reflns_number_gt                15240
_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-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_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)+(0.0369P)²+115.5219P] 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         21382
_refine_ls_number_parameters     1156
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.1024
_refine_ls_wR_factor_gt          0.0877
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.004
_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 0.49584(2) 0.49775(2) 0.87318(2) 0.01124(7) Uani 1 1 d . . . . .
N1A N 0.52413(6) 0.47473(6) 0.91066(4) 0.0142(3) Uani 1 1 d . . . . .
C2A C 0.55688(7) 0.51640(7) 0.92792(5) 0.0169(4) Uani 1 1 d . . . . .
H2A H 0.583154 0.534134 0.913626 0.020 Uiso 1 1 calc R U . . .
H2B H 0.567556 0.508336 0.947856 0.020 Uiso 1 1 calc R U . . .
C3A C 0.53616(7) 0.54481(7) 0.93730(5) 0.0182(4) Uani 1 1 d . . . . .
H3A H 0.515439 0.530653 0.955927 0.022 Uiso 1 1 calc R U . . .
H3B H 0.560145 0.574916 0.944296 0.022 Uiso 1 1 calc R U . . .
N4A N 0.51111(6) 0.54958(6) 0.90937(4) 0.0141(3) Uani 1 1 d . . . . .
C5A C 0.46589(7) 0.54110(7) 0.91922(5) 0.0180(4) Uani 1 1 d . . . . .
H5A H 0.452147 0.548603 0.900817 0.022 Uiso 1 1 calc R U . . .
H5B H 0.468997 0.560873 0.937805 0.022 Uiso 1 1 calc R U . . .
C6A C 0.43513(7) 0.49215(7) 0.92909(5) 0.0172(4) Uani 1 1 d . . . . .
H6A H 0.444965 0.486445 0.950383 0.021 Uiso 1 1 calc R U . . .
H6B H 0.404003 0.486273 0.931574 0.021 Uiso 1 1 calc R U . . .
N7A N 0.43621(6) 0.46129(6) 0.90394(4) 0.0144(3) Uani 1 1 d . . . . .
C8A C 0.44198(7) 0.42494(7) 0.91838(5) 0.0165(4) Uani 1 1 d . . . . .
H8A H 0.437188 0.402684 0.901233 0.020 Uiso 1 1 calc R U . . .
H8B H 0.418936 0.409436 0.935481 0.020 Uiso 1 1 calc R U . . .
C9A C 0.48861(7) 0.44262(7) 0.93335(5) 0.0171(4) Uani 1 1 d . . . . .
H9A H 0.490466 0.457914 0.954260 0.020 Uiso 1 1 calc R U . . .
H9B H 0.493555 0.417162 0.937969 0.020 Uiso 1 1 calc R U . . .
C10A C 0.54764(7) 0.45402(7) 0.89415(5) 0.0156(4) Uani 1 1 d . . . . .
H10A H 0.525474 0.423601 0.886332 0.019 Uiso 1 1 calc R U . . .
H10B H 0.568084 0.451157 0.909724 0.019 Uiso 1 1 calc R U . . .
P1A P 0.57994(2) 0.48927(2) 0.85945(2) 0.01298(11) Uani 1 1 d . . . . .
O1A O 0.55459(5) 0.51276(5) 0.84844(3) 0.0157(3) Uani 1 1 d . . . . .
O1B O 0.62842(5) 0.51869(5) 0.86855(4) 0.0190(3) Uani 1 1 d . . . . .
C11A C 0.57310(7) 0.45069(7) 0.82674(5) 0.0176(4) Uani 1 1 d . . . . .
H11A H 0.540624 0.429180 0.824036 0.021 Uiso 1 1 calc R U . . .
H11B H 0.583923 0.468050 0.806205 0.021 Uiso 1 1 calc R U . . .
C12A C 0.59665(8) 0.42464(8) 0.83122(6) 0.0238(5) Uani 1 1 d . . . . .
F1A F 0.58877(6) 0.40523(5) 0.86107(4) 0.0379(4) Uani 1 1 d . . . . .
F1B F 0.64109(5) 0.44951(5) 0.82804(4) 0.0427(4) Uani 1 1 d . . . . .
F1C F 0.58292(5) 0.39102(5) 0.80970(3) 0.0314(3) Uani 1 1 d . . . . .
C20A C 0.53689(7) 0.59430(7) 0.89383(5) 0.0157(4) Uani 1 1 d . . . . .
H20A H 0.568812 0.602611 0.891724 0.019 Uiso 1 1 calc R U . . .
H20B H 0.535321 0.617180 0.907551 0.019 Uiso 1 1 calc R U . . .
P2A P 0.51327(2) 0.59268(2) 0.85320(2) 0.01442(11) Uani 1 1 d . . . . .
O2A O 0.49113(5) 0.54401(5) 0.84235(3) 0.0171(3) Uani 1 1 d . . . . .
O2B O 0.48358(5) 0.61291(6) 0.85294(4) 0.0259(4) Uani 1 1 d . . . . .
C21A C 0.56151(7) 0.62479(7) 0.82677(5) 0.0204(5) Uani 1 1 d . . . . .
H21A H 0.583194 0.614195 0.830219 0.024 Uiso 1 1 calc R U . . .
H21B H 0.551346 0.618388 0.803783 0.024 Uiso 1 1 calc R U . . .
C22A C 0.58529(8) 0.67440(8) 0.83186(6) 0.0269(5) Uani 1 1 d . . . . .
F2A F 0.59525(6) 0.68567(5) 0.86358(3) 0.0396(4) Uani 1 1 d . . . . .
F2B F 0.56140(6) 0.69314(5) 0.82189(4) 0.0421(4) Uani 1 1 d . . . . .
F2C F 0.62441(5) 0.69567(5) 0.81571(4) 0.0373(4) Uani 1 1 d . . . . .
C30A C 0.39534(7) 0.44137(7) 0.88325(5) 0.0158(4) Uani 1 1 d . . . . .
H30A H 0.387245 0.464498 0.877847 0.019 Uiso 1 1 calc R U . . .
H30B H 0.369920 0.416814 0.895243 0.019 Uiso 1 1 calc R U . . .
P3A P 0.40607(2) 0.41928(2) 0.84551(2) 0.01274(11) Uani 1 1 d . . . . .
O3A O 0.45649(5) 0.44765(5) 0.84019(3) 0.0156(3) Uani 1 1 d . . . . .
O3B O 0.38768(5) 0.36956(5) 0.84637(3) 0.0183(3) Uani 1 1 d . . . . .
C31A C 0.37931(7) 0.43347(7) 0.81319(5) 0.0166(4) Uani 1 1 d . . . . .
H31A H 0.388813 0.465725 0.815083 0.020 Uiso 1 1 calc R U . . .
H31B H 0.390370 0.429153 0.791951 0.020 Uiso 1 1 calc R U . . .
C32A C 0.32937(8) 0.40712(8) 0.81299(6) 0.0235(5) Uani 1 1 d . . . . .
F3A F 0.31130(5) 0.40604(5) 0.84242(4) 0.0348(3) Uani 1 1 d . . . . .
F3B F 0.31303(5) 0.36419(4) 0.80406(4) 0.0324(3) Uani 1 1 d . . . . .
F3C F 0.31186(5) 0.42458(5) 0.79217(4) 0.0343(3) Uani 1 1 d . . . . .
Co1D Co 0.49690(2) 0.49623(2) 0.62634(2) 0.01149(7) Uani 1 1 d . . . . .
N1D N 0.54916(6) 0.52680(6) 0.58967(4) 0.0139(3) Uani 1 1 d . . . . .
C2D C 0.53990(7) 0.55927(7) 0.57246(5) 0.0167(4) Uani 1 1 d . . . . .
H2D H 0.559289 0.570778 0.552884 0.020 Uiso 1 1 calc R U . . .
H2E H 0.547369 0.585058 0.587014 0.020 Uiso 1 1 calc R U . . .
C3D C 0.49095(7) 0.53777(7) 0.56218(5) 0.0174(4) Uani 1 1 d . . . . .
H3D H 0.484323 0.561400 0.555152 0.021 Uiso 1 1 calc R U . . .
H3E H 0.485375 0.517459 0.543434 0.021 Uiso 1 1 calc R U . . .
