#------------------------------------------------------------------------------
#$Date: 2024-12-06 21:04:35 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296592 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/70/7717030.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7717030
loop_
_publ_author_name
'Guglielmero, Luca'
'Ciccone, Lidia'
'Mezzetta, Andrea'
'D'Andrea, Felicia'
'Guazzelli, Lorenzo'
'Pomelli, Christian Silvio'
_publ_section_title
;
 Synthesis and characterization of divalent metal-betaine-bistriflimide
 complexes: a property comparison with metal bistriflimide salts.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16693
_journal_page_last               16708
_journal_paper_doi               10.1039/d4dt01950d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C19 H33 Ca F12 N5 O14 S4'
_chemical_formula_weight         951.82
_chemical_name_systematic        CaBetTfN_2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2024-07-29 deposited with the CCDC.	2024-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                105.4270(10)
_cell_angle_beta                 105.0780(10)
_cell_angle_gamma                101.0740(10)
_cell_formula_units_Z            2
_cell_length_a                   9.0322(2)
_cell_length_b                   15.1177(4)
_cell_length_c                   15.2478(4)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.39
_cell_volume                     1860.00(8)
_computing_cell_refinement       'Apex4 (Bruker AXS Inc., 2022)'
_computing_data_collection       'Apex4 (Bruker AXS Inc., 2022)'
_computing_data_reduction        'Apex4 (Bruker AXS Inc., 2022)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            52290
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.291
_diffrn_reflns_theta_min         2.387
_diffrn_source                   micro-focus
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_meas      ?
_exptl_crystal_description       tabular
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         9211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0337P)²+1.7887P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8259
_reflns_number_total             9211
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01950d2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7717029--7717030.cif.
;
_cod_database_code               7717030
_shelx_shelxl_version_number     2018/1
_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.
;
_shelx_estimated_absorpt_t_min   0.880
_shelx_estimated_absorpt_t_max   0.974
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Ca1 Ca 0.500000 0.500000 0.000000 0.00858(8) Uani 1 2 d S . P . .
Ca2 Ca 0.000000 0.500000 0.000000 0.00872(8) Uani 1 2 d S . P . .
S1 S 0.89676(4) 0.73701(3) 0.47560(3) 0.01327(8) Uani 1 1 d . . . . .
S2 S 0.77194(4) 0.65629(3) 0.59552(3) 0.01574(8) Uani 1 1 d . . . . .
S3 S 0.66039(5) 1.05104(3) 0.73664(3) 0.01543(8) Uani 1 1 d . . . . .
S4 S 0.66544(5) 0.99849(3) 0.89880(3) 0.01490(8) Uani 1 1 d . . . . .
F1 F 1.03366(15) 0.90014(8) 0.46831(9) 0.0357(3) Uani 1 1 d . . . . .
F2 F 0.88063(15) 0.70617(9) 0.78200(8) 0.0335(3) Uani 1 1 d . . . . .
F3 F 1.02356(13) 0.79021(8) 0.72364(8) 0.0277(2) Uani 1 1 d . . . . .
F4 F 0.79844(16) 0.81344(9) 0.73064(9) 0.0373(3) Uani 1 1 d . . . . .
F5 F 0.79087(15) 0.88470(8) 0.46646(9) 0.0342(3) Uani 1 1 d . . . . .
F6 F 0.97749(17) 0.91055(8) 0.59911(8) 0.0393(3) Uani 1 1 d . . . . .
F7 F 0.44255(15) 0.96835(9) 0.56776(8) 0.0364(3) Uani 1 1 d . . . . .
F8 F 0.93499(12) 1.10673(9) 1.03236(8) 0.0297(2) Uani 1 1 d . . . . .
F9 F 0.72623(14) 1.11360(8) 1.07333(8) 0.0324(3) Uani 1 1 d . . . . .
F10 F 0.5895(2) 0.88162(10) 0.60989(10) 0.0603(5) Uani 1 1 d . . . . .
F11 F 0.40719(19) 0.90378(11) 0.67200(10) 0.0570(4) Uani 1 1 d . . . . .
F12 F 0.78100(14) 1.18516(7) 0.97606(8) 0.0283(2) Uani 1 1 d . . . . .
O1 O 0.91419(14) 0.44919(9) 0.11773(8) 0.0206(2) Uani 1 1 d . . . . .
O2 O 0.96439(13) 0.65264(8) 0.05372(8) 0.0174(2) Uani 1 1 d . . . . .
