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

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

data_DW_B1_0029
_audit_block_doi                 10.5517/ccdc.csd.cc1nbx74
_database_code_depnum_ccdc_archive 'CCDC 1529826'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7CC01938F 2017
_audit_update_record             
;
2017-01-26 deposited with the CCDC.
2018-10-10 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2014/7

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.0  (Andrew D. Bond, July 2015)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Evan Keyzer'
_cambridge_user_crsid            ek406
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             enk-2-8
_cambridge_data_id               DW_B1_0029
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H12 Ca F2 N4 O2 P +, F6 P -'
_chemical_formula_sum            'C8 H12 Ca F8 N4 O2 P2'
_chemical_formula_weight         450.24
_chemical_absolute_configuration unk

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'
N N 0.0311 0.0180 '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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'

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

_cell_length_a                   12.9151(14)
_cell_length_b                   20.3651(14)
_cell_length_c                   7.0543(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1855.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9961
_cell_measurement_theta_min      4.05
_cell_measurement_theta_max      66.57

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_F_000             904
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    5.405
_shelx_estimated_absorpt_T_min   0.397
_shelx_estimated_absorpt_T_max   0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4963
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11439
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         4.053
_diffrn_reflns_theta_max         66.551
_diffrn_reflns_theta_full        66.551
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1669
_reflns_number_gt                1644
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.996

_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       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          'Refined as a 2-component inversion 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)+(0.0695P)²+4.5812P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_Flack   0.31(3)
_refine_ls_abs_structure_details 'Refined as an inversion twin.'
_refine_ls_number_reflns         1669
_refine_ls_number_parameters     130
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0435
_refine_ls_wR_factor_ref         0.1170
_refine_ls_wR_factor_gt          0.1165
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.073

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 0.5000 0.55111(5) 0.90444(19) 0.0198(3) Uani 1 2 d S T P . .
P1 P 0.5000 0.60526(7) 0.4076(3) 0.0249(4) Uani 1 2 d S T P . .
O1 O 0.5000 0.5622(3) 0.5743(7) 0.0246(11) Uani 1 2 d S T P . .
O2 O 0.5000 0.5722(3) 0.2240(8) 0.0327(12) Uani 1 2 d S T P . .
F1 F 0.5902(3) 0.65337(16) 0.4186(7) 0.0577(10) Uani 1 1 d . . . . .
N1 N 0.6152(4) 0.6513(2) 0.8945(9) 0.0456(12) Uani 1 1 d . . . . .
N2 N 0.3177(3) 0.5074(2) 0.8652(7) 0.0366(12) Uani 1 1 d . . . . .
C1 C 0.6508(5) 0.7011(3) 0.8626(8) 0.0385(14) Uani 1 1 d . . . . .
C2 C 0.6942(7) 0.7658(3) 0.8219(13) 0.063(2) Uani 1 1 d . . . . .
H2A H 0.6692 0.7810 0.6983 0.095 Uiso 1 1 calc R U . . .
H2B H 0.7700 0.7630 0.8195 0.095 Uiso 1 1 calc R U . . .
H2C H 0.6727 0.7968 0.9204 0.095 Uiso 1 1 calc R U . . .
C3 C 0.2449(4) 0.4836(3) 0.8142(9) 0.0351(12) Uani 1 1 d . . . . .
C4 C 0.1506(5) 0.4521(4) 0.7444(12) 0.0557(18) Uani 1 1 d . . . . .
H4A H 0.0975 0.4855 0.7213 0.083 Uiso 1 1 calc R U . . .
H4B H 0.1254 0.4207 0.8391 0.083 Uiso 1 1 calc R U . . .
H4C H 0.1657 0.4288 0.6259 0.083 Uiso 1 1 calc R U . . .
P2 P 0.0000 0.35104(10) 0.2823(3) 0.0389(5) Uani 1 2 d S T P . .
F2 F 0.0000 0.4191(3) 0.3918(16) 0.094(2) Uani 1 2 d S T P . .
F3 F 0.0000 0.2839(4) 0.1803(16) 0.126(4) Uani 1 2 d S T P . .
F4 F 0.1132(6) 0.3499(6) 0.296(2) 0.251(9) Uani 1 1 d . . . . .
F5 F 0.0000 0.3834(7) 0.0956(19) 0.221(9) Uani 1 2 d S T P . .
F6 F 0.0000 0.3199(8) 0.4750(19) 0.247(12) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O2 2.295(6) 1_556 ?
Ca1 O1 2.340(5) . ?
Ca1 N1 2.525(4) 4_655 ?
Ca1 N1 2.525(4) . ?
Ca1 N2 2.532(4) 4_655 ?
Ca1 N2 2.532(4) . ?
Ca1 O1 2.601(5) 2_665 ?
Ca1 O2 2.816(6) 2_665 ?
Ca1 P1 3.1844(18) 2_665 ?
Ca1 Ca1 4.0955(11) 2_665 ?
Ca1 Ca1 4.0955(11) 2_664 ?
P1 O2 1.460(6) . ?
P1 O1 1.466(6) . ?
P1 F1 1.524(3) . ?
P1 F1 1.524(3) 4_655 ?
P1 Ca1 3.1844(18) 2_664 ?
O1 Ca1 2.600(5) 2_664 ?
O2 Ca1 2.295(6) 1_554 ?
O2 Ca1 2.816(6) 2_664 ?
N1 C1 1.138(7) . ?
N2 C3 1.117(7) . ?
C1 C2 1.460(8) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.463(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
P2 F4 1.465(7) . ?
P2 F4 1.465(7) 4 ?
P2 F5 1.473(12) . ?
P2 F6 1.500(13) . ?
P2 F3 1.545(8) . ?
P2 F2 1.586(7) . ?

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
O2 Ca1 O1 163.64(18) 1_556 . ?
O2 Ca1 N1 82.9(2) 1_556 4_655 ?
O1 Ca1 N1 83.93(19) . 4_655 ?
O2 Ca1 N1 82.9(2) 1_556 . ?
O1 Ca1 N1 83.93(19) . . ?
N1 Ca1 N1 72.2(2) 4_655 . ?
O2 Ca1 N2 99.98(12) 1_556 4_655 ?
O1 Ca1 N2 85.71(12) . 4_655 ?
N1 Ca1 N2 145.94(18) 4_655 4_655 ?
N1 Ca1 N2 74.52(16) . 4_655 ?
O2 Ca1 N2 99.98(12) 1_556 . ?
O1 Ca1 N2 85.71(12) . . ?
N1 Ca1 N2 74.52(16) 4_655 . ?
N1 Ca1 N2 145.94(17) . . ?
N2 Ca1 N2 136.8(2) 4_655 . ?
O2 Ca1 O1 73.37(18) 1_556 2_665 ?
O1 Ca1 O1 122.99(14) . 2_665 ?
N1 Ca1 O1 136.85(16) 4_655 2_665 ?
N1 Ca1 O1 136.85(16) . 2_665 ?
N2 Ca1 O1 74.84(11) 4_655 2_665 ?
N2 Ca1 O1 74.84(11) . 2_665 ?
O2 Ca1 O2 127.68(16) 1_556 2_665 ?
O1 Ca1 O2 68.68(16) . 2_665 ?
N1 Ca1 O2 135.06(15) 4_655 2_665 ?
N1 Ca1 O2 135.06(15) . 2_665 ?
N2 Ca1 O2 68.73(11) 4_655 2_665 ?
N2 Ca1 O2 68.72(11) . 2_665 ?
O1 Ca1 O2 54.31(13) 2_665 2_665 ?
O2 Ca1 P1 100.40(16) 1_556 2_665 ?
O1 Ca1 P1 95.96(14) . 2_665 ?
N1 Ca1 P1 143.88(12) 4_655 2_665 ?
N1 Ca1 P1 143.88(12) . 2_665 ?
N2 Ca1 P1 69.48(11) 4_655 2_665 ?
N2 Ca1 P1 69.47(11) . 2_665 ?
O1 Ca1 P1 27.03(12) 2_665 2_665 ?
O2 Ca1 P1 27.28(13) 2_665 2_665 ?
O2 Ca1 Ca1 41.35(15) 1_556 2_665 ?
O1 Ca1 Ca1 155.01(14) . 2_665 ?
N1 Ca1 Ca1 115.74(16) 4_655 2_665 ?
N1 Ca1 Ca1 115.74(16) . 2_665 ?
N2 Ca1 Ca1 85.16(11) 4_655 2_665 ?
N2 Ca1 Ca1 85.16(11) . 2_665 ?
O1 Ca1 Ca1 32.02(12) 2_665 2_665 ?
O2 Ca1 Ca1 86.33(13) 2_665 2_665 ?
P1 Ca1 Ca1 59.05(5) 2_665 2_665 ?
O2 Ca1 Ca1 160.26(16) 1_556 2_664 ?
O1 Ca1 Ca1 36.10(13) . 2_664 ?
N1 Ca1 Ca1 112.75(15) 4_655 2_664 ?
N1 Ca1 Ca1 112.75(15) . 2_664 ?
N2 Ca1 Ca1 74.17(12) 4_655 2_664 ?
N2 Ca1 Ca1 74.17(12) . 2_664 ?
O1 Ca1 Ca1 86.89(12) 2_665 2_664 ?
O2 Ca1 Ca1 32.58(12) 2_665 2_664 ?
P1 Ca1 Ca1 59.86(5) 2_665 2_664 ?
Ca1 Ca1 Ca1 118.91(5) 2_665 2_664 ?
O2 P1 O1 115.9(3) . . ?
O2 P1 F1 110.0(2) . . ?
O1 P1 F1 110.1(2) . . ?
O2 P1 F1 110.0(2) . 4_655 ?
O1 P1 F1 110.1(2) . 4_655 ?
F1 P1 F1 99.7(3) . 4_655 ?
O2 P1 Ca1 62.2(2) . 2_664 ?
O1 P1 Ca1 53.7(2) . 2_664 ?
F1 P1 Ca1 130.03(17) . 2_664 ?
F1 P1 Ca1 130.04(17) 4_655 2_664 ?
P1 O1 Ca1 148.9(3) . . ?
P1 O1 Ca1 99.3(3) . 2_664 ?
Ca1 O1 Ca1 111.9(2) . 2_664 ?
P1 O2 Ca1 163.4(4) . 1_554 ?
P1 O2 Ca1 90.6(3) . 2_664 ?
Ca1 O2 Ca1 106.1(2) 1_554 2_664 ?
C1 N1 Ca1 164.8(6) . . ?
C3 N2 Ca1 165.9(5) . . ?
N1 C1 C2 178.7(7) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 C4 179.0(7) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
F4 P2 F4 172.4(14) . 4 ?
F4 P2 F5 93.7(7) . . ?
F4 P2 F5 93.7(7) 4 . ?
F4 P2 F6 86.3(7) . . ?
F4 P2 F6 86.3(7) 4 . ?
F5 P2 F6 178.5(9) . . ?
F4 P2 F3 90.9(4) . . ?
F4 P2 F3 90.9(4) 4 . ?
F5 P2 F3 88.8(7) . . ?
F6 P2 F3 92.7(8) . . ?
F4 P2 F2 89.0(4) . . ?
F4 P2 F2 89.0(4) 4 . ?
F5 P2 F2 92.6(8) . . ?
F6 P2 F2 85.9(8) . . ?
F3 P2 F2 178.6(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 P1 O1 Ca1 180.000(2) . . . . ?
F1 P1 O1 Ca1 54.5(2) . . . . ?
F1 P1 O1 Ca1 -54.5(2) 4_655 . . . ?
Ca1 P1 O1 Ca1 180.000(4) 2_664 . . . ?
O2 P1 O1 Ca1 0.000(1) . . . 2_664 ?
F1 P1 O1 Ca1 -125.5(2) . . . 2_664 ?
F1 P1 O1 Ca1 125.5(2) 4_655 . . 2_664 ?
O1 P1 O2 Ca1 180.000(5) . . . 1_554 ?
F1 P1 O2 Ca1 -54.40(19) . . . 1_554 ?
F1 P1 O2 Ca1 54.40(19) 4_655 . . 1_554 ?
Ca1 P1 O2 Ca1 180.000(7) 2_664 . . 1_554 ?
O1 P1 O2 Ca1 0.000(1) . . . 2_664 ?
F1 P1 O2 Ca1 125.60(19) . . . 2_664 ?
F1 P1 O2 Ca1 -125.60(19) 4_655 . . 2_664 ?