N4D N 0.46084(6) 0.51188(6) 0.58972(4) 0.0146(3) Uani 1 1 d . . . . .
C5D C 0.42487(7) 0.46676(7) 0.57929(5) 0.0176(4) Uani 1 1 d . . . . .
H5D H 0.408550 0.469940 0.560505 0.021 Uiso 1 1 calc R U . . .
H5E H 0.403171 0.452478 0.597376 0.021 Uiso 1 1 calc R U . . .
C6D C 0.44387(7) 0.43666(7) 0.56957(5) 0.0164(4) Uani 1 1 d . . . . .
H6D H 0.418940 0.405434 0.566799 0.020 Uiso 1 1 calc R U . . .
H6E H 0.459729 0.446909 0.548422 0.020 Uiso 1 1 calc R U . . .
N7D N 0.47561(6) 0.43775(6) 0.59486(4) 0.0139(3) Uani 1 1 d . . . . .
C8D C 0.51858(7) 0.44486(7) 0.58066(5) 0.0157(4) Uani 1 1 d . . . . .
H8D H 0.511860 0.422607 0.563090 0.019 Uiso 1 1 calc R U . . .
H8E H 0.535852 0.439748 0.597786 0.019 Uiso 1 1 calc R U . . .
C9D C 0.54725(7) 0.49209(7) 0.56675(5) 0.0164(4) Uani 1 1 d . . . . .
H9D H 0.578053 0.497820 0.562666 0.020 Uiso 1 1 calc R U . . .
H9E H 0.534461 0.494289 0.545633 0.020 Uiso 1 1 calc R U . . .
C10D C 0.59307(7) 0.55113(7) 0.60664(5) 0.0161(4) Uani 1 1 d . . . . .
H10D H 0.616363 0.572335 0.591379 0.019 Uiso 1 1 calc R U . . .
H10E H 0.602090 0.529519 0.614407 0.019 Uiso 1 1 calc R U . . .
P1D P 0.58803(2) 0.58203(2) 0.64148(2) 0.01375(11) Uani 1 1 d . . . . .
O1D O 0.53936(5) 0.55454(5) 0.65255(3) 0.0156(3) Uani 1 1 d . . . . .
O1E O 0.60453(5) 0.63030(5) 0.63296(4) 0.0190(3) Uani 1 1 d . . . . .
C11D C 0.62161(7) 0.57753(7) 0.67396(5) 0.0188(4) Uani 1 1 d . . . . .
H11D H 0.615389 0.588766 0.694417 0.023 Uiso 1 1 calc R U . . .
H11E H 0.611700 0.545371 0.677237 0.023 Uiso 1 1 calc R U . . .
C12D C 0.67107(8) 0.60227(8) 0.66833(6) 0.0262(5) Uani 1 1 d . . . . .
F1D F 0.68208(5) 0.59456(6) 0.63845(4) 0.0428(4) Uani 1 1 d . . . . .
F1E F 0.68963(5) 0.64667(5) 0.67152(5) 0.0483(5) Uani 1 1 d . . . . .
F1F F 0.69270(5) 0.58993(5) 0.68945(4) 0.0384(4) Uani 1 1 d . . . . .
C20D C 0.44150(7) 0.53708(7) 0.60543(5) 0.0180(4) Uani 1 1 d . . . . .
H20D H 0.417057 0.535429 0.591670 0.022 Uiso 1 1 calc R U . . .
H20E H 0.464922 0.569050 0.607662 0.022 Uiso 1 1 calc R U . . .
P2D P 0.41925(2) 0.51325(2) 0.64605(2) 0.01624(11) Uani 1 1 d . . . . .
O2D O 0.44306(5) 0.48765(5) 0.65557(3) 0.0182(3) Uani 1 1 d . . . . .
O2E O 0.36910(5) 0.48703(5) 0.64659(4) 0.0262(4) Uani 1 1 d . . . . .
C21D C 0.44021(8) 0.56107(7) 0.67344(5) 0.0219(5) Uani 1 1 d . . . . .
H21D H 0.435972 0.549940 0.696186 0.026 Uiso 1 1 calc R U . . .
H21E H 0.472898 0.580359 0.669767 0.026 Uiso 1 1 calc R U . . .
C22E C 0.41870(9) 0.58920(9) 0.66995(6) 0.0311(6) Uani 1 1 d . . . . .
F2D F 0.41844(7) 0.60151(6) 0.63870(4) 0.0511(5) Uani 1 1 d . . . . .
F2E F 0.37637(5) 0.56863(6) 0.67994(5) 0.0518(5) Uani 1 1 d . . . . .
F2F F 0.44001(6) 0.62732(5) 0.68705(5) 0.0517(5) Uani 1 1 d . . . . .
C30D C 0.45490(7) 0.39639(7) 0.61496(5) 0.0152(4) Uani 1 1 d . . . . .
H30D H 0.454388 0.371420 0.602562 0.018 Uiso 1 1 calc R U . . .
H30E H 0.423572 0.387859 0.620393 0.018 Uiso 1 1 calc R U . . .
P3D P 0.48759(2) 0.40653(2) 0.65262(2) 0.01289(11) Uani 1 1 d . . . . .
O3D O 0.50798(5) 0.45669(5) 0.65904(3) 0.0170(3) Uani 1 1 d . . . . .
O3E O 0.52055(5) 0.39023(5) 0.65064(4) 0.0205(3) Uani 1 1 d . . . . .
C31D C 0.44713(7) 0.37721(7) 0.68476(5) 0.0165(4) Uani 1 1 d . . . . .
H31D H 0.462443 0.387779 0.706075 0.020 Uiso 1 1 calc R U . . .
H31E H 0.423450 0.385538 0.683573 0.020 Uiso 1 1 calc R U . . .
C32D C 0.42523(7) 0.32724(7) 0.68373(5) 0.0218(5) Uani 1 1 d . . . . .
F3D F 0.40849(5) 0.31028(4) 0.65396(3) 0.0326(3) Uani 1 1 d . . . . .
F3E F 0.45299(5) 0.31194(5) 0.69173(4) 0.0327(3) Uani 1 1 d . . . . .
F3F F 0.39036(5) 0.30771(5) 0.70449(4) 0.0315(3) Uani 1 1 d . . . . .
Co1G Co 0.666667 0.333333 0.70986(2) 0.01195(10) Uani 1 3 d S T P . .
N1G N 0.68780(6) 0.38773(6) 0.74538(4) 0.0145(3) Uani 1 1 d . . . . .
C2G C 0.64491(7) 0.38067(7) 0.75945(5) 0.0163(4) Uani 1 1 d . . . . .
H2G H 0.628718 0.388049 0.742811 0.020 Uiso 1 1 calc R U . . .
H2H H 0.651480 0.401202 0.778202 0.020 Uiso 1 1 calc R U . . .
C3G C 0.61513(7) 0.33242(7) 0.77075(5) 0.0165(4) Uani 1 1 d . . . . .
H3G H 0.627489 0.327413 0.791127 0.020 Uiso 1 1 calc R U . . .
H3H H 0.584647 0.327162 0.775503 0.020 Uiso 1 1 calc R U . . .
C10G C 0.71104(7) 0.43132(7) 0.72789(5) 0.0160(4) Uani 1 1 d . . . . .
H10G H 0.742333 0.439253 0.722938 0.019 Uiso 1 1 calc R U . . .
H10H H 0.711873 0.455267 0.741813 0.019 Uiso 1 1 calc R U . . .
P1G P 0.68095(2) 0.42689(2) 0.68986(2) 0.01446(11) Uani 1 1 d . . . . .
O1G O 0.66043(5) 0.37827(5) 0.67919(3) 0.0175(3) Uani 1 1 d . . . . .
O1H O 0.64905(5) 0.44421(5) 0.69390(4) 0.0226(3) Uani 1 1 d . . . . .
C11G C 0.72444(8) 0.46018(7) 0.66018(5) 0.0216(5) Uani 1 1 d . . . . .
H11G H 0.747586 0.451110 0.660979 0.026 Uiso 1 1 calc R U . . .
H11H H 0.710911 0.452903 0.638106 0.026 Uiso 1 1 calc R U . . .
C12G C 0.74684(8) 0.50958(8) 0.66488(6) 0.0265(5) Uani 1 1 d . . . . .