O3 O 0.23393(13) 0.55940(8) 0.12787(8) 0.0167(2) Uani 1 1 d . . . . .
O4 O 0.83039(15) 0.70060(9) 0.37268(8) 0.0206(2) Uani 1 1 d . . . . .
O5 O 1.04974(14) 0.72594(10) 0.51924(9) 0.0231(3) Uani 1 1 d . . . . .
O6 O 0.61361(15) 0.62258(10) 0.59748(10) 0.0276(3) Uani 1 1 d . . . . .
O7 O 0.86900(15) 0.59155(8) 0.58952(9) 0.0210(2) Uani 1 1 d . . . . .
O8 O 0.50348(14) 1.00175(9) 0.88215(9) 0.0220(2) Uani 1 1 d . . . . .
O9 O 0.77909(16) 1.07930(10) 0.69533(9) 0.0270(3) Uani 1 1 d . . . . .
O10 O 0.56499(16) 1.11413(9) 0.75815(9) 0.0227(3) Uani 1 1 d . . . . .
O11 O 0.71057(16) 0.92300(9) 0.92894(9) 0.0240(3) Uani 1 1 d . . . . .
O12 O 0.65256(14) 0.42860(9) 0.08893(8) 0.0196(2) Uani 1 1 d . . . . .
O13 O 0.49474(13) 0.59401(8) 0.14895(8) 0.0169(2) Uani 1 1 d . . . . .
O14 O 0.70277(14) 0.63044(8) 0.02452(9) 0.0207(2) Uani 1 1 d . . . . .
N1 N 0.67241(15) 0.37521(10) 0.25825(9) 0.0140(2) Uani 1 1 d . . . . .
N2 N 0.29994(14) 0.66635(9) 0.32827(9) 0.0111(2) Uani 1 1 d . . . . .
N3 N 0.77694(14) 0.83257(9) 0.13763(9) 0.0113(2) Uani 1 1 d . . . . .
N4 N 0.76266(15) 0.71143(10) 0.52125(10) 0.0164(3) Uani 1 1 d . . . . .
N5 N 0.73767(16) 1.01131(10) 0.81769(10) 0.0166(3) Uani 1 1 d . . . . .
C1 C 0.7186(2) 0.33379(16) 0.33727(14) 0.0290(4) Uani 1 1 d . . . . .
H20 H 0.724605 0.268691 0.309650 0.044 Uiso 1 1 calc R U . . .
H19 H 0.638431 0.332176 0.369909 0.044 Uiso 1 1 calc R U . . .
H1 H 0.823032 0.373481 0.383777 0.044 Uiso 1 1 calc R U . . .
C2 C 0.7984(2) 0.37479(14) 0.20937(13) 0.0219(3) Uani 1 1 d . . . . .
H18 H 0.794789 0.307460 0.179023 0.026 Uiso 1 1 calc R U . . .
H27 H 0.904365 0.406145 0.259748 0.026 Uiso 1 1 calc R U . . .
C3 C 0.78618(18) 0.42377(11) 0.13212(11) 0.0143(3) Uani 1 1 d . . . . .
C4 C 0.37645(17) 0.60143(10) 0.17526(10) 0.0109(3) Uani 1 1 d . . . . .
C5 C 0.42107(17) 0.67370(10) 0.27677(10) 0.0122(3) Uani 1 1 d . . . . .
H6 H 0.520930 0.667432 0.317438 0.015 Uiso 1 1 calc R U . . .
H5 H 0.444983 0.738727 0.272244 0.015 Uiso 1 1 calc R U . . .
C6 C 0.14919(19) 0.68577(13) 0.27849(12) 0.0187(3) Uani 1 1 d . . . . .
H29 H 0.175557 0.747342 0.268161 0.028 Uiso 1 1 calc R U . . .
H2 H 0.080038 0.687755 0.318562 0.028 Uiso 1 1 calc R U . . .
H28 H 0.093505 0.634884 0.216226 0.028 Uiso 1 1 calc R U . . .
C7 C 0.37495(19) 0.74061(12) 0.42628(11) 0.0195(3) Uani 1 1 d . . . . .
H4 H 0.402636 0.803989 0.419900 0.029 Uiso 1 1 calc R U . . .
H33 H 0.471880 0.727923 0.460958 0.029 Uiso 1 1 calc R U . . .