####################################################################### 
# 
# 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_DW_B2_0130
_audit_block_doi                 10.5517/ccdc.csd.cc1nbxb7
_database_code_depnum_ccdc_archive 'CCDC 1529829'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7CC01938F 2017
_audit_update_record             
;
2017-01-26 deposited with the CCDC.
2018-10-10 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2014/7

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.0  (Andrew D. Bond, July 2015)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Evan Keyzer'
_cambridge_user_crsid            ek406
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             enk-3-9
_cambridge_data_id               DW_B2_0130
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C34 H66 Ca4 F10 N2 O15 P 3+, 3(F6 P -), 2(C2 H3 N)'
_chemical_formula_sum            'C38 H72 Ca4 F28 N4 O15 P4'
_chemical_formula_weight         1641.19

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'
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'
F F 0.0727 0.0534 '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'
Ca Ca 0.3641 1.2855 '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                   12.7225(6)
_cell_length_b                   13.4339(6)
_cell_length_c                   21.7776(10)
_cell_angle_alpha                73.456(2)
_cell_angle_beta                 89.794(2)
_cell_angle_gamma                68.867(2)
_cell_volume                     3307.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9888
_cell_measurement_theta_min      3.75
_cell_measurement_theta_max      59.14

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_F_000             1680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    5.042
_shelx_estimated_absorpt_T_min   0.464
_shelx_estimated_absorpt_T_max   0.633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5411
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34975
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.668
_diffrn_reflns_theta_max         59.315
_diffrn_reflns_theta_full        59.315
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             9471
_reflns_number_gt                8222
_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       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_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)+(0.0557P)²+8.9532P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9471
_refine_ls_number_parameters     972
_refine_ls_number_restraints     426
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_ref         0.1388
_refine_ls_wR_factor_gt          0.1332
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.078