F1G F 0.75894(6) 0.52192(5) 0.69621(3) 0.0395(4) Uani 1 1 d . . . . .
F1H F 0.72111(5) 0.52692(5) 0.65605(4) 0.0408(4) Uani 1 1 d . . . . .
F1I F 0.78487(5) 0.53169(5) 0.64741(4) 0.0382(4) Uani 1 1 d . . . . .
Co1J Co 0.666667 0.333333 0.45561(2) 0.01238(10) Uani 1 3 d S T P . .
N1J N 0.63493(6) 0.35600(7) 0.42057(4) 0.0214(4) Uani 1 1 d . . . . .
C2J C 0.59895(10) 0.31274(11) 0.40531(7) 0.0430(7) Uani 1 1 d . . . . .
H2J H 0.573871 0.297416 0.421004 0.052 Uiso 1 1 calc R U . . .
H2K H 0.587103 0.320162 0.385699 0.052 Uiso 1 1 calc R U . . .
C3J C 0.61456(11) 0.28158(9) 0.39586(7) 0.0435(8) Uani 1 1 d . . . . .
H3J H 0.588232 0.251307 0.392467 0.052 Uiso 1 1 calc R U . . .
H3K H 0.631003 0.291591 0.374904 0.052 Uiso 1 1 calc R U . . .
C10J C 0.61409(7) 0.37810(7) 0.43870(5) 0.0189(4) Uani 1 1 d . . . . .
H10J H 0.592273 0.380862 0.424535 0.023 Uiso 1 1 calc R U . . .
H10K H 0.637461 0.408629 0.445440 0.023 Uiso 1 1 calc R U . . .
P1J P 0.58548(2) 0.34447(2) 0.47477(2) 0.01946(12) Uani 1 1 d . . . . .
O1J O 0.61189(5) 0.32184(5) 0.48495(3) 0.0196(3) Uani 1 1 d . . . . .
O1K O 0.53665(6) 0.31434(7) 0.46820(5) 0.0410(5) Uani 1 1 d . . . . .
C11J C 0.59412(9) 0.38430(9) 0.50695(6) 0.0314(6) Uani 1 1 d . . . . .
H11J H 0.584318 0.367778 0.527881 0.038 Uiso 1 1 calc R U . . .
H11K H 0.626703 0.405895 0.508708 0.038 Uiso 1 1 calc R U . . .
C12J C 0.57021(11) 0.41015(11) 0.50253(7) 0.0429(7) Uani 1 1 d . . . . .
F1J F 0.57734(7) 0.42870(7) 0.47255(4) 0.0556(5) Uani 1 1 d . . . . .
F1K F 0.52593(7) 0.38523(8) 0.50669(5) 0.0698(6) Uani 1 1 d . . . . .
F1L F 0.58437(7) 0.44418(7) 0.52344(4) 0.0614(6) Uani 1 1 d . . . . .
Co2A Co 0.50360(2) 0.50156(2) 0.74988(2) 0.01268(7) Uani 1 1 d . . . . .
O1W O 0.55660(5) 0.53474(5) 0.78278(3) 0.0224(3) Uani 1 1 d . . . . .
H1W H 0.554763 0.527140 0.801323 0.034 Uiso 1 1 d R U . . .
H1V H 0.582950 0.556237 0.778919 0.034 Uiso 1 1 d R U . . .
O2W O 0.46830(5) 0.52422(5) 0.77762(3) 0.0207(3) Uani 1 1 d . . . . .
H2W H 0.472660 0.526989 0.798330 0.031 Uiso 1 1 d R U . . .
H2V H 0.443154 0.519495 0.773537 0.031 Uiso 1 1 d R U . . .
O3W O 0.48054(5) 0.44330(5) 0.77761(3) 0.0204(3) Uani 1 1 d . . . . .
H3W H 0.475330 0.444342 0.798898 0.031 Uiso 1 1 d R U . . .
H3V H 0.486331 0.423542 0.772194 0.031 Uiso 1 1 d R U . . .
O4W O 0.52519(5) 0.55743(5) 0.71918(3) 0.0217(3) Uani 1 1 d . . . . .
H4W H 0.528293 0.554701 0.698626 0.033 Uiso 1 1 d R U . . .
H4V H 0.524495 0.581398 0.722813 0.033 Uiso 1 1 d R U . . .
O5W O 0.44608(5) 0.46701(5) 0.72093(3) 0.0190(3) Uani 1 1 d . . . . .
H5W H 0.445583 0.472044 0.699240 0.028 Uiso 1 1 d R U . . .
H5V H 0.424783 0.440741 0.726534 0.028 Uiso 1 1 d R U . . .
O6W O 0.54035(5) 0.48329(5) 0.72081(3) 0.0228(3) Uani 1 1 d . . . . .
H6W H 0.534068 0.476112 0.701369 0.034 Uiso 1 1 d R U . . .
H6V H 0.557579 0.474611 0.726664 0.034 Uiso 1 1 d R U . . .
Co2G Co 0.666667 0.333333 0.58297(2) 0.01248(10) Uani 1 3 d S T P . .
O7W O 0.63923(5) 0.36185(5) 0.61361(3) 0.0209(3) Uani 1 1 d . . . . .
H7W H 0.644912 0.366002 0.633418 0.031 Uiso 1 1 d R U . . .
H7V H 0.614506 0.365900 0.611418 0.031 Uiso 1 1 d R U . . .
O8W O 0.61053(5) 0.30398(5) 0.55217(4) 0.0231(3) Uani 1 1 d . . . . .
H8W H 0.611125 0.308576 0.532166 0.035 Uiso 1 1 d R U . . .
H8V H 0.583022 0.277882 0.554180 0.035 Uiso 1 1 d R U . . .
O9W O 0.63990(5) 0.60677(5) 0.77135(4) 0.0252(4) Uani 1 1 d . . . . .
H9W H 0.637990 0.624661 0.760243 0.038 Uiso 1 1 d R U . . .
H9V H 0.656390 0.620362 0.786546 0.038 Uiso 1 1 d R U . . .
O10W O 0.38740(6) 0.51812(6) 0.75544(4) 0.0350(4) Uani 1 1 d . . . . .
H10W H 0.367329 0.494539 0.740722 0.053 Uiso 1 1 d R U . . .
H10V H 0.373657 0.527762 0.769700 0.053 Uiso 1 1 d R U . . .
O11W O 0.49642(6) 0.37570(6) 0.75822(4) 0.0336(4) Uani 1 1 d . . . . .
H11W H 0.519122 0.376085 0.748663 0.050 Uiso 1 1 d R U . . .
H11V H 0.484026 0.347885 0.767466 0.050 Uiso 1 1 d R U . . .
O12W O 0.52750(7) 0.63703(6) 0.73443(5) 0.0450(5) Uani 1 1 d . . . . .
H12W H 0.531877 0.656611 0.723042 0.067 Uiso 1 1 d R U . . .
H12V H 0.503079 0.627514 0.738745 0.067 Uiso 1 1 d R U . . .
O13W O 0.37549(5) 0.38457(5) 0.74001(4) 0.0240(3) Uani 1 1 d . . . . .
H13W H 0.376594 0.363932 0.753004 0.036 Uiso 1 1 d R U . . .
H13V H 0.350396 0.367233 0.728598 0.036 Uiso 1 1 d R U . . .
O14W O 0.60267(6) 0.46408(7) 0.74236(4) 0.0358(4) Uani 1 1 d . . . . .
H14W H 0.618274 0.455555 0.728512 0.054 Uiso 1 1 d R U . . .
H14V H 0.625271 0.493548 0.749912 0.054 Uiso 1 1 d R U . . .
O15W O 0.56507(5) 0.37051(6) 0.60330(4) 0.0268(4) Uani 1 1 d . . . . .
H15W H 0.551319 0.372377 0.618490 0.040 Uiso 1 1 d R U . . .
H15V H 0.543127 0.346477 0.590889 0.040 Uiso 1 1 d R U . . .
O16W O 0.52849(5) 0.23038(6) 0.56608(4) 0.0323(4) Uani 1 1 d . . . . .
H16W H 0.510392 0.217093 0.551184 0.049 Uiso 1 1 d R U . . .
H16V H 0.530991 0.209993 0.577285 0.049 Uiso 1 1 d R U . . .