H3 H 0.299433 0.738515 0.462156 0.029 Uiso 1 1 calc R U . . .
C8 C 0.84332(17) 0.68083(10) 0.05093(10) 0.0116(3) Uani 1 1 d . . . . .
C9 C 0.87504(17) 0.79001(10) 0.08050(11) 0.0122(3) Uani 1 1 d . . . . .
H7 H 0.989413 0.819859 0.119032 0.015 Uiso 1 1 calc R U . . .
H8 H 0.855650 0.807667 0.021318 0.015 Uiso 1 1 calc R U . . .
C10 C 0.84357(19) 0.93955(11) 0.17152(12) 0.0175(3) Uani 1 1 d . . . . .
H10 H 0.840379 0.960722 0.115809 0.026 Uiso 1 1 calc R U . . .
H9 H 0.954313 0.958001 0.214299 0.026 Uiso 1 1 calc R U . . .
H11 H 0.779392 0.969602 0.206531 0.026 Uiso 1 1 calc R U . . .
C11 C 0.79130(19) 0.80061(12) 0.22361(11) 0.0169(3) Uani 1 1 d . . . . .
H14 H 0.742944 0.731409 0.202195 0.025 Uiso 1 1 calc R U . . .
H12 H 0.735966 0.833502 0.263543 0.025 Uiso 1 1 calc R U . . .
H13 H 0.904381 0.816002 0.261380 0.025 Uiso 1 1 calc R U . . .
C12 C 0.60408(17) 0.80684(11) 0.07773(11) 0.0160(3) Uani 1 1 d . . . . .
H16 H 0.595096 0.831162 0.023629 0.024 Uiso 1 1 calc R U . . .
H17 H 0.544743 0.835412 0.117509 0.024 Uiso 1 1 calc R U . . .
H15 H 0.559696 0.737156 0.053000 0.024 Uiso 1 1 calc R U . . .
C13 C 0.5113(2) 0.31352(17) 0.18955(14) 0.0365(5) Uani 1 1 d . . . . .
H23 H 0.477823 0.339461 0.137541 0.055 Uiso 1 1 calc R U . . .
H21 H 0.433521 0.312456 0.223964 0.055 Uiso 1 1 calc R U . . .
H22 H 0.517186 0.248344 0.162286 0.055 Uiso 1 1 calc R U . . .
C14 C 0.6668(3) 0.47378(14) 0.30108(15) 0.0333(4) Uani 1 1 d . . . . .
H25 H 0.632027 0.500410 0.249804 0.050 Uiso 1 1 calc R U . . .
H24 H 0.773382 0.513172 0.344834 0.050 Uiso 1 1 calc R U . . .
H26 H 0.591348 0.473225 0.337056 0.050 Uiso 1 1 calc R U . . .
C15 C 0.2603(2) 0.56995(12) 0.33907(13) 0.0224(3) Uani 1 1 d . . . . .
H30 H 0.208942 0.520963 0.275248 0.034 Uiso 1 1 calc R U . . .
H32 H 0.187409 0.568154 0.376667 0.034 Uiso 1 1 calc R U . . .
H31 H 0.358539 0.557566 0.372381 0.034 Uiso 1 1 calc R U . . .
C16 C 0.9258(2) 0.86626(12) 0.50492(13) 0.0236(3) Uani 1 1 d . . . . .
C17 C 0.8747(2) 0.74778(13) 0.71478(12) 0.0221(3) Uani 1 1 d . . . . .
C18 C 0.5162(2) 0.94473(13) 0.64131(13) 0.0265(4) Uani 1 1 d . . . . .
C20 C 0.7838(2) 1.10771(12) 1.00085(12) 0.0187(3) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O14 Ca1 O14 180.0 . 2_665 ?
O14 Ca1 O12 96.81(4) . . ?
O14 Ca1 O12 83.19(4) 2_665 . ?
O14 Ca1 O12 83.19(4) . 2_665 ?
O14 Ca1 O12 96.81(4) 2_665 2_665 ?
O12 Ca1 O12 180.0 . 2_665 ?
O14 Ca1 O13 82.84(4) . . ?
O14 Ca1 O13 97.16(4) 2_665 . ?
O12 Ca1 O13 85.38(4) . . ?
O12 Ca1 O13 94.62(4) 2_665 . ?
O14 Ca1 O13 97.16(4) . 2_665 ?
O14 Ca1 O13 82.84(4) 2_665 2_665 ?