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 0.43650(7) 0.28906(7) 0.23781(4) 0.0327(2) Uani 1 1 d . . . . .
Ca2 Ca 0.19653(6) 0.26812(6) 0.31337(3) 0.02313(19) Uani 1 1 d . . . . .
Ca3 Ca 0.30056(6) 0.48387(6) 0.31921(4) 0.02375(19) Uani 1 1 d . . . . .
Ca4 Ca 0.16743(7) 0.49851(6) 0.16974(4) 0.02488(19) Uani 1 1 d . . . . .
O1 O 0.2945(2) 0.1175(2) 0.41479(13) 0.0312(6) Uani 1 1 d . . . . .
O2 O 0.3421(2) 0.0921(2) 0.29788(13) 0.0338(7) Uani 1 1 d . . . . .
O3 O 0.1111(3) 0.1636(3) 0.26841(16) 0.0436(8) Uani 1 1 d . . . . .
O4 O -0.0045(2) 0.3070(3) 0.32992(15) 0.0417(8) Uani 1 1 d . . . . .
O5 O 0.1416(2) 0.3196(2) 0.41420(13) 0.0341(7) Uani 1 1 d . . . . .
O6 O 0.3954(2) 0.6216(2) 0.28163(14) 0.0381(7) Uani 1 1 d . . . . .
O7 O 0.5154(2) 0.3985(2) 0.32846(14) 0.0359(7) Uani 1 1 d . . . . .
O8 O 0.3890(2) 0.4204(3) 0.43057(14) 0.0387(7) Uani 1 1 d . . . . .
O9 O 0.1742(2) 0.5585(3) 0.39382(14) 0.0383(7) Uani 1 1 d . . . . .
O10 O 0.1662(2) 0.6797(2) 0.27098(15) 0.0379(7) Uani 1 1 d . . . . .
O11 O 0.0001(3) 0.6697(2) 0.15406(15) 0.0433(8) Uani 1 1 d . . . . .
O12 O -0.0186(3) 0.4746(3) 0.17239(14) 0.0425(8) Uani 1 1 d . . . . .
O13 O 0.1215(3) 0.4344(3) 0.07848(14) 0.0421(8) Uani 1 1 d . . . . .
O14 O 0.3203(3) 0.4574(3) 0.09538(14) 0.0391(7) Uani 1 1 d . . . . .
O15 O 0.1834(3) 0.6700(2) 0.09558(14) 0.0383(7) Uani 1 1 d . . . . .
F7 F 0.33584(17) 0.47465(17) 0.21904(10) 0.0251(5) Uani 1 1 d . U . . .
F8 F 0.35791(17) 0.29640(17) 0.32981(10) 0.0249(5) Uani 1 1 d . U . . .
F9 F 0.25529(19) 0.31119(17) 0.21232(10) 0.0285(5) Uani 1 1 d . U . . .
F10 F 0.14719(17) 0.45965(17) 0.27816(9) 0.0250(5) Uani 1 1 d . U . . .
N1 N 0.4930(4) 0.1518(4) 0.1760(2) 0.0583(12) Uani 1 1 d D . . . .
C1 C 0.5405(5) 0.0720(5) 0.1638(3) 0.0683(17) Uani 1 1 d D . . . .
C2 C 0.6015(9) -0.0316(7) 0.1491(6) 0.138(4) Uani 1 1 d D . . . .
H2A H 0.6765 -0.0689 0.1740 0.208 Uiso 1 1 calc R U . . .
H2B H 0.6101 -0.0147 0.1030 0.208 Uiso 1 1 calc R U . . .
H2C H 0.5588 -0.0809 0.1604 0.208 Uiso 1 1 calc R U . . .
N2 N 0.6098(3) 0.1385(3) 0.30814(19) 0.0477(10) Uani 1 1 d D . . . .
C3 C 0.6965(4) 0.0745(4) 0.3304(2) 0.0386(11) Uani 1 1 d D . . . .
C4 C 0.8084(4) -0.0086(4) 0.3591(2) 0.0487(12) Uani 1 1 d D . . . .
H4A H 0.8042 -0.0829 0.3747 0.073 Uiso 1 1 calc R U . . .
H4B H 0.8342 0.0099 0.3952 0.073 Uiso 1 1 calc R U . . .
H4C H 0.8619 -0.0086 0.3267 0.073 Uiso 1 1 calc R U . . .
N3 N 0.6216(13) 0.7162(13) 0.1157(7) 0.237(6) Uani 1 1 d D U . . .
C35 C 0.5732(11) 0.7631(11) 0.0663(6) 0.141(4) Uani 1 1 d D U . . .
C36 C 0.5171(13) 0.8285(13) 0.0011(6) 0.220(7) Uani 1 1 d D U . . .
H36A H 0.5745 0.8313 -0.0288 0.331 Uiso 1 1 calc R U . . .
H36B H 0.4699 0.9048 0.0006 0.331 Uiso 1 1 calc R U . . .
H36C H 0.4695 0.7933 -0.0121 0.331 Uiso 1 1 calc R U . . .
N4 N 0.9277(6) -0.0214(4) 0.2166(2) 0.0880(19) Uani 1 1 d D . . . .
C37 C 0.9065(5) 0.0237(4) 0.1637(2) 0.0612(15) Uani 1 1 d D . . . .
C38 C 0.8829(7) 0.0810(5) 0.0954(2) 0.085(2) Uani 1 1 d D . . . .
H38A H 0.9182 0.0275 0.0717 0.128 Uiso 1 1 calc R U . . .
H38B H 0.9139 0.1401 0.0848 0.128 Uiso 1 1 calc R U . . .
H38C H 0.8008 0.1143 0.0832 0.128 Uiso 1 1 calc R U . . .
C5 C 0.4047(4) 0.0434(4) 0.4085(2) 0.0376(10) Uani 1 1 d . . . . .
H5A H 0.4359 -0.0187 0.4491 0.045 Uiso 1 1 calc R U . . .
H5B H 0.4568 0.0843 0.3990 0.045 Uiso 1 1 calc R U . . .
C6 C 0.3932(4) -0.0013(4) 0.3549(2) 0.0412(11) Uani 1 1 d . . . . .
H6A H 0.4686 -0.0500 0.3476 0.049 Uiso 1 1 calc R U . . .
H6B H 0.3451 -0.0463 0.3658 0.049 Uiso 1 1 calc R U . . .
C7 C 0.2964(4) 0.0621(4) 0.2486(2) 0.0418(11) Uani 1 1 d . . . . .
H7A H 0.3484 -0.0124 0.2472 0.050 Uiso 1 1 calc R U . . .
H7B H 0.2906 0.1173 0.2062 0.050 Uiso 1 1 calc R U . . .
C8 C 0.1807(4) 0.0588(4) 0.2613(2) 0.0444(12) Uani 1 1 d . . . . .
H8A H 0.1475 0.0453 0.2248 0.053 Uiso 1 1 calc R U . . .
H8B H 0.1869 -0.0025 0.3010 0.053 Uiso 1 1 calc R U . . .
C9 C 0.0010(5) 0.1709(7) 0.2832(6) 0.125(4) Uani 1 1 d . . . . .
H9A H -0.0423 0.1779 0.2435 0.150 Uiso 1 1 calc R U . . .
H9B H 0.0080 0.0988 0.3150 0.150 Uiso 1 1 calc R U . . .
C10 C -0.0590(6) 0.2499(8) 0.3056(4) 0.098(3) Uani 1 1 d . . . . .
H10A H -0.0982 0.2176 0.3405 0.118 Uiso 1 1 calc R U . . .
H10B H -0.1183 0.3060 0.2708 0.118 Uiso 1 1 calc R U . . .
C11 C -0.0505(4) 0.3427(4) 0.3832(2) 0.0467(12) Uani 1 1 d . . . . .
H11A H -0.0524 0.2782 0.4186 0.056 Uiso 1 1 calc R U . . .
H11B H -0.1288 0.3988 0.3701 0.056 Uiso 1 1 calc R U . . .
C12 C 0.0241(4) 0.3928(4) 0.4047(2) 0.0427(11) Uani 1 1 d . . . . .
H12A H 0.0140 0.4649 0.3720 0.051 Uiso 1 1 calc R U . . .
H12B H 0.0014 0.4083 0.4456 0.051 Uiso 1 1 calc R U . . .
C13 C 0.1721(4) 0.2265(4) 0.4723(2) 0.0458(12) Uani 1 1 d . . . . .
H13A H 0.1218 0.1844 0.4741 0.055 Uiso 1 1 calc R U . . .
H13B H 0.1655 0.2531 0.5106 0.055 Uiso 1 1 calc R U . . .
C14 C 0.2917(4) 0.1542(4) 0.4703(2) 0.0429(11) Uani 1 1 d . . . . .
H14A H 0.3415 0.1970 0.4677 0.051 Uiso 1 1 calc R U . . .
H14B H 0.3183 0.0890 0.5098 0.051 Uiso 1 1 calc R U . . .
C15 C 0.5020(4) 0.5755(4) 0.2573(2) 0.0438(12) Uani 1 1 d . . . . .
H15A H 0.5385 0.6311 0.2456 0.053 Uiso 1 1 calc R U . . .
H15B H 0.4898 0.5550 0.2184 0.053 Uiso 1 1 calc R U . . .
C16 C 0.5750(4) 0.4743(4) 0.3094(3) 0.0482(12) Uani 1 1 d . . . . .
H16A H 0.6474 0.4369 0.2936 0.058 Uiso 1 1 calc R U . . .
H16B H 0.5922 0.4960 0.3468 0.058 Uiso 1 1 calc R U . . .
C17 C 0.5577(4) 0.3206(4) 0.3920(2) 0.0403(11) Uani 1 1 d . . . . .
H17A H 0.6415 0.2931 0.3975 0.048 Uiso 1 1 calc R U . . .
H17B H 0.5355 0.2555 0.3972 0.048 Uiso 1 1 calc R U . . .
C18 C 0.5110(4) 0.3760(5) 0.4425(2) 0.0498(13) Uani 1 1 d . . . . .
H18A H 0.5362 0.3208 0.4860 0.060 Uiso 1 1 calc R U . . .
H18B H 0.5384 0.4371 0.4401 0.060 Uiso 1 1 calc R U . . .
C19 C 0.3365(4) 0.4889(4) 0.4702(2) 0.0441(12) Uani 1 1 d . . . . .
H19A H 0.3515 0.5590 0.4573 0.053 Uiso 1 1 calc R U . . .
H19B H 0.3668 0.4487 0.5160 0.053 Uiso 1 1 calc R U . . .
C20 C 0.2124(4) 0.5145(5) 0.4612(2) 0.0453(12) Uani 1 1 d . . . . .
H20A H 0.1971 0.4455 0.4802 0.054 Uiso 1 1 calc R U . . .
H20B H 0.1713 0.5700 0.4833 0.054 Uiso 1 1 calc R U . . .
C21 C 0.0880(4) 0.6688(4) 0.3730(2) 0.0468(12) Uani 1 1 d . . . . .
H21A H 0.1148 0.7228 0.3841 0.056 Uiso 1 1 calc R U . . .