O17W O 0.62040(7) 0.66272(6) 0.73944(4) 0.0359(4) Uani 1 1 d . . . . .
H17W H 0.628676 0.672526 0.721366 0.054 Uiso 1 1 d R U . . .
H17V H 0.588476 0.652827 0.740767 0.054 Uiso 1 1 d R U . . .
O18W O 0.32421(6) 0.45564(6) 0.70829(4) 0.0350(4) Uani 1 1 d . . . . .
H18W H 0.334120 0.465647 0.687037 0.053 Uiso 1 1 d R U . . .
H18V H 0.316117 0.425347 0.706031 0.053 Uiso 1 1 d R U . . .
O19W O 0.55589(7) 0.36617(7) 0.70396(6) 0.0536(6) Uani 1 1 d . . . . .
H19W H 0.539507 0.373603 0.689725 0.080 Uiso 1 1 d R U . . .
H19V H 0.584702 0.389003 0.696926 0.080 Uiso 1 1 d R U . . .
O20W O 0.37153(6) 0.31878(6) 0.78685(4) 0.0290(4) Uani 1 1 d . . . . .
H20W H 0.394779 0.312053 0.788539 0.044 Uiso 1 1 d R U . . .
H20V H 0.373578 0.334453 0.805739 0.044 Uiso 1 1 d R U . . .
O21W O 0.66983(6) 0.54491(7) 0.76138(4) 0.0401(5) Uani 1 1 d . . . . .
H21W H 0.676350 0.544599 0.783070 0.060 Uiso 1 1 d R U . . .
H21V H 0.659354 0.564894 0.759269 0.060 Uiso 1 1 d R U . . .
O22W O 0.50328(6) 0.29652(6) 0.57313(5) 0.0384(4) Uani 1 1 d . . . . .
H22W H 0.492265 0.294525 0.553293 0.058 Uiso 1 1 d R U . . .
H22V H 0.512757 0.275825 0.575090 0.058 Uiso 1 1 d R U . . .
O23W O 0.53803(6) 0.16492(6) 0.59281(4) 0.0342(4) Uani 1 1 d . . . . .
H23W H 0.570190 0.174709 0.591963 0.051 Uiso 1 1 d R U . . .
H23V H 0.531290 0.157709 0.613903 0.051 Uiso 1 1 d R U . . .
O24W O 0.63953(5) 0.69889(5) 0.67800(4) 0.0238(3) Uani 1 1 d . . . . .
H24W H 0.630851 0.678979 0.664130 0.036 Uiso 1 1 d R U . . .
H24V H 0.618057 0.703279 0.678630 0.036 Uiso 1 1 d R U . . .
O25W O 0.69820(5) 0.55945(5) 0.82493(4) 0.0237(3) Uani 1 1 d . . . . .
H25W H 0.677294 0.543729 0.839280 0.036 Uiso 1 1 d R U . . .
H25V H 0.702978 0.587625 0.825779 0.036 Uiso 1 1 d R U . . .
O26W O 0.46869(5) 0.27392(5) 0.51118(4) 0.0270(4) Uani 1 1 d . . . . .
H26W H 0.462347 0.245021 0.510337 0.040 Uiso 1 1 d R U . . .
H26V H 0.487347 0.286921 0.496138 0.040 Uiso 1 1 d R U . . .
O27W O 0.86926(5) 0.39061(5) 0.65505(4) 0.0247(3) Uani 1 1 d . . . . .
H27W H 0.846786 0.373583 0.667340 0.037 Uiso 1 1 d R U . . .
H27V H 0.874285 0.417283 0.659339 0.037 Uiso 1 1 d R U . . .
C1X C 0.70357(12) 0.49498(12) 0.45406(8) 0.0582(9) Uiso 1 1 d . . . . .
H1X1 H 0.718428 0.525934 0.461746 0.087 Uiso 0.546(3) 1 d R U P A 1
H1X2 H 0.676482 0.488073 0.441862 0.087 Uiso 0.546(3) 1 d R U P A 1
H1X3 H 0.723870 0.489890 0.440507 0.087 Uiso 0.546(3) 1 d R U P A 1
H1Y1 H 0.710955 0.473806 0.464440 0.087 Uiso 0.454(3) 1 d R U P A 2
H1Y2 H 0.670943 0.482386 0.454230 0.087 Uiso 0.454(3) 1 d R U P A 2
H1Y3 H 0.717977 0.523414 0.466101 0.087 Uiso 0.454(3) 1 d R U P A 2
O1X O 0.69077(11) 0.46573(11) 0.48209(8) 0.0353(6) Uiso 0.546(3) 1 d . . P A 1
H1XO H 0.696924 0.442034 0.490198 0.053 Uiso 0.546(3) 1 d R U P A 1
O1Y O 0.71942(13) 0.50345(13) 0.42120(10) 0.0353(6) Uiso 0.454(3) 1 d . . P A 2
H1YO H 0.732427 0.496498 0.410791 0.053 Uiso 0.454(3) 1 d R U 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
Co1A O3A 2.0720(14) . ?
Co1A O1A 2.0811(14) . ?
Co1A O2A 2.0998(14) . ?
Co1A N1A 2.1680(17) . ?
Co1A N4A 2.1711(16) . ?
Co1A N7A 2.1892(17) . ?
N1A C10A 1.481(3) . ?
N1A C2A 1.486(3) . ?
N1A C9A 1.492(3) . ?
C2A C3A 1.518(3) . ?
C2A H2A 0.9900 . ?
C2A H2B 0.9900 . ?
C3A N4A 1.489(3) . ?
C3A H3A 0.9900 . ?
C3A H3B 0.9900 . ?
N4A C20A 1.481(3) . ?
N4A C5A 1.487(3) . ?
C5A C6A 1.528(3) . ?
C5A H5A 0.9900 . ?
C5A H5B 0.9900 . ?
C6A N7A 1.493(2) . ?
C6A H6A 0.9900 . ?
C6A H6B 0.9900 . ?
N7A C8A 1.483(3) . ?
N7A C30A 1.483(3) . ?
C8A C9A 1.530(3) . ?
C8A H8A 0.9900 . ?
C8A H8B 0.9900 . ?
C9A H9A 0.9900 . ?
C9A H9B 0.9900 . ?
C10A P1A 1.838(2) . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
P1A O1B 1.5015(15) . ?
P1A O1A 1.5232(15) . ?
P1A C11A 1.816(2) . ?
C11A C12A 1.489(3) . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C12A F1B 1.333(3) . ?
C12A F1C 1.338(3) . ?
C12A F1A 1.354(3) . ?
C20A P2A 1.840(2) . ?
C20A H20A 0.9900 . ?
C20A H20B 0.9900 . ?
P2A O2B 1.4953(16) . ?
P2A O2A 1.5177(15) . ?
P2A C21A 1.820(2) . ?
C21A C22A 1.492(3) . ?
C21A H21A 0.9900 . ?
C21A H21B 0.9900 . ?
C22A F2B 1.337(3) . ?
C22A F2C 1.341(3) . ?
C22A F2A 1.350(3) . ?
C30A P3A 1.839(2) . ?
C30A H30A 0.9900 . ?
C30A H30B 0.9900 . ?
P3A O3B 1.4977(15) . ?
P3A O3A 1.5210(15) . ?
P3A C31A 1.813(2) . ?
C31A C32A 1.488(3) . ?
C31A H31A 0.9900 . ?
C31A H31B 0.9900 . ?
C32A F3B 1.341(3) . ?
C32A F3C 1.346(2) . ?
C32A F3A 1.348(3) . ?
Co1D O3D 2.0750(14) . ?
Co1D O1D 2.0919(14) . ?
Co1D O2D 2.0978(15) . ?
Co1D N1D 2.1683(17) . ?
Co1D N4D 2.1778(17) . ?
Co1D N7D 2.1842(17) . ?
N1D C10D 1.483(3) . ?
N1D C2D 1.483(3) . ?
N1D C9D 1.494(3) . ?
C2D C3D 1.521(3) . ?
C2D H2D 0.9900 . ?
C2D H2E 0.9900 . ?
C3D N4D 1.488(3) . ?
C3D H3D 0.9900 . ?
C3D H3E 0.9900 . ?
N4D C20D 1.477(3) . ?
N4D C5D 1.484(3) . ?
C5D C6D 1.527(3) . ?