O12 Ca1 O13 94.62(4) . 2_665 ?
O12 Ca1 O13 85.38(4) 2_665 2_665 ?
O13 Ca1 O13 180.00(5) . 2_665 ?
O3 Ca2 O3 180.0 . 2_565 ?
O3 Ca2 O2 94.56(4) . 2_665 ?
O3 Ca2 O2 85.44(4) 2_565 2_665 ?
O3 Ca2 O2 85.44(4) . 1_455 ?
O3 Ca2 O2 94.56(4) 2_565 1_455 ?
O2 Ca2 O2 180.0 2_665 1_455 ?
O3 Ca2 O1 79.49(4) . 1_455 ?
O3 Ca2 O1 100.51(4) 2_565 1_455 ?
O2 Ca2 O1 86.14(4) 2_665 1_455 ?
O2 Ca2 O1 93.86(4) 1_455 1_455 ?
O3 Ca2 O1 100.51(4) . 2_665 ?
O3 Ca2 O1 79.49(4) 2_565 2_665 ?
O2 Ca2 O1 93.86(4) 2_665 2_665 ?
O2 Ca2 O1 86.14(4) 1_455 2_665 ?
O1 Ca2 O1 180.00(6) 1_455 2_665 ?
O4 S1 O5 117.87(8) . . ?
O4 S1 N4 109.91(7) . . ?
O5 S1 N4 116.86(7) . . ?
O4 S1 C16 103.74(8) . . ?
O5 S1 C16 105.66(8) . . ?
N4 S1 C16 100.13(8) . . ?
O6 S2 O7 118.64(8) . . ?
O6 S2 N4 108.08(8) . . ?
O7 S2 N4 115.24(7) . . ?
O6 S2 C17 103.22(8) . . ?
O7 S2 C17 104.30(8) . . ?
N4 S2 C17 105.78(8) . . ?
O9 S3 O10 117.86(8) . . ?
O9 S3 N5 107.87(8) . . ?
O10 S3 N5 117.41(7) . . ?
O9 S3 C18 104.16(9) . . ?
O10 S3 C18 103.65(9) . . ?
N5 S3 C18 103.95(8) . . ?
O11 S4 O8 118.49(8) . . ?
O11 S4 N5 109.21(8) . . ?
O8 S4 N5 115.73(7) . . ?
O11 S4 C20 104.34(8) . . ?
O8 S4 C20 104.76(8) . . ?
N5 S4 C20 102.15(7) . . ?
C3 O1 Ca2 137.42(10) . 1_655 ?
C8 O2 Ca2 132.57(10) . 1_655 ?
C4 O3 Ca2 159.42(10) . . ?
C3 O12 Ca1 149.49(11) . . ?
C4 O13 Ca1 128.49(10) . . ?
C8 O14 Ca1 156.94(11) . . ?
C14 N1 C13 110.68(16) . . ?
C14 N1 C1 108.86(14) . . ?
C13 N1 C1 107.87(14) . . ?
C14 N1 C2 110.59(14) . . ?
C13 N1 C2 111.34(14) . . ?
C1 N1 C2 107.37(12) . . ?
C15 N2 C7 108.89(12) . . ?
C15 N2 C6 109.41(13) . . ?
C7 N2 C6 108.13(12) . . ?
C15 N2 C5 110.74(12) . . ?
C7 N2 C5 106.86(11) . . ?
C6 N2 C5 112.68(11) . . ?
C11 N3 C12 109.89(12) . . ?
C11 N3 C10 108.92(12) . . ?
C12 N3 C10 108.34(11) . . ?
C11 N3 C9 110.14(11) . . ?
C12 N3 C9 112.10(11) . . ?
C10 N3 C9 107.36(11) . . ?
S2 N4 S1 125.26(8) . . ?
S3 N5 S4 123.89(9) . . ?
N1 C1 H20 109.5 . . ?
N1 C1 H19 109.5 . . ?
H20 C1 H19 109.5 . . ?
N1 C1 H1 109.5 . . ?
H20 C1 H1 109.5 . . ?
H19 C1 H1 109.5 . . ?
N1 C2 C3 116.95(13) . . ?
N1 C2 H18 108.1 . . ?
C3 C2 H18 108.1 . . ?
N1 C2 H27 108.1 . . ?
C3 C2 H27 108.1 . . ?
H18 C2 H27 107.3 . . ?
O1 C3 O12 128.05(14) . . ?