H21B H 0.0188 0.6698 0.3941 0.056 Uiso 1 1 calc R U . . .
C22 C 0.0633(4) 0.6994(4) 0.3019(2) 0.0433(11) Uani 1 1 d . . . . .
H22A H 0.0225 0.6546 0.2919 0.052 Uiso 1 1 calc R U . . .
H22B H 0.0135 0.7795 0.2848 0.052 Uiso 1 1 calc R U . . .
C23 C 0.2144(4) 0.7639(4) 0.2653(3) 0.0482(12) Uani 1 1 d . . . . .
H23A H 0.2281 0.7715 0.3081 0.058 Uiso 1 1 calc R U . . .
H23B H 0.1623 0.8373 0.2368 0.058 Uiso 1 1 calc R U . . .
C24 C 0.3225(4) 0.7257(4) 0.2373(3) 0.0476(12) Uani 1 1 d . . . . .
H24A H 0.3088 0.7155 0.1952 0.057 Uiso 1 1 calc R U . . .
H24B H 0.3581 0.7820 0.2305 0.057 Uiso 1 1 calc R U . . .
C25 C -0.1118(4) 0.6717(4) 0.1626(2) 0.0499(13) Uani 1 1 d . . . . .
H25A H -0.1572 0.6973 0.1203 0.060 Uiso 1 1 calc R U . . .
H25B H -0.1501 0.7230 0.1876 0.060 Uiso 1 1 calc R U . . .
C26 C -0.0990(4) 0.5536(4) 0.1985(3) 0.0487(12) Uani 1 1 d . . . . .
H26A H -0.0736 0.5368 0.2445 0.058 Uiso 1 1 calc R U . . .
H26B H -0.1734 0.5462 0.1959 0.058 Uiso 1 1 calc R U . . .
C27 C -0.0611(5) 0.4742(6) 0.1117(3) 0.0646(16) Uani 1 1 d . . . . .
H27A H -0.0840 0.5495 0.0798 0.078 Uiso 1 1 calc R U . . .
H27B H -0.1277 0.4521 0.1165 0.078 Uiso 1 1 calc R U . . .
C28 C 0.0334(5) 0.3911(5) 0.0901(3) 0.0622(16) Uani 1 1 d . . . . .
H28A H 0.0613 0.3174 0.1239 0.075 Uiso 1 1 calc R U . . .
H28B H 0.0069 0.3816 0.0502 0.075 Uiso 1 1 calc R U . . .
C29 C 0.2212(5) 0.3584(4) 0.0631(2) 0.0502(13) Uani 1 1 d . . . . .
H29A H 0.2025 0.3332 0.0275 0.060 Uiso 1 1 calc R U . . .
H29B H 0.2576 0.2919 0.1011 0.060 Uiso 1 1 calc R U . . .
C30 C 0.2983(5) 0.4203(5) 0.0432(2) 0.0570(14) Uani 1 1 d . . . . .
H30A H 0.3702 0.3707 0.0327 0.068 Uiso 1 1 calc R U . . .
H30B H 0.2623 0.4854 0.0045 0.068 Uiso 1 1 calc R U . . .
C31 C 0.3594(4) 0.5485(4) 0.0757(2) 0.0451(12) Uani 1 1 d . . . . .
H31A H 0.4125 0.5360 0.0428 0.054 Uiso 1 1 calc R U . . .
H31B H 0.4009 0.5510 0.1132 0.054 Uiso 1 1 calc R U . . .
C32 C 0.2619(4) 0.6583(4) 0.0483(2) 0.0493(13) Uani 1 1 d . . . . .
H32A H 0.2893 0.7208 0.0382 0.059 Uiso 1 1 calc R U . . .
H32B H 0.2245 0.6596 0.0082 0.059 Uiso 1 1 calc R U . . .
C33 C 0.0803(4) 0.7641(4) 0.0697(2) 0.0466(12) Uani 1 1 d . . . . .
H33A H 0.0414 0.7525 0.0346 0.056 Uiso 1 1 calc R U . . .
H33B H 0.0966 0.8328 0.0519 0.056 Uiso 1 1 calc R U . . .
C34 C 0.0078(4) 0.7755(4) 0.1224(2) 0.0467(12) Uani 1 1 d . . . . .
H34A H 0.0405 0.8004 0.1536 0.056 Uiso 1 1 calc R U . . .
H34B H -0.0688 0.8324 0.1047 0.056 Uiso 1 1 calc R U . . .
P1 P 0.67812(10) 0.34391(12) 0.14461(6) 0.0485(3) Uani 0.801(11) 1 d D . P A 1
F1 F 0.5634(2) 0.3606(2) 0.17975(13) 0.0573(8) Uani 0.801(11) 1 d D U P A 1
F2 F 0.6268(4) 0.4729(4) 0.1035(3) 0.086(2) Uani 0.801(11) 1 d D U P A 1
F3 F 0.6210(4) 0.3190(6) 0.0904(2) 0.087(2) Uani 0.801(11) 1 d D U P A 1
F4 F 0.7905(2) 0.3271(3) 0.11009(15) 0.0692(9) Uani 0.801(11) 1 d D U P A 1
F5 F 0.7265(4) 0.2207(4) 0.1861(3) 0.100(3) Uani 0.801(11) 1 d D U P A 1
F6 F 0.7285(4) 0.3810(6) 0.1957(2) 0.088(2) Uani 0.801(11) 1 d D U P A 1
P1A P 0.67812(10) 0.34391(12) 0.14461(6) 0.0485(3) Uani 0.199(11) 1 d D . P A 2
F1A F 0.5634(2) 0.3606(2) 0.17975(13) 0.0573(8) Uani 0.199(11) 1 d D U P A 2
F2A F 0.6783(14) 0.4531(12) 0.1539(11) 0.096(9) Uani 0.199(11) 1 d D U P A 2
F3A F 0.6064(8) 0.4076(19) 0.0785(4) 0.103(10) Uani 0.199(11) 1 d D U P A 2
F4A F 0.7905(2) 0.3271(3) 0.11009(15) 0.0692(9) Uani 0.199(11) 1 d D U P A 2
F5A F 0.6769(13) 0.2305(12) 0.1373(11) 0.080(8) Uani 0.199(11) 1 d D U P A 2
F6A F 0.7485(8) 0.2755(18) 0.2121(4) 0.108(9) Uani 0.199(11) 1 d D U P A 2
P2 P 0.82575(9) 0.13867(9) 0.52397(5) 0.0329(3) Uani 1 1 d D . . . .
F11 F 0.8822(3) 0.0071(2) 0.55137(18) 0.0746(10) Uani 1 1 d D U . . .
F12 F 0.8508(3) 0.1347(3) 0.45334(14) 0.0624(8) Uani 1 1 d D U . . .
F13 F 0.9434(2) 0.1502(2) 0.53603(14) 0.0531(7) Uani 1 1 d D U . . .
F14 F 0.7063(2) 0.1298(2) 0.51159(13) 0.0505(7) Uani 1 1 d D U . . .
F15 F 0.7981(3) 0.1461(3) 0.59391(14) 0.0742(10) Uani 1 1 d D U . . .
F16 F 0.7684(2) 0.2717(2) 0.49599(14) 0.0522(7) Uani 1 1 d D U . . .
P3 P 0.70689(11) 0.71681(11) 0.34411(7) 0.0493(3) Uani 0.550(9) 1 d D . P B 1
F17 F 0.8082(6) 0.6316(7) 0.3957(3) 0.110(4) Uani 0.550(9) 1 d D U P B 1
F18 F 0.6263(8) 0.6602(8) 0.3761(4) 0.113(4) Uani 0.550(9) 1 d D U P B 1
F19 F 0.6078(6) 0.8039(7) 0.2916(3) 0.110(4) Uani 0.550(9) 1 d D U P B 1
F20 F 0.7901(6) 0.7722(7) 0.3081(4) 0.101(3) Uani 0.550(9) 1 d D U P B 1
F21 F 0.7375(7) 0.6376(7) 0.2995(4) 0.107(3) Uani 0.550(9) 1 d D U P B 1
F22 F 0.6774(7) 0.7977(7) 0.3856(4) 0.096(3) Uani 0.550(9) 1 d D U P B 1
P3A P 0.70689(11) 0.71681(11) 0.34411(7) 0.0493(3) Uani 0.450(9) 1 d . . P B 2
F17A F 0.7189(9) 0.5916(5) 0.3780(4) 0.087(3) Uani 0.450(9) 1 d D U P B 2
F18A F 0.5793(6) 0.7454(9) 0.3209(6) 0.121(5) Uani 0.450(9) 1 d D U P B 2
F19A F 0.6856(11) 0.8440(6) 0.3146(5) 0.123(5) Uani 0.450(9) 1 d D U P B 2
F20A F 0.8278(7) 0.6893(11) 0.3725(7) 0.182(8) Uani 0.450(9) 1 d D U P B 2
F21A F 0.7446(11) 0.6899(9) 0.2828(4) 0.174(8) Uani 0.450(9) 1 d D U P B 2
F22A F 0.6624(10) 0.7441(8) 0.4091(4) 0.112(5) Uani 0.450(9) 1 d D U P B 2
P4 P 0.22268(14) 0.03178(13) 0.05822(7) 0.0644(4) Uani 0.544(15) 1 d D . P C 1
F23 F 0.3029(7) -0.0572(11) 0.0307(7) 0.189(8) Uani 0.544(15) 1 d D U P C 1
F24 F 0.3230(4) 0.0388(5) 0.0942(3) 0.180(3) Uani 0.544(15) 1 d D U P C 1
F25 F 0.2238(11) 0.1292(11) -0.0018(4) 0.160(6) Uani 0.544(15) 1 d D U P C 1
F26 F 0.1381(7) 0.1241(8) 0.0857(6) 0.128(5) Uani 0.544(15) 1 d D U P C 1
F27 F 0.1166(3) 0.0286(3) 0.02161(17) 0.0907(12) Uani 0.544(15) 1 d D U P C 1
F28 F 0.2111(9) -0.0581(8) 0.1181(4) 0.119(5) Uani 0.544(15) 1 d D U P C 1
P4A P 0.22268(14) 0.03178(13) 0.05822(7) 0.0644(4) Uani 0.456(15) 1 d . . P C 2
F23A F 0.2855(7) -0.0971(5) 0.0694(6) 0.110(5) Uani 0.456(15) 1 d D U P C 2
F24A F 0.3230(4) 0.0388(5) 0.0942(3) 0.180(3) Uani 0.456(15) 1 d D U P C 2
F25A F 0.2753(8) 0.0532(11) -0.0069(3) 0.135(6) Uani 0.456(15) 1 d D U P C 2
F26A F 0.1550(8) 0.1597(6) 0.0431(8) 0.139(6) Uani 0.456(15) 1 d D U P C 2
F27A F 0.1166(3) 0.0286(3) 0.02161(17) 0.0907(12) Uani 0.456(15) 1 d D U P C 2
F28A F 0.1695(9) 0.0055(14) 0.1224(4) 0.149(7) Uani 0.456(15) 1 d D U P C 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
Ca1 F8 2.247(2) . ?