C5D H5D 0.9900 . ?
C5D H5E 0.9900 . ?
C6D N7D 1.492(2) . ?
C6D H6D 0.9900 . ?
C6D H6E 0.9900 . ?
N7D C30D 1.481(2) . ?
N7D C8D 1.490(3) . ?
C8D C9D 1.527(3) . ?
C8D H8D 0.9900 . ?
C8D H8E 0.9900 . ?
C9D H9D 0.9900 . ?
C9D H9E 0.9900 . ?
C10D P1D 1.838(2) . ?
C10D H10D 0.9900 . ?
C10D H10E 0.9900 . ?
P1D O1E 1.5021(15) . ?
P1D O1D 1.5224(15) . ?
P1D C11D 1.818(2) . ?
C11D C12D 1.491(3) . ?
C11D H11D 0.9900 . ?
C11D H11E 0.9900 . ?
C12D F1E 1.335(3) . ?
C12D F1F 1.341(3) . ?
C12D F1D 1.346(3) . ?
C20D P2D 1.843(2) . ?
C20D H20D 0.9900 . ?
C20D H20E 0.9900 . ?
P2D O2E 1.4941(16) . ?
P2D O2D 1.5224(16) . ?
P2D C21D 1.816(2) . ?
C21D C22E 1.490(3) . ?
C21D H21D 0.9900 . ?
C21D H21E 0.9900 . ?
C22E F2E 1.326(3) . ?
C22E F2F 1.336(3) . ?
C22E F2D 1.350(3) . ?
C30D P3D 1.837(2) . ?
C30D H30D 0.9900 . ?
C30D H30E 0.9900 . ?
P3D O3E 1.4969(15) . ?
P3D O3D 1.5252(15) . ?
P3D C31D 1.812(2) . ?
C31D C32D 1.493(3) . ?
C31D H31D 0.9900 . ?
C31D H31E 0.9900 . ?
C32D F3E 1.341(3) . ?
C32D F3F 1.344(2) . ?
C32D F3D 1.350(3) . ?
Co1G O1G 2.0838(14) 3_665 ?
Co1G O1G 2.0838(14) 2_655 ?
Co1G O1G 2.0838(14) . ?
Co1G N1G 2.1872(17) 3_665 ?
Co1G N1G 2.1872(17) 2_655 ?
Co1G N1G 2.1872(17) . ?
N1G C10G 1.484(3) . ?
N1G C2G 1.486(3) . ?
N1G C3G 1.489(2) 3_665 ?
C2G C3G 1.522(3) . ?
C2G H2G 0.9900 . ?
C2G H2H 0.9900 . ?
C3G H3G 0.9900 . ?
C3G H3H 0.9900 . ?
C10G P1G 1.833(2) . ?
C10G H10G 0.9900 . ?
C10G H10H 0.9900 . ?
P1G O1H 1.4961(16) . ?
P1G O1G 1.5180(15) . ?
P1G C11G 1.820(2) . ?
C11G C12G 1.486(3) . ?
C11G H11G 0.9900 . ?
C11G H11H 0.9900 . ?
C12G F1H 1.340(3) . ?
C12G F1I 1.344(3) . ?
C12G F1G 1.350(3) . ?
Co1J O1J 2.0983(14) 2_655 ?
Co1J O1J 2.0983(15) 3_665 ?
Co1J O1J 2.0983(14) . ?
Co1J N1J 2.1701(18) 2_655 ?
Co1J N1J 2.1701(18) 3_665 ?
Co1J N1J 2.1701(18) . ?
N1J C3J 1.466(3) 3_665 ?
N1J C10J 1.479(3) . ?
N1J C2J 1.514(3) . ?
C2J C3J 1.470(4) . ?
C2J H2J 0.9900 . ?
C2J H2K 0.9900 . ?
C3J H3J 0.9900 . ?
C3J H3K 0.9900 . ?
C10J P1J 1.830(2) . ?
C10J H10J 0.9900 . ?
C10J H10K 0.9900 . ?
P1J O1K 1.4916(18) . ?
P1J O1J 1.5201(16) . ?
P1J C11J 1.815(3) . ?
C11J C12J 1.493(3) . ?
C11J H11J 0.9900 . ?
C11J H11K 0.9900 . ?
C12J F1L 1.330(4) . ?
C12J F1K 1.333(4) . ?
C12J F1J 1.349(3) . ?
Co2A O6W 2.0501(15) . ?
Co2A O2W 2.0777(15) . ?
Co2A O3W 2.0840(15) . ?
Co2A O1W 2.0879(15) . ?
Co2A O5W 2.0928(14) . ?
Co2A O4W 2.0968(15) . ?
O1W H1W 0.7955 . ?
O1W H1V 0.8499 . ?
O2W H2W 0.8585 . ?
O2W H2V 0.8132 . ?
O3W H3W 0.8946 . ?
O3W H3V 0.8281 . ?
O4W H4W 0.8596 . ?
O4W H4V 0.8496 . ?
O5W H5W 0.9068 . ?
O5W H5V 0.8623 . ?
O6W H6W 0.8297 . ?
O6W H6V 0.8213 . ?
Co2G O7W 2.0859(14) 3_665 ?
Co2G O7W 2.0859(14) 2_655 ?
Co2G O7W 2.0860(14) . ?
Co2G O8W 2.0949(15) 2_655 ?
Co2G O8W 2.0949(15) 3_665 ?
Co2G O8W 2.0950(15) . ?
O7W H7W 0.8300 . ?
O7W H7V 0.9320 . ?
O8W H8W 0.8327 . ?
O8W H8V 0.9261 . ?
O9W H9W 0.7939 . ?
O9W H9V 0.8139 . ?
O10W H10W 0.9682 . ?
O10W H10V 0.9117 . ?
O11W H11W 0.8676 . ?
O11W H11V 0.9121 . ?
O12W H12W 0.7693 . ?
O12W H12V 0.7540 . ?
O13W H13W 0.9029 . ?
O13W H13V 0.8967 . ?
O14W H14W 0.9236 . ?
O14W H14V 0.9690 . ?
O15W H15W 0.8033 . ?
O15W H15V 0.9417 . ?
O16W H16W 0.8270 . ?
O16W H16V 0.8774 . ?
O17W H17W 0.8044 . ?
O17W H17V 0.9748 . ?
O18W H18W 0.9356 . ?
O18W H18V 0.9388 . ?
O19W H19W 0.9309 . ?
O19W H19V 0.9503 . ?
O20W H20W 0.9392 . ?
O20W H20V 0.9252 . ?
O21W H21W 0.9174 . ?
O21W H21V 0.9260 . ?
O22W H22W 0.8845 . ?
O22W H22V 0.9224 . ?
O23W H23W 0.9825 . ?
O23W H23V 0.8968 . ?
O24W H24W 0.8224 . ?
O24W H24V 0.8248 . ?
O25W H25W 0.8751 . ?
O25W H25V 0.8988 . ?
O26W H26W 0.9053 . ?
O26W H26V 0.8391 . ?
O27W H27W 0.8608 . ?
O27W H27V 0.8621 . ?
C1X O1Y 1.427(5) . ?
C1X O1X 1.442(5) . ?
C1X H1X1 0.9743 . ?
C1X H1X2 0.9759 . ?
C1X H1X3 0.9737 . ?
C1X H1Y1 0.9799 . ?
C1X H1Y2 0.9800 . ?
C1X H1Y3 0.9799 . ?
O1X H1XO 0.9958 . ?
O1Y H1YO 0.7389 . ?

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
O3A Co1A O1A 92.18(6) . . ?
O3A Co1A O2A 88.39(6) . . ?
O1A Co1A O2A 87.26(6) . . ?
O3A Co1A N1A 112.58(6) . . ?
O1A Co1A N1A 83.01(6) . . ?
O2A Co1A N1A 157.10(6) . . ?
O3A Co1A N4A 156.51(6) . . ?
O1A Co1A N4A 108.81(6) . . ?
O2A Co1A N4A 82.38(6) . . ?
N1A Co1A N4A 81.23(7) . . ?
O3A Co1A N7A 82.18(6) . . ?
O1A Co1A N7A 159.59(6) . . ?
O2A Co1A N7A 112.03(6) . . ?
N1A Co1A N7A 81.14(6) . . ?
N4A Co1A N7A 81.37(6) . . ?