O1 C3 C2 113.77(13) . . ?
O12 C3 C2 118.06(13) . . ?
O3 C4 O13 127.07(14) . . ?
O3 C4 C5 119.76(13) . . ?
O13 C4 C5 113.14(12) . . ?
N2 C5 C4 117.44(12) . . ?
N2 C5 H6 107.9 . . ?
C4 C5 H6 107.9 . . ?
N2 C5 H5 107.9 . . ?
C4 C5 H5 107.9 . . ?
H6 C5 H5 107.2 . . ?
N2 C6 H29 109.5 . . ?
N2 C6 H2 109.5 . . ?
H29 C6 H2 109.5 . . ?
N2 C6 H28 109.5 . . ?
H29 C6 H28 109.5 . . ?
H2 C6 H28 109.5 . . ?
N2 C7 H4 109.5 . . ?
N2 C7 H33 109.5 . . ?
H4 C7 H33 109.5 . . ?
N2 C7 H3 109.5 . . ?
H4 C7 H3 109.5 . . ?
H33 C7 H3 109.5 . . ?
O2 C8 O14 127.05(14) . . ?
O2 C8 C9 114.53(13) . . ?
O14 C8 C9 118.39(13) . . ?
N3 C9 C8 116.22(11) . . ?
N3 C9 H7 108.2 . . ?
C8 C9 H7 108.2 . . ?
N3 C9 H8 108.2 . . ?
C8 C9 H8 108.2 . . ?
H7 C9 H8 107.4 . . ?
N3 C10 H10 109.5 . . ?
N3 C10 H9 109.5 . . ?
H10 C10 H9 109.5 . . ?
N3 C10 H11 109.5 . . ?
H10 C10 H11 109.5 . . ?
H9 C10 H11 109.5 . . ?
N3 C11 H14 109.5 . . ?
N3 C11 H12 109.5 . . ?
H14 C11 H12 109.5 . . ?
N3 C11 H13 109.5 . . ?
H14 C11 H13 109.5 . . ?
H12 C11 H13 109.5 . . ?
N3 C12 H16 109.5 . . ?
N3 C12 H17 109.5 . . ?
H16 C12 H17 109.5 . . ?
N3 C12 H15 109.5 . . ?
H16 C12 H15 109.5 . . ?
H17 C12 H15 109.5 . . ?
N1 C13 H23 109.5 . . ?
N1 C13 H21 109.5 . . ?
H23 C13 H21 109.5 . . ?
N1 C13 H22 109.5 . . ?
H23 C13 H22 109.5 . . ?
H21 C13 H22 109.5 . . ?
N1 C14 H25 109.5 . . ?
N1 C14 H24 109.5 . . ?
H25 C14 H24 109.5 . . ?
N1 C14 H26 109.5 . . ?
H25 C14 H26 109.5 . . ?
H24 C14 H26 109.5 . . ?
N2 C15 H30 109.5 . . ?
N2 C15 H32 109.5 . . ?
H30 C15 H32 109.5 . . ?
N2 C15 H31 109.5 . . ?
H30 C15 H31 109.5 . . ?
H32 C15 H31 109.5 . . ?
F6 C16 F5 108.94(16) . . ?
F6 C16 F1 108.85(15) . . ?
F5 C16 F1 108.43(15) . . ?
F6 C16 S1 111.42(12) . . ?
F5 C16 S1 110.73(12) . . ?
F1 C16 S1 108.41(13) . . ?
F4 C17 F3 108.82(15) . . ?
F4 C17 F2 108.48(14) . . ?
F3 C17 F2 108.07(14) . . ?
F4 C17 S2 111.26(12) . . ?
F3 C17 S2 111.15(11) . . ?
F2 C17 S2 108.97(13) . . ?
F11 C18 F7 108.04(17) . . ?
F11 C18 F10 108.49(18) . . ?
F7 C18 F10 108.05(16) . . ?
F11 C18 S3 111.53(13) . . ?
F7 C18 S3 110.15(13) . . ?
F10 C18 S3 110.48(14) . . ?
F12 C20 F9 108.60(14) . . ?
F12 C20 F8 108.36(13) . . ?
F9 C20 F8 107.82(14) . . ?
F12 C20 S4 111.22(11) . . ?
F9 C20 S4 110.06(11) . . ?
F8 C20 S4 110.67(12) . . ?
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
Ca1 O14 2.2906(11) . ?