Ca1 F9 2.266(2) . ?
Ca1 F7 2.268(2) . ?
Ca1 F1A 2.354(3) . ?
Ca1 F1 2.354(3) . ?
Ca1 N1 2.486(4) . ?
Ca1 N2 2.518(4) . ?
Ca1 O7 3.129(3) . ?
Ca1 Ca3 3.5127(11) . ?
Ca1 Ca2 3.5254(11) . ?
Ca1 Ca4 3.5424(11) . ?
Ca2 F8 2.266(2) . ?
Ca2 F9 2.305(2) . ?
Ca2 F10 2.306(2) . ?
Ca2 O3 2.450(3) . ?
Ca2 O4 2.466(3) . ?
Ca2 O1 2.487(3) . ?
Ca2 O5 2.508(3) . ?
Ca2 O2 2.536(3) . ?
Ca2 Ca3 3.6256(10) . ?
Ca2 Ca4 3.6290(10) . ?
Ca3 F7 2.254(2) . ?
Ca3 F8 2.296(2) . ?
Ca3 F10 2.313(2) . ?
Ca3 O9 2.445(3) . ?
Ca3 O8 2.455(3) . ?
Ca3 O10 2.478(3) . ?
Ca3 O6 2.508(3) . ?
Ca3 O7 2.537(3) . ?
Ca3 Ca4 3.5969(10) . ?
Ca4 F9 2.257(2) . ?
Ca4 F7 2.274(2) . ?
Ca4 F10 2.303(2) . ?
Ca4 O11 2.442(3) . ?
Ca4 O15 2.484(3) . ?
Ca4 O12 2.499(3) . ?
Ca4 O13 2.525(3) . ?
Ca4 O14 2.534(3) . ?
O1 C14 1.426(5) . ?
O1 C5 1.430(5) . ?
O2 C6 1.438(5) . ?
O2 C7 1.439(5) . ?
O3 C9 1.411(7) . ?
O3 C8 1.420(6) . ?
O4 C10 1.403(7) . ?
O4 C11 1.424(6) . ?
O5 C13 1.437(5) . ?
O5 C12 1.440(5) . ?
O6 C24 1.432(6) . ?
O6 C15 1.442(5) . ?
O7 C17 1.440(5) . ?
O7 C16 1.448(5) . ?
O8 C19 1.430(5) . ?
O8 C18 1.442(6) . ?
O9 C20 1.430(5) . ?
O9 C21 1.433(6) . ?
O10 C22 1.444(5) . ?
O10 C23 1.445(5) . ?
O11 C25 1.426(6) . ?
O11 C34 1.431(5) . ?
O12 C26 1.432(6) . ?
O12 C27 1.433(6) . ?
O13 C29 1.422(6) . ?
O13 C28 1.430(6) . ?
O14 C30 1.429(6) . ?
O14 C31 1.438(6) . ?
O15 C33 1.428(5) . ?
O15 C32 1.433(5) . ?
N1 C1 1.130(5) . ?
C1 C2 1.454(7) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
N2 C3 1.129(5) . ?
C3 C4 1.458(6) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N3 C35 1.128(8) . ?
C35 C36 1.462(8) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
N4 C37 1.121(5) . ?
C37 C38 1.442(6) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C5 C6 1.486(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.510(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.286(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.489(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.489(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.489(7) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.502(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.491(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.486(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.480(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.505(7) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.496(8) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.491(8) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.501(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.478(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
P1 F5 1.534(4) . ?
P1 F3 1.561(4) . ?
P1 F6 1.565(4) . ?
P1 F4 1.586(3) . ?
P1 F2 1.592(4) . ?
P1 F1 1.618(2) . ?
P1A F2A 1.538(7) . ?
P1A F3A 1.544(7) . ?
P1A F6A 1.567(7) . ?
P1A F5A 1.581(7) . ?
P1A F4A 1.586(3) . ?
P1A F1A 1.618(2) . ?
P2 F11 1.576(3) . ?
P2 F12 1.582(3) . ?
P2 F15 1.585(3) . ?
P2 F13 1.590(3) . ?
P2 F16 1.594(3) . ?
P2 F14 1.596(3) . ?
P3 F18 1.539(5) . ?
P3 F22 1.550(5) . ?
P3 F17 1.564(5) . ?
P3 F19 1.565(6) . ?
P3 F21 1.586(6) . ?
P3 F20 1.588(5) . ?
P3A F21A 1.512(7) . ?
P3A F20A 1.533(7) . ?
P3A F19A 1.565(6) . ?
P3A F18A 1.576(6) . ?
P3A F17A 1.582(6) . ?
P3A F22A 1.611(6) . ?
P4 F23 1.534(6) . ?
P4 F24 1.546(4) . ?
P4 F28 1.552(6) . ?
P4 F25 1.568(6) . ?
P4 F26 1.584(6) . ?
P4 F27 1.590(3) . ?
P4A F24A 1.546(4) . ?
P4A F26A 1.554(6) . ?
P4A F28A 1.556(6) . ?
P4A F25A 1.562(6) . ?
P4A F23A 1.568(6) . ?
P4A F27A 1.590(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F8 Ca1 F9 76.68(8) . . ?
F8 Ca1 F7 76.77(8) . . ?
F9 Ca1 F7 75.48(8) . . ?
F8 Ca1 F1A 136.12(10) . . ?
F9 Ca1 F1A 132.64(9) . . ?
F7 Ca1 F1A 80.88(9) . . ?
F8 Ca1 F1 136.12(10) . . ?
F9 Ca1 F1 132.64(9) . . ?
F7 Ca1 F1 80.88(9) . . ?
F8 Ca1 N1 135.54(12) . . ?
F9 Ca1 N1 86.55(12) . . ?
F7 Ca1 N1 138.24(13) . . ?
F1A Ca1 N1 84.60(13) . . ?
F1 Ca1 N1 84.60(13) . . ?
F8 Ca1 N2 86.23(11) . . ?
F9 Ca1 N2 137.17(12) . . ?
F7 Ca1 N2 138.30(12) . . ?
F1A Ca1 N2 86.02(12) . . ?
F1 Ca1 N2 86.02(12) . . ?
N1 Ca1 N2 78.70(15) . . ?
F8 Ca1 O7 60.19(8) . . ?
F9 Ca1 O7 126.02(8) . . ?
F7 Ca1 O7 64.86(8) . . ?
F1A Ca1 O7 76.20(9) . . ?
F1 Ca1 O7 76.20(9) . . ?
N1 Ca1 O7 147.10(12) . . ?
N2 Ca1 O7 73.61(11) . . ?
F8 Ca1 Ca3 39.88(5) . . ?
F9 Ca1 Ca3 81.72(6) . . ?
F7 Ca1 Ca3 38.90(5) . . ?
F1A Ca1 Ca3 104.24(8) . . ?
F1 Ca1 Ca3 104.24(8) . . ?
N1 Ca1 Ca3 168.21(11) . . ?
N2 Ca1 Ca3 109.31(10) . . ?
O7 Ca1 Ca3 44.45(5) . . ?
F8 Ca1 Ca2 38.82(5) . . ?
F9 Ca1 Ca2 39.93(5) . . ?
F7 Ca1 Ca2 81.95(6) . . ?
F1A Ca1 Ca2 162.80(8) . . ?
F1 Ca1 Ca2 162.80(8) . . ?
N1 Ca1 Ca2 107.75(11) . . ?
N2 Ca1 Ca2 107.79(9) . . ?
O7 Ca1 Ca2 97.46(6) . . ?
Ca3 Ca1 Ca2 62.01(2) . . ?
F8 Ca1 Ca4 81.78(6) . . ?
F9 Ca1 Ca4 38.34(5) . . ?
F7 Ca1 Ca4 38.81(5) . . ?
F1A Ca1 Ca4 103.24(7) . . ?
F1 Ca1 Ca4 103.24(7) . . ?
N1 Ca1 Ca4 109.47(12) . . ?
N2 Ca1 Ca4 167.98(9) . . ?
O7 Ca1 Ca4 100.87(6) . . ?
Ca3 Ca1 Ca4 61.30(2) . . ?
Ca2 Ca1 Ca4 61.79(2) . . ?
F8 Ca2 F9 75.54(8) . . ?
F8 Ca2 F10 74.39(7) . . ?
F9 Ca2 F10 73.23(7) . . ?
F8 Ca2 O3 145.26(10) . . ?
F9 Ca2 O3 83.40(10) . . ?
F10 Ca2 O3 125.43(10) . . ?
F8 Ca2 O4 149.13(10) . . ?
F9 Ca2 O4 122.36(10) . . ?
F10 Ca2 O4 86.58(9) . . ?
O3 Ca2 O4 65.55(11) . . ?
F8 Ca2 O1 76.61(8) . . ?
F9 Ca2 O1 130.95(9) . . ?
F10 Ca2 O1 134.48(9) . . ?
O3 Ca2 O1 97.98(10) . . ?
O4 Ca2 O1 101.74(10) . . ?
F8 Ca2 O5 86.44(9) . . ?
F9 Ca2 O5 149.36(9) . . ?
F10 Ca2 O5 78.20(8) . . ?
O3 Ca2 O5 123.08(10) . . ?
O4 Ca2 O5 65.68(10) . . ?
O1 Ca2 O5 65.63(9) . . ?
F8 Ca2 O2 79.89(9) . . ?
F9 Ca2 O2 70.84(8) . . ?
F10 Ca2 O2 139.88(9) . . ?
O3 Ca2 O2 67.11(10) . . ?
O4 Ca2 O2 128.03(10) . . ?
O1 Ca2 O2 65.08(9) . . ?
O5 Ca2 O2 130.63(9) . . ?
F8 Ca2 Ca1 38.45(5) . . ?
F9 Ca2 Ca1 39.12(6) . . ?
F10 Ca2 Ca1 78.89(6) . . ?
O3 Ca2 Ca1 111.62(8) . . ?
O4 Ca2 Ca1 159.36(8) . . ?
O1 Ca2 Ca1 98.90(7) . . ?
O5 Ca2 Ca1 124.29(7) . . ?
O2 Ca2 Ca1 62.01(7) . . ?
F8 Ca2 Ca3 37.66(5) . . ?
F9 Ca2 Ca3 78.69(6) . . ?
F10 Ca2 Ca3 38.34(5) . . ?
O3 Ca2 Ca3 159.17(8) . . ?
O4 Ca2 Ca3 116.08(8) . . ?
O1 Ca2 Ca3 101.76(7) . . ?
O5 Ca2 Ca3 72.04(7) . . ?
O2 Ca2 Ca3 115.82(7) . . ?
Ca1 Ca2 Ca3 58.82(2) . . ?
F8 Ca2 Ca4 79.56(5) . . ?
F9 Ca2 Ca4 36.83(5) . . ?
F10 Ca2 Ca4 38.04(5) . . ?