C10A N1A C2A 110.39(16) . . ?
C10A N1A C9A 111.74(16) . . ?
C2A N1A C9A 111.25(15) . . ?
C10A N1A Co1A 107.73(12) . . ?
C2A N1A Co1A 104.30(12) . . ?
C9A N1A Co1A 111.13(12) . . ?
N1A C2A C3A 111.57(17) . . ?
N1A C2A H2A 109.3 . . ?
C3A C2A H2A 109.3 . . ?
N1A C2A H2B 109.3 . . ?
C3A C2A H2B 109.3 . . ?
H2A C2A H2B 108.0 . . ?
N4A C3A C2A 111.09(16) . . ?
N4A C3A H3A 109.4 . . ?
C2A C3A H3A 109.4 . . ?
N4A C3A H3B 109.4 . . ?
C2A C3A H3B 109.4 . . ?
H3A C3A H3B 108.0 . . ?
C20A N4A C5A 110.16(16) . . ?
C20A N4A C3A 111.45(16) . . ?
C5A N4A C3A 112.05(16) . . ?
C20A N4A Co1A 109.41(11) . . ?
C5A N4A Co1A 102.96(12) . . ?
C3A N4A Co1A 110.47(12) . . ?
N4A C5A C6A 111.58(17) . . ?
N4A C5A H5A 109.3 . . ?
C6A C5A H5A 109.3 . . ?
N4A C5A H5B 109.3 . . ?
C6A C5A H5B 109.3 . . ?
H5A C5A H5B 108.0 . . ?
N7A C6A C5A 110.55(16) . . ?
N7A C6A H6A 109.5 . . ?
C5A C6A H6A 109.5 . . ?
N7A C6A H6B 109.5 . . ?
C5A C6A H6B 109.5 . . ?
H6A C6A H6B 108.1 . . ?
C8A N7A C30A 109.51(16) . . ?
C8A N7A C6A 112.67(16) . . ?
C30A N7A C6A 111.58(16) . . ?
C8A N7A Co1A 103.34(12) . . ?
C30A N7A Co1A 109.60(12) . . ?
C6A N7A Co1A 109.82(12) . . ?
N7A C8A C9A 112.33(17) . . ?
N7A C8A H8A 109.1 . . ?
C9A C8A H8A 109.1 . . ?
N7A C8A H8B 109.1 . . ?
C9A C8A H8B 109.1 . . ?
H8A C8A H8B 107.9 . . ?
N1A C9A C8A 110.60(16) . . ?
N1A C9A H9A 109.5 . . ?
C8A C9A H9A 109.5 . . ?
N1A C9A H9B 109.5 . . ?
C8A C9A H9B 109.5 . . ?
H9A C9A H9B 108.1 . . ?
N1A C10A P1A 109.34(13) . . ?
N1A C10A H10A 109.8 . . ?
P1A C10A H10A 109.8 . . ?
N1A C10A H10B 109.8 . . ?
P1A C10A H10B 109.8 . . ?
H10A C10A H10B 108.3 . . ?
O1B P1A O1A 116.95(9) . . ?
O1B P1A C11A 111.71(9) . . ?
O1A P1A C11A 105.63(9) . . ?
O1B P1A C10A 110.72(9) . . ?
O1A P1A C10A 105.15(9) . . ?
C11A P1A C10A 105.90(10) . . ?
P1A O1A Co1A 117.79(8) . . ?
C12A C11A P1A 115.95(15) . . ?
C12A C11A H11A 108.3 . . ?
P1A C11A H11A 108.3 . . ?
C12A C11A H11B 108.3 . . ?
P1A C11A H11B 108.3 . . ?
H11A C11A H11B 107.4 . . ?
F1B C12A F1C 106.61(18) . . ?
F1B C12A F1A 106.7(2) . . ?
F1C C12A F1A 105.77(19) . . ?
F1B C12A C11A 113.3(2) . . ?
F1C C12A C11A 112.06(19) . . ?
F1A C12A C11A 111.90(18) . . ?
N4A C20A P2A 109.35(13) . . ?
N4A C20A H20A 109.8 . . ?
P2A C20A H20A 109.8 . . ?
N4A C20A H20B 109.8 . . ?
P2A C20A H20B 109.8 . . ?
H20A C20A H20B 108.3 . . ?
O2B P2A O2A 115.35(9) . . ?
O2B P2A C21A 109.91(10) . . ?
O2A P2A C21A 107.29(9) . . ?
O2B P2A C20A 112.71(10) . . ?
O2A P2A C20A 105.59(9) . . ?
C21A P2A C20A 105.36(10) . . ?
P2A O2A Co1A 118.22(8) . . ?
C22A C21A P2A 115.00(16) . . ?
C22A C21A H21A 108.5 . . ?
P2A C21A H21A 108.5 . . ?
C22A C21A H21B 108.5 . . ?
P2A C21A H21B 108.5 . . ?
H21A C21A H21B 107.5 . . ?
F2B C22A F2C 106.09(18) . . ?
F2B C22A F2A 106.5(2) . . ?
F2C C22A F2A 106.07(19) . . ?
F2B C22A C21A 113.0(2) . . ?
F2C C22A C21A 112.4(2) . . ?
F2A C22A C21A 112.20(18) . . ?
N7A C30A P3A 109.36(13) . . ?
N7A C30A H30A 109.8 . . ?
P3A C30A H30A 109.8 . . ?
N7A C30A H30B 109.8 . . ?
P3A C30A H30B 109.8 . . ?
H30A C30A H30B 108.2 . . ?
O3B P3A O3A 115.51(9) . . ?
O3B P3A C31A 110.07(9) . . ?
O3A P3A C31A 106.98(9) . . ?
O3B P3A C30A 113.21(9) . . ?
O3A P3A C30A 104.78(9) . . ?
C31A P3A C30A 105.61(10) . . ?
P3A O3A Co1A 120.06(8) . . ?
C32A C31A P3A 115.25(15) . . ?
C32A C31A H31A 108.5 . . ?
P3A C31A H31A 108.5 . . ?
C32A C31A H31B 108.5 . . ?
P3A C31A H31B 108.5 . . ?
H31A C31A H31B 107.5 . . ?
F3B C32A F3C 106.46(18) . . ?
F3B C32A F3A 106.25(19) . . ?
F3C C32A F3A 106.02(18) . . ?
F3B C32A C31A 113.12(19) . . ?
F3C C32A C31A 111.68(19) . . ?
F3A C32A C31A 112.80(18) . . ?
O3D Co1D O1D 91.60(6) . . ?
O3D Co1D O2D 88.72(6) . . ?
O1D Co1D O2D 89.20(6) . . ?
O3D Co1D N1D 112.68(6) . . ?
O1D Co1D N1D 83.04(6) . . ?
O2D Co1D N1D 157.32(6) . . ?
O3D Co1D N4D 156.94(6) . . ?
O1D Co1D N4D 109.11(6) . . ?
O2D Co1D N4D 81.75(6) . . ?
N1D Co1D N4D 80.75(6) . . ?
O3D Co1D N7D 82.21(6) . . ?
O1D Co1D N7D 159.60(6) . . ?
O2D Co1D N7D 109.97(6) . . ?
N1D Co1D N7D 81.50(6) . . ?
N4D Co1D N7D 81.42(6) . . ?
C10D N1D C2D 109.84(16) . . ?
C10D N1D C9D 111.78(16) . . ?
C2D N1D C9D 111.24(15) . . ?
C10D N1D Co1D 108.17(12) . . ?
C2D N1D Co1D 104.86(12) . . ?
C9D N1D Co1D 110.70(12) . . ?
N1D C2D C3D 111.57(17) . . ?
N1D C2D H2D 109.3 . . ?
C3D C2D H2D 109.3 . . ?
N1D C2D H2E 109.3 . . ?
C3D C2D H2E 109.3 . . ?
H2D C2D H2E 108.0 . . ?
N4D C3D C2D 110.52(16) . . ?
N4D C3D H3D 109.5 . . ?
C2D C3D H3D 109.5 . . ?
N4D C3D H3E 109.5 . . ?
C2D C3D H3E 109.5 . . ?
H3D C3D H3E 108.1 . . ?
C20D N4D C5D 110.75(16) . . ?
C20D N4D C3D 111.21(16) . . ?