Ca1 O14 2.2906(11) 2_665 ?
Ca1 O12 2.2979(11) . ?
Ca1 O12 2.2980(11) 2_665 ?
Ca1 O13 2.3548(11) . ?
Ca1 O13 2.3548(11) 2_665 ?
Ca2 O3 2.2954(11) . ?
Ca2 O3 2.2954(11) 2_565 ?
Ca2 O2 2.3485(11) 2_665 ?
Ca2 O2 2.3485(11) 1_455 ?
Ca2 O1 2.3753(11) 1_455 ?
Ca2 O1 2.3753(11) 2_665 ?
S1 O4 1.4315(12) . ?
S1 O5 1.4316(12) . ?
S1 N4 1.5820(13) . ?
S1 C16 1.8341(18) . ?
S2 O6 1.4339(12) . ?
S2 O7 1.4347(12) . ?
S2 N4 1.5699(13) . ?
S2 C17 1.8362(19) . ?
S3 O9 1.4307(13) . ?
S3 O10 1.4340(12) . ?
S3 N5 1.5757(14) . ?
S3 C18 1.8331(18) . ?
S4 O11 1.4283(12) . ?
S4 O8 1.4311(12) . ?
S4 N5 1.5784(14) . ?
S4 C20 1.8385(17) . ?
F1 C16 1.329(2) . ?
F2 C17 1.333(2) . ?
F3 C17 1.329(2) . ?
F4 C17 1.319(2) . ?
F5 C16 1.324(2) . ?
F6 C16 1.322(2) . ?
F7 C18 1.320(2) . ?
F8 C20 1.329(2) . ?
F9 C20 1.3285(18) . ?
F10 C18 1.321(2) . ?
F11 C18 1.316(2) . ?
F12 C20 1.3254(19) . ?
O1 C3 1.2405(19) . ?
O2 C8 1.2425(18) . ?
O3 C4 1.2412(18) . ?
O12 C3 1.2416(19) . ?
O13 C4 1.2490(18) . ?
O14 C8 1.2463(18) . ?
N1 C14 1.476(2) . ?
N1 C13 1.500(2) . ?
N1 C1 1.503(2) . ?
N1 C2 1.5140(19) . ?
N2 C15 1.496(2) . ?
N2 C7 1.4971(19) . ?
N2 C6 1.5002(19) . ?
N2 C5 1.5075(18) . ?
N3 C11 1.4972(19) . ?
N3 C12 1.5030(18) . ?
N3 C10 1.5048(19) . ?
N3 C9 1.5101(18) . ?
C1 H20 0.9800 . ?
C1 H19 0.9800 . ?
C1 H1 0.9800 . ?
C2 C3 1.541(2) . ?
C2 H18 0.9900 . ?
C2 H27 0.9900 . ?
C4 C5 1.5358(19) . ?
C5 H6 0.9900 . ?
C5 H5 0.9900 . ?
C6 H29 0.9800 . ?
C6 H2 0.9800 . ?
C6 H28 0.9800 . ?
C7 H4 0.9800 . ?
C7 H33 0.9800 . ?
C7 H3 0.9800 . ?
C8 C9 1.538(2) . ?
C9 H7 0.9900 . ?
C9 H8 0.9900 . ?
C10 H10 0.9800 . ?
C10 H9 0.9800 . ?
C10 H11 0.9800 . ?
C11 H14 0.9800 . ?
C11 H12 0.9800 . ?
C11 H13 0.9800 . ?
C12 H16 0.9800 . ?
C12 H17 0.9800 . ?
C12 H15 0.9800 . ?
C13 H23 0.9800 . ?
C13 H21 0.9800 . ?
C13 H22 0.9800 . ?
C14 H25 0.9800 . ?
C14 H24 0.9800 . ?
C14 H26 0.9800 . ?
C15 H30 0.9800 . ?
C15 H32 0.9800 . ?
C15 H31 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 S2 N4 S1 -163.06(11) . . . . ?
O7 S2 N4 S1 -27.72(14) . . . . ?
C17 S2 N4 S1 86.92(12) . . . . ?
O4 S1 N4 S2 124.83(11) . . . . ?
O5 S1 N4 S2 -12.97(15) . . . . ?
C16 S1 N4 S2 -126.42(11) . . . . ?
O9 S3 N5 S4 162.98(10) . . . . ?
O10 S3 N5 S4 26.91(14) . . . . ?