O3 Ca2 Ca4 99.74(8) . . ?
O4 Ca2 Ca4 100.34(8) . . ?
O1 Ca2 Ca4 155.95(7) . . ?
O5 Ca2 Ca4 116.20(7) . . ?
O2 Ca2 Ca4 107.58(7) . . ?
Ca1 Ca2 Ca4 59.34(2) . . ?
Ca3 Ca2 Ca4 59.45(2) . . ?
F7 Ca3 F8 76.07(8) . . ?
F7 Ca3 F10 74.47(7) . . ?
F8 Ca3 F10 73.69(7) . . ?
F7 Ca3 O9 151.02(9) . . ?
F8 Ca3 O9 118.70(9) . . ?
F10 Ca3 O9 85.65(9) . . ?
F7 Ca3 O8 143.16(9) . . ?
F8 Ca3 O8 84.98(9) . . ?
F10 Ca3 O8 129.98(9) . . ?
O9 Ca3 O8 65.71(10) . . ?
F7 Ca3 O10 88.82(9) . . ?
F8 Ca3 O10 150.41(9) . . ?
F10 Ca3 O10 77.83(9) . . ?
O9 Ca3 O10 66.15(10) . . ?
O8 Ca3 O10 120.28(10) . . ?
F7 Ca3 O6 77.62(9) . . ?
F8 Ca3 O6 132.21(9) . . ?
F10 Ca3 O6 134.45(9) . . ?
O9 Ca3 O6 103.35(10) . . ?
O8 Ca3 O6 93.17(10) . . ?
O10 Ca3 O6 66.26(10) . . ?
F7 Ca3 O7 76.80(9) . . ?
F8 Ca3 O7 70.65(9) . . ?
F10 Ca3 O7 138.43(9) . . ?
O9 Ca3 O7 130.42(10) . . ?
O8 Ca3 O7 67.14(10) . . ?
O10 Ca3 O7 130.93(10) . . ?
O6 Ca3 O7 64.89(10) . . ?
F7 Ca3 Ca1 39.18(5) . . ?
F8 Ca3 Ca1 38.86(5) . . ?
F10 Ca3 Ca1 79.10(6) . . ?
O9 Ca3 Ca1 155.91(8) . . ?
O8 Ca3 Ca1 110.96(7) . . ?
O10 Ca3 Ca1 127.23(8) . . ?
O6 Ca3 Ca1 100.64(7) . . ?
O7 Ca3 Ca1 59.74(7) . . ?
F7 Ca3 Ca4 37.60(5) . . ?
F8 Ca3 Ca4 79.93(5) . . ?
F10 Ca3 Ca4 38.71(5) . . ?
O9 Ca3 Ca4 116.51(7) . . ?
O8 Ca3 Ca4 163.59(8) . . ?
O10 Ca3 Ca4 72.82(7) . . ?
O6 Ca3 Ca4 101.71(7) . . ?
O7 Ca3 Ca4 113.06(7) . . ?
Ca1 Ca3 Ca4 59.76(2) . . ?
F7 Ca3 Ca2 79.81(6) . . ?
F8 Ca3 Ca2 37.08(5) . . ?
F10 Ca3 Ca2 38.21(5) . . ?
O9 Ca3 Ca2 97.57(8) . . ?
O8 Ca3 Ca2 103.51(8) . . ?
O10 Ca3 Ca2 115.87(7) . . ?
O6 Ca3 Ca2 157.29(7) . . ?
O7 Ca3 Ca2 107.41(7) . . ?
Ca1 Ca3 Ca2 59.16(2) . . ?
Ca4 Ca3 Ca2 60.32(2) . . ?
F9 Ca4 F7 75.54(8) . . ?
F9 Ca4 F10 74.17(8) . . ?
F7 Ca4 F10 74.28(7) . . ?
F9 Ca4 O11 150.17(10) . . ?
F7 Ca4 O11 121.72(10) . . ?
F10 Ca4 O11 86.86(9) . . ?
F9 Ca4 O15 144.50(10) . . ?
F7 Ca4 O15 84.33(9) . . ?
F10 Ca4 O15 128.07(9) . . ?
O11 Ca4 O15 65.18(10) . . ?
F9 Ca4 O12 88.98(10) . . ?
F7 Ca4 O12 151.47(9) . . ?
F10 Ca4 O12 78.53(9) . . ?
O11 Ca4 O12 64.39(11) . . ?
O15 Ca4 O12 119.98(10) . . ?
F9 Ca4 O13 79.48(9) . . ?
F7 Ca4 O13 131.51(10) . . ?
F10 Ca4 O13 136.08(9) . . ?
O11 Ca4 O13 100.10(11) . . ?
O15 Ca4 O13 93.16(10) . . ?
O12 Ca4 O13 66.36(10) . . ?
F9 Ca4 O14 79.03(9) . . ?
F7 Ca4 O14 70.45(9) . . ?
F10 Ca4 O14 139.89(9) . . ?
O11 Ca4 O14 128.08(10) . . ?
O15 Ca4 O14 66.68(10) . . ?
O12 Ca4 O14 130.59(11) . . ?
O13 Ca4 O14 64.36(10) . . ?
F9 Ca4 Ca1 38.52(6) . . ?
F7 Ca4 Ca1 38.69(5) . . ?
F10 Ca4 Ca1 78.55(6) . . ?
O11 Ca4 Ca1 158.29(9) . . ?
O15 Ca4 Ca1 112.00(7) . . ?
O12 Ca4 Ca1 126.80(8) . . ?
O13 Ca4 Ca1 101.56(8) . . ?
O14 Ca4 Ca1 62.03(7) . . ?
F9 Ca4 Ca3 79.89(6) . . ?
F7 Ca4 Ca3 37.22(5) . . ?
F10 Ca4 Ca3 38.90(5) . . ?
O11 Ca4 Ca3 99.78(8) . . ?
O15 Ca4 Ca3 101.34(8) . . ?
O12 Ca4 Ca3 117.24(8) . . ?
O13 Ca4 Ca3 158.98(8) . . ?
O14 Ca4 Ca3 107.57(7) . . ?
Ca1 Ca4 Ca3 58.94(2) . . ?
F9 Ca4 Ca2 37.75(5) . . ?
F7 Ca4 Ca2 79.50(5) . . ?
F10 Ca4 Ca2 38.09(5) . . ?
O11 Ca4 Ca2 116.58(8) . . ?
O15 Ca4 Ca2 161.51(8) . . ?
O12 Ca4 Ca2 73.78(7) . . ?
O13 Ca4 Ca2 104.25(7) . . ?
O14 Ca4 Ca2 115.28(7) . . ?
Ca1 Ca4 Ca2 58.87(2) . . ?
Ca3 Ca4 Ca2 60.23(2) . . ?
C14 O1 C5 113.1(3) . . ?
C14 O1 Ca2 114.9(2) . . ?
C5 O1 Ca2 114.1(2) . . ?
C6 O2 C7 112.8(3) . . ?
C6 O2 Ca2 116.9(2) . . ?
C7 O2 Ca2 109.5(2) . . ?
C9 O3 C8 114.1(4) . . ?
C9 O3 Ca2 117.3(4) . . ?
C8 O3 Ca2 119.7(3) . . ?
C10 O4 C11 115.5(4) . . ?
C10 O4 Ca2 117.6(3) . . ?
C11 O4 Ca2 121.3(3) . . ?
C13 O5 C12 113.9(3) . . ?
C13 O5 Ca2 114.9(2) . . ?
C12 O5 Ca2 109.7(2) . . ?
C24 O6 C15 111.7(3) . . ?
C24 O6 Ca3 113.2(2) . . ?
C15 O6 Ca3 113.1(2) . . ?
C17 O7 C16 112.3(3) . . ?
C17 O7 Ca3 109.1(2) . . ?
C16 O7 Ca3 117.6(3) . . ?
C17 O7 Ca1 111.4(2) . . ?
C16 O7 Ca1 125.1(3) . . ?
Ca3 O7 Ca1 75.81(7) . . ?
C19 O8 C18 112.2(3) . . ?
C19 O8 Ca3 116.4(2) . . ?
C18 O8 Ca3 118.8(3) . . ?
C20 O9 C21 115.8(3) . . ?
C20 O9 Ca3 118.5(3) . . ?
C21 O9 Ca3 121.1(3) . . ?
C22 O10 C23 114.1(3) . . ?
C22 O10 Ca3 110.4(2) . . ?
C23 O10 Ca3 114.9(3) . . ?
C25 O11 C34 115.7(3) . . ?
C25 O11 Ca4 124.0(3) . . ?
C34 O11 Ca4 119.1(3) . . ?
C26 O12 C27 113.2(4) . . ?
C26 O12 Ca4 111.0(3) . . ?
C27 O12 Ca4 113.1(3) . . ?
C29 O13 C28 112.6(4) . . ?
C29 O13 Ca4 110.9(3) . . ?
C28 O13 Ca4 112.8(3) . . ?
C30 O14 C31 113.3(4) . . ?
C30 O14 Ca4 117.6(3) . . ?
C31 O14 Ca4 109.9(3) . . ?
C33 O15 C32 111.2(3) . . ?
C33 O15 Ca4 117.1(3) . . ?
C32 O15 Ca4 118.7(3) . . ?
Ca3 F7 Ca1 101.92(8) . . ?
Ca3 F7 Ca4 105.17(8) . . ?
Ca1 F7 Ca4 102.50(8) . . ?
Ca1 F8 Ca2 102.73(9) . . ?
Ca1 F8 Ca3 101.26(8) . . ?
Ca2 F8 Ca3 105.26(8) . . ?
Ca4 F9 Ca1 103.14(9) . . ?
Ca4 F9 Ca2 105.42(9) . . ?
Ca1 F9 Ca2 100.95(8) . . ?
Ca4 F10 Ca2 103.87(8) . . ?
Ca4 F10 Ca3 102.39(8) . . ?
Ca2 F10 Ca3 103.44(8) . . ?
C1 N1 Ca1 159.6(5) . . ?
N1 C1 C2 179.2(8) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 N2 Ca1 168.1(4) . . ?
N2 C3 C4 179.7(6) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C35 C36 175.3(18) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N4 C37 C38 178.2(8) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O1 C5 C6 107.8(3) . . ?
O1 C5 H5A 110.2 . . ?
C6 C5 H5A 110.2 . . ?
O1 C5 H5B 110.2 . . ?
C6 C5 H5B 110.2 . . ?
H5A C5 H5B 108.5 . . ?
O2 C6 C5 108.1(3) . . ?
O2 C6 H6A 110.1 . . ?
C5 C6 H6A 110.1 . . ?
O2 C6 H6B 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
O2 C7 C8 111.3(4) . . ?
O2 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
O2 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
O3 C8 C7 107.9(3) . . ?
O3 C8 H8A 110.1 . . ?
C7 C8 H8A 110.1 . . ?
O3 C8 H8B 110.1 . . ?
C7 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
C10 C9 O3 118.8(5) . . ?
C10 C9 H9A 107.6 . . ?
O3 C9 H9A 107.6 . . ?
C10 C9 H9B 107.6 . . ?
O3 C9 H9B 107.6 . . ?
H9A C9 H9B 107.0 . . ?
C9 C10 O4 118.6(5) . . ?
C9 C10 H10A 107.7 . . ?
O4 C10 H10A 107.7 . . ?
C9 C10 H10B 107.7 . . ?
O4 C10 H10B 107.7 . . ?
H10A C10 H10B 107.1 . . ?
O4 C11 C12 107.1(3) . . ?
O4 C11 H11A 110.3 . . ?
C12 C11 H11A 110.3 . . ?
O4 C11 H11B 110.3 . . ?
C12 C11 H11B 110.3 . . ?
H11A C11 H11B 108.6 . . ?
O5 C12 C11 111.7(4) . . ?
O5 C12 H12A 109.3 . . ?
C11 C12 H12A 109.3 . . ?
O5 C12 H12B 109.3 . . ?
C11 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