C5D N4D C3D 111.96(16) . . ?
C20D N4D Co1D 108.88(12) . . ?
C5D N4D Co1D 102.71(12) . . ?
C3D N4D Co1D 110.99(12) . . ?
N4D C5D C6D 111.60(17) . . ?
N4D C5D H5D 109.3 . . ?
C6D C5D H5D 109.3 . . ?
N4D C5D H5E 109.3 . . ?
C6D C5D H5E 109.3 . . ?
H5D C5D H5E 108.0 . . ?
N7D C6D C5D 110.96(16) . . ?
N7D C6D H6D 109.4 . . ?
C5D C6D H6D 109.4 . . ?
N7D C6D H6E 109.4 . . ?
C5D C6D H6E 109.4 . . ?
H6D C6D H6E 108.0 . . ?
C30D N7D C8D 109.63(16) . . ?
C30D N7D C6D 111.55(16) . . ?
C8D N7D C6D 112.72(15) . . ?
C30D N7D Co1D 109.56(11) . . ?
C8D N7D Co1D 103.36(12) . . ?
C6D N7D Co1D 109.70(12) . . ?
N7D C8D C9D 112.34(16) . . ?
N7D C8D H8D 109.1 . . ?
C9D C8D H8D 109.1 . . ?
N7D C8D H8E 109.1 . . ?
C9D C8D H8E 109.1 . . ?
H8D C8D H8E 107.9 . . ?
N1D C9D C8D 111.23(16) . . ?
N1D C9D H9D 109.4 . . ?
C8D C9D H9D 109.4 . . ?
N1D C9D H9E 109.4 . . ?
C8D C9D H9E 109.4 . . ?
H9D C9D H9E 108.0 . . ?
N1D C10D P1D 109.05(13) . . ?
N1D C10D H10D 109.9 . . ?
P1D C10D H10D 109.9 . . ?
N1D C10D H10E 109.9 . . ?
P1D C10D H10E 109.9 . . ?
H10D C10D H10E 108.3 . . ?
O1E P1D O1D 116.48(9) . . ?
O1E P1D C11D 111.04(9) . . ?
O1D P1D C11D 106.09(9) . . ?
O1E P1D C10D 111.43(9) . . ?
O1D P1D C10D 105.32(9) . . ?
C11D P1D C10D 105.75(10) . . ?
P1D O1D Co1D 117.78(8) . . ?
C12D C11D P1D 115.48(15) . . ?
C12D C11D H11D 108.4 . . ?
P1D C11D H11D 108.4 . . ?
C12D C11D H11E 108.4 . . ?
P1D C11D H11E 108.4 . . ?
H11D C11D H11E 107.5 . . ?
F1E C12D F1F 105.97(19) . . ?
F1E C12D F1D 107.1(2) . . ?
F1F C12D F1D 105.63(19) . . ?
F1E C12D C11D 113.2(2) . . ?
F1F C12D C11D 112.0(2) . . ?
F1D C12D C11D 112.41(19) . . ?
N4D C20D P2D 109.94(14) . . ?
N4D C20D H20D 109.7 . . ?
P2D C20D H20D 109.7 . . ?
N4D C20D H20E 109.7 . . ?
P2D C20D H20E 109.7 . . ?
H20D C20D H20E 108.2 . . ?
O2E P2D O2D 116.05(9) . . ?
O2E P2D C21D 110.67(10) . . ?
O2D P2D C21D 106.30(10) . . ?
O2E P2D C20D 112.28(10) . . ?
O2D P2D C20D 105.33(9) . . ?
C21D P2D C20D 105.47(10) . . ?
P2D O2D Co1D 117.66(8) . . ?
C22E C21D P2D 115.31(16) . . ?
C22E C21D H21D 108.4 . . ?
P2D C21D H21D 108.4 . . ?
C22E C21D H21E 108.4 . . ?
P2D C21D H21E 108.4 . . ?
H21D C21D H21E 107.5 . . ?
F2E C22E F2F 106.2(2) . . ?
F2E C22E F2D 106.4(2) . . ?
F2F C22E F2D 106.0(2) . . ?
F2E C22E C21D 113.2(2) . . ?
F2F C22E C21D 112.3(2) . . ?
F2D C22E C21D 112.2(2) . . ?
N7D C30D P3D 109.25(13) . . ?
N7D C30D H30D 109.8 . . ?
P3D C30D H30D 109.8 . . ?
N7D C30D H30E 109.8 . . ?
P3D C30D H30E 109.8 . . ?
H30D C30D H30E 108.3 . . ?
O3E P3D O3D 115.26(9) . . ?
O3E P3D C31D 110.21(9) . . ?
O3D P3D C31D 107.15(9) . . ?
O3E P3D C30D 112.93(9) . . ?
O3D P3D C30D 104.54(9) . . ?
C31D P3D C30D 106.15(10) . . ?
P3D O3D Co1D 119.90(8) . . ?
C32D C31D P3D 115.15(15) . . ?
C32D C31D H31D 108.5 . . ?
P3D C31D H31D 108.5 . . ?
C32D C31D H31E 108.5 . . ?
P3D C31D H31E 108.5 . . ?
H31D C31D H31E 107.5 . . ?
F3E C32D F3F 106.37(17) . . ?
F3E C32D F3D 106.53(18) . . ?
F3F C32D F3D 105.95(18) . . ?
F3E C32D C31D 113.36(19) . . ?
F3F C32D C31D 111.58(18) . . ?
F3D C32D C31D 112.54(18) . . ?
O1G Co1G O1G 87.42(6) 3_665 2_655 ?
O1G Co1G O1G 87.42(6) 3_665 . ?
O1G Co1G O1G 87.42(6) 2_655 . ?
O1G Co1G N1G 83.13(6) 3_665 3_665 ?
O1G Co1G N1G 114.24(6) 2_655 3_665 ?
O1G Co1G N1G 155.79(6) . 3_665 ?
O1G Co1G N1G 155.79(6) 3_665 2_655 ?
O1G Co1G N1G 83.13(6) 2_655 2_655 ?
O1G Co1G N1G 114.24(6) . 2_655 ?
N1G Co1G N1G 80.57(7) 3_665 2_655 ?
O1G Co1G N1G 114.24(6) 3_665 . ?
O1G Co1G N1G 155.79(6) 2_655 . ?
O1G Co1G N1G 83.13(6) . . ?
N1G Co1G N1G 80.57(7) 3_665 . ?
N1G Co1G N1G 80.57(7) 2_655 . ?
C10G N1G C2G 109.96(16) . . ?
C10G N1G C3G 111.30(16) . 3_665 ?
C2G N1G C3G 111.81(15) . 3_665 ?
C10G N1G Co1G 108.89(12) . . ?
C2G N1G Co1G 103.89(12) . . ?
C3G N1G Co1G 110.72(12) 3_665 . ?
N1G C2G C3G 111.58(17) . . ?
N1G C2G H2G 109.3 . . ?
C3G C2G H2G 109.3 . . ?
N1G C2G H2H 109.3 . . ?
C3G C2G H2H 109.3 . . ?
H2G C2G H2H 108.0 . . ?
N1G C3G C2G 111.05(16) 2_655 . ?
N1G C3G H3G 109.4 2_655 . ?
C2G C3G H3G 109.4 . . ?
N1G C3G H3H 109.4 2_655 . ?
C2G C3G H3H 109.4 . . ?
H3G C3G H3H 108.0 . . ?
N1G C10G P1G 109.25(13) . . ?
N1G C10G H10G 109.8 . . ?
P1G C10G H10G 109.8 . . ?
N1G C10G H10H 109.8 . . ?
P1G C10G H10H 109.8 . . ?
H10G C10G H10H 108.3 . . ?
O1H P1G O1G 116.13(9) . . ?
O1H P1G C11G 111.02(10) . . ?
O1G P1G C11G 106.48(9) . . ?
O1H P1G C10G 111.62(9) . . ?
O1G P1G C10G 105.58(9) . . ?
C11G P1G C10G 105.27(10) . . ?
P1G O1G Co1G 118.65(8) . . ?
C12G C11G P1G 115.20(16) . . ?
C12G C11G H11G 108.5 . . ?
P1G C11G H11G 108.5 . . ?
C12G C11G H11H 108.5 . . ?
P1G C11G H11H 108.5 . . ?