C18 S3 N5 S4 -86.84(12) . . . . ?
O11 S4 N5 S3 152.11(10) . . . . ?
O8 S4 N5 S3 15.34(14) . . . . ?
C20 S4 N5 S3 -97.81(11) . . . . ?
C14 N1 C2 C3 -55.2(2) . . . . ?
C13 N1 C2 C3 68.3(2) . . . . ?
C1 N1 C2 C3 -173.86(15) . . . . ?
Ca2 O1 C3 O12 -10.0(3) 1_655 . . . ?
Ca2 O1 C3 C2 165.78(12) 1_655 . . . ?
Ca1 O12 C3 O1 -25.9(3) . . . . ?
Ca1 O12 C3 C2 158.50(16) . . . . ?
N1 C2 C3 O1 157.57(15) . . . . ?
N1 C2 C3 O12 -26.2(2) . . . . ?
Ca2 O3 C4 O13 -46.9(4) . . . . ?
Ca2 O3 C4 C5 131.1(2) . . . . ?
Ca1 O13 C4 O3 0.7(2) . . . . ?
Ca1 O13 C4 C5 -177.47(9) . . . . ?
C15 N2 C5 C4 58.74(17) . . . . ?
C7 N2 C5 C4 177.20(13) . . . . ?
C6 N2 C5 C4 -64.18(16) . . . . ?
O3 C4 C5 N2 20.8(2) . . . . ?
O13 C4 C5 N2 -160.91(13) . . . . ?
Ca2 O2 C8 O14 7.2(2) 1_655 . . . ?
Ca2 O2 C8 C9 -170.54(9) 1_655 . . . ?
Ca1 O14 C8 O2 30.1(4) . . . . ?
Ca1 O14 C8 C9 -152.3(2) . . . . ?
C11 N3 C9 C8 53.10(16) . . . . ?
C12 N3 C9 C8 -69.58(16) . . . . ?
C10 N3 C9 C8 171.56(12) . . . . ?
O2 C8 C9 N3 -142.58(13) . . . . ?
O14 C8 C9 N3 39.48(19) . . . . ?
O4 S1 C16 F6 175.84(13) . . . . ?
O5 S1 C16 F6 -59.52(15) . . . . ?
N4 S1 C16 F6 62.27(15) . . . . ?
O4 S1 C16 F5 54.43(14) . . . . ?
O5 S1 C16 F5 179.07(12) . . . . ?
N4 S1 C16 F5 -59.14(13) . . . . ?
O4 S1 C16 F1 -64.40(14) . . . . ?
O5 S1 C16 F1 60.24(14) . . . . ?
N4 S1 C16 F1 -177.97(12) . . . . ?
O6 S2 C17 F4 -55.64(14) . . . . ?
O7 S2 C17 F4 179.75(12) . . . . ?
N4 S2 C17 F4 57.79(14) . . . . ?
O6 S2 C17 F3 -177.09(12) . . . . ?
O7 S2 C17 F3 58.30(13) . . . . ?
N4 S2 C17 F3 -63.66(13) . . . . ?
O6 S2 C17 F2 63.92(13) . . . . ?
O7 S2 C17 F2 -60.69(13) . . . . ?
N4 S2 C17 F2 177.35(11) . . . . ?
O9 S3 C18 F11 173.23(14) . . . . ?
O10 S3 C18 F11 -62.91(16) . . . . ?
N5 S3 C18 F11 60.35(16) . . . . ?
O9 S3 C18 F7 -66.81(16) . . . . ?
O10 S3 C18 F7 57.06(15) . . . . ?
N5 S3 C18 F7 -179.69(13) . . . . ?
O9 S3 C18 F10 52.48(16) . . . . ?
O10 S3 C18 F10 176.35(14) . . . . ?
N5 S3 C18 F10 -60.39(16) . . . . ?
O11 S4 C20 F12 166.56(12) . . . . ?
O8 S4 C20 F12 -68.23(13) . . . . ?
N5 S4 C20 F12 52.83(13) . . . . ?
O11 S4 C20 F9 -73.03(14) . . . . ?
O8 S4 C20 F9 52.18(14) . . . . ?
N5 S4 C20 F9 173.24(12) . . . . ?
O11 S4 C20 F8 46.04(13) . . . . ?
O8 S4 C20 F8 171.26(11) . . . . ?
N5 S4 C20 F8 -67.68(12) . . . . ?