O5 C13 C14 106.4(4) . . ?
O5 C13 H13A 110.5 . . ?
C14 C13 H13A 110.5 . . ?
O5 C13 H13B 110.5 . . ?
C14 C13 H13B 110.5 . . ?
H13A C13 H13B 108.6 . . ?
O1 C14 C13 107.5(4) . . ?
O1 C14 H14A 110.2 . . ?
C13 C14 H14A 110.2 . . ?
O1 C14 H14B 110.2 . . ?
C13 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
O6 C15 C16 107.3(4) . . ?
O6 C15 H15A 110.3 . . ?
C16 C15 H15A 110.3 . . ?
O6 C15 H15B 110.3 . . ?
C16 C15 H15B 110.3 . . ?
H15A C15 H15B 108.5 . . ?
O7 C16 C15 108.7(4) . . ?
O7 C16 H16A 109.9 . . ?
C15 C16 H16A 109.9 . . ?
O7 C16 H16B 109.9 . . ?
C15 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
O7 C17 C18 110.5(4) . . ?
O7 C17 H17A 109.5 . . ?
C18 C17 H17A 109.5 . . ?
O7 C17 H17B 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 108.1 . . ?
O8 C18 C17 107.8(4) . . ?
O8 C18 H18A 110.1 . . ?
C17 C18 H18A 110.1 . . ?
O8 C18 H18B 110.1 . . ?
C17 C18 H18B 110.1 . . ?
H18A C18 H18B 108.5 . . ?
O8 C19 C20 107.0(4) . . ?
O8 C19 H19A 110.3 . . ?
C20 C19 H19A 110.3 . . ?
O8 C19 H19B 110.3 . . ?
C20 C19 H19B 110.3 . . ?
H19A C19 H19B 108.6 . . ?
O9 C20 C19 109.0(4) . . ?
O9 C20 H20A 109.9 . . ?
C19 C20 H20A 109.9 . . ?
O9 C20 H20B 109.9 . . ?
C19 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
O9 C21 C22 107.1(4) . . ?
O9 C21 H21A 110.3 . . ?
C22 C21 H21A 110.3 . . ?
O9 C21 H21B 110.3 . . ?
C22 C21 H21B 110.3 . . ?
H21A C21 H21B 108.5 . . ?
O10 C22 C21 111.3(4) . . ?
O10 C22 H22A 109.4 . . ?
C21 C22 H22A 109.4 . . ?
O10 C22 H22B 109.4 . . ?
C21 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
O10 C23 C24 106.5(4) . . ?
O10 C23 H23A 110.4 . . ?
C24 C23 H23A 110.4 . . ?
O10 C23 H23B 110.4 . . ?
C24 C23 H23B 110.4 . . ?
H23A C23 H23B 108.6 . . ?
O6 C24 C23 107.7(4) . . ?
O6 C24 H24A 110.2 . . ?
C23 C24 H24A 110.2 . . ?
O6 C24 H24B 110.2 . . ?
C23 C24 H24B 110.2 . . ?
H24A C24 H24B 108.5 . . ?
O11 C25 C26 106.4(4) . . ?
O11 C25 H25A 110.5 . . ?
C26 C25 H25A 110.5 . . ?
O11 C25 H25B 110.5 . . ?
C26 C25 H25B 110.5 . . ?
H25A C25 H25B 108.6 . . ?
O12 C26 C25 111.2(4) . . ?
O12 C26 H26A 109.4 . . ?
C25 C26 H26A 109.4 . . ?
O12 C26 H26B 109.4 . . ?
C25 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
O12 C27 C28 106.5(5) . . ?
O12 C27 H27A 110.4 . . ?
C28 C27 H27A 110.4 . . ?
O12 C27 H27B 110.4 . . ?
C28 C27 H27B 110.4 . . ?
H27A C27 H27B 108.6 . . ?
O13 C28 C27 106.8(4) . . ?
O13 C28 H28A 110.4 . . ?
C27 C28 H28A 110.4 . . ?
O13 C28 H28B 110.4 . . ?
C27 C28 H28B 110.4 . . ?
H28A C28 H28B 108.6 . . ?
O13 C29 C30 106.5(4) . . ?
O13 C29 H29A 110.4 . . ?
C30 C29 H29A 110.4 . . ?
O13 C29 H29B 110.4 . . ?
C30 C29 H29B 110.4 . . ?
H29A C29 H29B 108.6 . . ?
O14 C30 C29 108.3(4) . . ?
O14 C30 H30A 110.0 . . ?
C29 C30 H30A 110.0 . . ?
O14 C30 H30B 110.0 . . ?
C29 C30 H30B 110.0 . . ?
H30A C30 H30B 108.4 . . ?
O14 C31 C32 111.0(4) . . ?
O14 C31 H31A 109.4 . . ?
C32 C31 H31A 109.4 . . ?
O14 C31 H31B 109.4 . . ?
C32 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
O15 C32 C31 107.9(3) . . ?
O15 C32 H32A 110.1 . . ?
C31 C32 H32A 110.1 . . ?
O15 C32 H32B 110.1 . . ?
C31 C32 H32B 110.1 . . ?
H32A C32 H32B 108.4 . . ?
O15 C33 C34 107.9(4) . . ?
O15 C33 H33A 110.1 . . ?
C34 C33 H33A 110.1 . . ?
O15 C33 H33B 110.1 . . ?
C34 C33 H33B 110.1 . . ?
H33A C33 H33B 108.4 . . ?
O11 C34 C33 109.2(4) . . ?
O11 C34 H34A 109.8 . . ?
C33 C34 H34A 109.8 . . ?
O11 C34 H34B 109.8 . . ?
C33 C34 H34B 109.8 . . ?
H34A C34 H34B 108.3 . . ?
F5 P1 F3 93.3(3) . . ?
F5 P1 F6 92.1(3) . . ?
F3 P1 F6 174.5(3) . . ?
F5 P1 F4 90.7(2) . . ?
F3 P1 F4 91.1(2) . . ?
F6 P1 F4 90.04(19) . . ?
F5 P1 F2 178.2(3) . . ?
F3 P1 F2 88.0(3) . . ?
F6 P1 F2 86.6(3) . . ?
F4 P1 F2 90.5(2) . . ?
F5 P1 F1 89.14(18) . . ?
F3 P1 F1 88.7(2) . . ?
F6 P1 F1 90.17(19) . . ?
F4 P1 F1 179.73(19) . . ?
F2 P1 F1 89.70(19) . . ?
P1 F1 Ca1 151.38(18) . . ?
F2A P1A F3A 91.8(5) . . ?
F2A P1A F6A 90.3(5) . . ?
F3A P1A F6A 177.6(6) . . ?
F2A P1A F5A 178.2(6) . . ?
F3A P1A F5A 89.4(5) . . ?
F6A P1A F5A 88.4(5) . . ?
F2A P1A F4A 91.2(4) . . ?
F3A P1A F4A 89.9(4) . . ?
F6A P1A F4A 91.3(4) . . ?
F5A P1A F4A 90.2(4) . . ?
F2A P1A F1A 89.1(4) . . ?
F3A P1A F1A 90.1(4) . . ?
F6A P1A F1A 88.7(4) . . ?
F5A P1A F1A 89.6(3) . . ?
F4A P1A F1A 179.73(19) . . ?
P1A F1A Ca1 151.38(18) . . ?
F11 P2 F12 91.1(2) . . ?
F11 P2 F15 90.4(2) . . ?
F12 P2 F15 178.4(2) . . ?
F11 P2 F13 91.36(17) . . ?
F12 P2 F13 90.61(17) . . ?
F15 P2 F13 89.88(17) . . ?
F11 P2 F16 179.7(2) . . ?
F12 P2 F16 88.67(17) . . ?
F15 P2 F16 89.79(19) . . ?
F13 P2 F16 88.82(15) . . ?
F11 P2 F14 89.80(16) . . ?
F12 P2 F14 89.60(16) . . ?
F15 P2 F14 89.87(17) . . ?
F13 P2 F14 178.82(16) . . ?
F16 P2 F14 90.02(15) . . ?
F18 P3 F22 92.3(4) . . ?
F18 P3 F17 91.7(4) . . ?
F22 P3 F17 89.9(4) . . ?
F18 P3 F19 90.0(4) . . ?
F22 P3 F19 89.9(4) . . ?
F17 P3 F19 178.3(4) . . ?
F18 P3 F21 89.5(4) . . ?
F22 P3 F21 177.9(4) . . ?
F17 P3 F21 91.2(4) . . ?
F19 P3 F21 88.9(4) . . ?
F18 P3 F20 176.9(4) . . ?
F22 P3 F20 90.7(4) . . ?
F17 P3 F20 89.2(4) . . ?
F19 P3 F20 89.2(4) . . ?
F21 P3 F20 87.5(3) . . ?
F21A P3A F20A 93.7(5) . . ?
F21A P3A F19A 93.5(4) . . ?
F20A P3A F19A 92.3(5) . . ?
F21A P3A F18A 91.3(5) . . ?
F20A P3A F18A 175.0(6) . . ?
F19A P3A F18A 88.4(4) . . ?
F21A P3A F17A 91.2(4) . . ?
F20A P3A F17A 90.3(4) . . ?
F19A P3A F17A 174.5(5) . . ?
F18A P3A F17A 88.7(4) . . ?
F21A P3A F22A 177.7(6) . . ?
F20A P3A F22A 88.4(5) . . ?
F19A P3A F22A 87.5(4) . . ?
F18A P3A F22A 86.7(4) . . ?
F17A P3A F22A 87.7(4) . . ?
F23 P4 F24 91.9(4) . . ?
F23 P4 F28 92.4(5) . . ?
F24 P4 F28 91.6(3) . . ?
F23 P4 F25 91.8(5) . . ?
F24 P4 F25 90.7(4) . . ?
F28 P4 F25 175.1(5) . . ?
F23 P4 F26 179.0(5) . . ?
F24 P4 F26 89.0(4) . . ?
F28 P4 F26 87.8(4) . . ?
F25 P4 F26 87.9(5) . . ?
F23 P4 F27 90.1(4) . . ?
F24 P4 F27 178.0(3) . . ?
F28 P4 F27 88.8(3) . . ?
F25 P4 F27 88.8(3) . . ?
F26 P4 F27 89.0(3) . . ?
F24A P4A F26A 91.5(4) . . ?
F24A P4A F28A 90.5(4) . . ?
F26A P4A F28A 91.9(5) . . ?
F24A P4A F25A 91.3(4) . . ?
F26A P4A F25A 90.2(5) . . ?
F28A P4A F25A 177.2(5) . . ?
F24A P4A F23A 92.3(4) . . ?
F26A P4A F23A 175.9(5) . . ?
F28A P4A F23A 89.5(5) . . ?
F25A P4A F23A 88.3(4) . . ?
F24A P4A F27A 178.0(3) . . ?
F26A P4A F27A 86.6(3) . . ?
F28A P4A F27A 88.7(4) . . ?
F25A P4A F27A 89.5(4) . . ?
F23A P4A F27A 89.6(3) . . ?