H11G C11G H11H 107.5 . . ?
F1H C12G F1I 106.05(18) . . ?
F1H C12G F1G 106.6(2) . . ?
F1I C12G F1G 105.58(19) . . ?
F1H C12G C11G 113.2(2) . . ?
F1I C12G C11G 112.3(2) . . ?
F1G C12G C11G 112.62(18) . . ?
O1J Co1J O1J 90.47(6) 2_655 3_665 ?
O1J Co1J O1J 90.47(6) 2_655 . ?
O1J Co1J O1J 90.47(6) 3_665 . ?
O1J Co1J N1J 83.18(6) 2_655 2_655 ?
O1J Co1J N1J 160.12(7) 3_665 2_655 ?
O1J Co1J N1J 108.34(7) . 2_655 ?
O1J Co1J N1J 108.34(7) 2_655 3_665 ?
O1J Co1J N1J 83.18(6) 3_665 3_665 ?
O1J Co1J N1J 160.12(7) . 3_665 ?
N1J Co1J N1J 81.01(7) 2_655 3_665 ?
O1J Co1J N1J 160.12(7) 2_655 . ?
O1J Co1J N1J 108.34(7) 3_665 . ?
O1J Co1J N1J 83.18(6) . . ?
N1J Co1J N1J 81.01(7) 2_655 . ?
N1J Co1J N1J 81.01(7) 3_665 . ?
C3J N1J C10J 112.51(19) 3_665 . ?
C3J N1J C2J 110.9(2) 3_665 . ?
C10J N1J C2J 110.13(19) . . ?
C3J N1J Co1J 111.38(15) 3_665 . ?
C10J N1J Co1J 108.19(12) . . ?
C2J N1J Co1J 103.35(14) . . ?
C3J C2J N1J 114.1(2) . . ?
C3J C2J H2J 108.7 . . ?
N1J C2J H2J 108.7 . . ?
C3J C2J H2K 108.7 . . ?
N1J C2J H2K 108.7 . . ?
H2J C2J H2K 107.6 . . ?
N1J C3J C2J 112.2(2) 2_655 . ?
N1J C3J H3J 109.2 2_655 . ?
C2J C3J H3J 109.2 . . ?
N1J C3J H3K 109.2 2_655 . ?
C2J C3J H3K 109.2 . . ?
H3J C3J H3K 107.9 . . ?
N1J C10J P1J 109.04(14) . . ?
N1J C10J H10J 109.9 . . ?
P1J C10J H10J 109.9 . . ?
N1J C10J H10K 109.9 . . ?
P1J C10J H10K 109.9 . . ?
H10J C10J H10K 108.3 . . ?
O1K P1J O1J 116.55(11) . . ?
O1K P1J C11J 110.95(12) . . ?
O1J P1J C11J 105.83(10) . . ?
O1K P1J C10J 110.87(10) . . ?
O1J P1J C10J 105.95(9) . . ?
C11J P1J C10J 106.02(11) . . ?
P1J O1J Co1J 117.14(8) . . ?
C12J C11J P1J 115.48(19) . . ?
C12J C11J H11J 108.4 . . ?
P1J C11J H11J 108.4 . . ?
C12J C11J H11K 108.4 . . ?
P1J C11J H11K 108.4 . . ?
H11J C11J H11K 107.5 . . ?
F1L C12J F1K 106.3(2) . . ?
F1L C12J F1J 105.7(3) . . ?
F1K C12J F1J 107.4(2) . . ?
F1L C12J C11J 112.2(2) . . ?
F1K C12J C11J 113.2(3) . . ?
F1J C12J C11J 111.6(2) . . ?
O6W Co2A O2W 176.07(6) . . ?
O6W Co2A O3W 91.07(6) . . ?
O2W Co2A O3W 92.84(6) . . ?
O6W Co2A O1W 92.23(6) . . ?
O2W Co2A O1W 87.49(6) . . ?
O3W Co2A O1W 88.98(6) . . ?
O6W Co2A O5W 92.82(6) . . ?
O2W Co2A O5W 87.67(6) . . ?
O3W Co2A O5W 88.04(6) . . ?
O1W Co2A O5W 174.18(6) . . ?
O6W Co2A O4W 86.69(6) . . ?
O2W Co2A O4W 89.43(6) . . ?
O3W Co2A O4W 176.13(6) . . ?
O1W Co2A O4W 94.25(6) . . ?
O5W Co2A O4W 88.93(6) . . ?
Co2A O1W H1W 122.2 . . ?
Co2A O1W H1V 127.9 . . ?
H1W O1W H1V 109.8 . . ?
Co2A O2W H2W 118.7 . . ?
Co2A O2W H2V 125.1 . . ?
H2W O2W H2V 109.5 . . ?
Co2A O3W H3W 118.7 . . ?
Co2A O3W H3V 120.7 . . ?
H3W O3W H3V 115.4 . . ?
Co2A O4W H4W 119.6 . . ?
Co2A O4W H4V 127.9 . . ?
H4W O4W H4V 110.0 . . ?
Co2A O5W H5W 123.3 . . ?
Co2A O5W H5V 120.7 . . ?
H5W O5W H5V 111.9 . . ?
Co2A O6W H6W 122.7 . . ?
Co2A O6W H6V 127.5 . . ?
H6W O6W H6V 107.4 . . ?
O7W Co2G O7W 87.54(6) 3_665 2_655 ?
O7W Co2G O7W 87.54(6) 3_665 . ?
O7W Co2G O7W 87.54(6) 2_655 . ?
O7W Co2G O8W 91.31(6) 3_665 2_655 ?
O7W Co2G O8W 93.70(6) 2_655 2_655 ?
O7W Co2G O8W 178.28(6) . 2_655 ?
O7W Co2G O8W 93.70(6) 3_665 3_665 ?
O7W Co2G O8W 178.27(6) 2_655 3_665 ?
O7W Co2G O8W 91.32(6) . 3_665 ?
O8W Co2G O8W 87.47(6) 2_655 3_665 ?
O7W Co2G O8W 178.27(6) 3_665 . ?
O7W Co2G O8W 91.31(6) 2_655 . ?
O7W Co2G O8W 93.70(6) . . ?
O8W Co2G O8W 87.47(6) 2_655 . ?
O8W Co2G O8W 87.47(6) 3_665 . ?
Co2G O7W H7W 123.1 . . ?
Co2G O7W H7V 132.3 . . ?
H7W O7W H7V 102.8 . . ?
Co2G O8W H8W 124.9 . . ?
Co2G O8W H8V 131.4 . . ?
H8W O8W H8V 100.8 . . ?
H9W O9W H9V 107.3 . . ?
H10W O10W H10V 114.9 . . ?
H11W O11W H11V 98.5 . . ?
H12W O12W H12V 102.2 . . ?
H13W O13W H13V 100.9 . . ?
H14W O14W H14V 103.8 . . ?
H15W O15W H15V 104.1 . . ?
H16W O16W H16V 107.0 . . ?
H17W O17W H17V 107.3 . . ?
H18W O18W H18V 99.6 . . ?
H19W O19W H19V 96.2 . . ?
H20W O20W H20V 104.8 . . ?
H21W O21W H21V 106.7 . . ?
H22W O22W H22V 108.8 . . ?
H23W O23W H23V 102.7 . . ?
H24W O24W H24V 100.9 . . ?
H25W O25W H25V 106.9 . . ?
H26W O26W H26V 104.9 . . ?
H27W O27W H27V 103.8 . . ?
O1X C1X H1X1 108.4 . . ?
O1X C1X H1X2 108.5 . . ?
H1X1 C1X H1X2 110.3 . . ?
O1X C1X H1X3 109.0 . . ?
H1X1 C1X H1X3 110.4 . . ?
H1X2 C1X H1X3 110.3 . . ?
O1Y C1X H1Y1 110.3 . . ?
O1Y C1X H1Y2 109.4 . . ?
H1Y1 C1X H1Y2 109.5 . . ?
O1Y C1X H1Y3 108.7 . . ?
H1Y1 C1X H1Y3 109.5 . . ?
H1Y2 C1X H1Y3 109.5 . . ?
C1X O1X H1XO 136.1 . . ?
C1X O1Y H1YO 135.2 . . ?

_refine_diff_density_max         1.436
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.071