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
C14 O1 C5 C6 172.0(3) . . . . ?
Ca2 O1 C5 C6 -54.2(4) . . . . ?
C7 O2 C6 C5 -162.7(4) . . . . ?
Ca2 O2 C6 C5 -34.5(4) . . . . ?
O1 C5 C6 O2 56.8(4) . . . . ?
C6 O2 C7 C8 81.3(4) . . . . ?
Ca2 O2 C7 C8 -50.7(4) . . . . ?
C9 O3 C8 C7 -177.5(6) . . . . ?
Ca2 O3 C8 C7 -31.0(5) . . . . ?
O2 C7 C8 O3 54.3(5) . . . . ?
C8 O3 C9 C10 163.5(9) . . . . ?
Ca2 O3 C9 C10 16.2(13) . . . . ?
O3 C9 C10 O4 -16.2(15) . . . . ?
C11 O4 C10 C9 -145.8(9) . . . . ?
Ca2 O4 C10 C9 8.3(11) . . . . ?
C10 O4 C11 C12 175.6(5) . . . . ?
Ca2 O4 C11 C12 22.5(5) . . . . ?
C13 O5 C12 C11 -75.6(5) . . . . ?
Ca2 O5 C12 C11 54.8(4) . . . . ?
O4 C11 C12 O5 -50.7(5) . . . . ?
C12 O5 C13 C14 173.9(4) . . . . ?
Ca2 O5 C13 C14 46.2(4) . . . . ?
C5 O1 C14 C13 -177.9(4) . . . . ?
Ca2 O1 C14 C13 48.6(4) . . . . ?
O5 C13 C14 O1 -61.1(5) . . . . ?
C24 O6 C15 C16 174.5(4) . . . . ?
Ca3 O6 C15 C16 -56.4(4) . . . . ?
C17 O7 C16 C15 -158.6(4) . . . . ?
Ca3 O7 C16 C15 -30.7(5) . . . . ?
Ca1 O7 C16 C15 60.9(5) . . . . ?
O6 C15 C16 O7 55.8(5) . . . . ?
C16 O7 C17 C18 79.0(5) . . . . ?
Ca3 O7 C17 C18 -53.2(4) . . . . ?
Ca1 O7 C17 C18 -135.0(3) . . . . ?
C19 O8 C18 C17 -171.5(4) . . . . ?
Ca3 O8 C18 C17 -31.0(5) . . . . ?
O7 C17 C18 O8 56.0(5) . . . . ?
C18 O8 C19 C20 -171.2(4) . . . . ?
Ca3 O8 C19 C20 47.3(5) . . . . ?
C21 O9 C20 C19 -120.5(4) . . . . ?
Ca3 O9 C20 C19 35.8(5) . . . . ?
O8 C19 C20 O9 -52.1(5) . . . . ?
C20 O9 C21 C22 178.4(4) . . . . ?
Ca3 O9 C21 C22 22.7(5) . . . . ?
C23 O10 C22 C21 -77.2(5) . . . . ?
Ca3 O10 C22 C21 54.1(4) . . . . ?
O9 C21 C22 O10 -49.8(5) . . . . ?
C22 O10 C23 C24 175.8(4) . . . . ?
Ca3 O10 C23 C24 46.8(5) . . . . ?
C15 O6 C24 C23 177.9(4) . . . . ?
Ca3 O6 C24 C23 48.8(4) . . . . ?
O10 C23 C24 O6 -62.2(5) . . . . ?
C34 O11 C25 C26 -178.0(4) . . . . ?
Ca4 O11 C25 C26 14.7(5) . . . . ?
C27 O12 C26 C25 -73.7(5) . . . . ?
Ca4 O12 C26 C25 54.7(4) . . . . ?
O11 C25 C26 O12 -44.7(5) . . . . ?
C26 O12 C27 C28 178.1(4) . . . . ?
Ca4 O12 C27 C28 50.7(5) . . . . ?
C29 O13 C28 C27 174.7(4) . . . . ?
Ca4 O13 C28 C27 48.4(5) . . . . ?
O12 C27 C28 O13 -65.4(5) . . . . ?
C28 O13 C29 C30 172.1(4) . . . . ?
Ca4 O13 C29 C30 -60.5(4) . . . . ?
C31 O14 C30 C29 -159.7(4) . . . . ?
Ca4 O14 C30 C29 -29.6(5) . . . . ?
O13 C29 C30 O14 58.6(5) . . . . ?
C30 O14 C31 C32 81.2(5) . . . . ?
Ca4 O14 C31 C32 -52.6(4) . . . . ?
C33 O15 C32 C31 -171.3(4) . . . . ?
Ca4 O15 C32 C31 -30.9(5) . . . . ?
O14 C31 C32 O15 55.4(5) . . . . ?
C32 O15 C33 C34 -175.8(4) . . . . ?
Ca4 O15 C33 C34 43.1(5) . . . . ?
C25 O11 C34 C33 -130.0(5) . . . . ?
Ca4 O11 C34 C33 37.9(5) . . . . ?
O15 C33 C34 O11 -50.7(5) . . . . ?
F5 P1 F1 Ca1 -22.7(5) . . . . ?
F3 P1 F1 Ca1 70.6(4) . . . . ?
F6 P1 F1 Ca1 -114.7(4) . . . . ?
F2 P1 F1 Ca1 158.7(4) . . . . ?
F2A P1A F1A Ca1 -156.6(10) . . . . ?
F3A P1A F1A Ca1 111.6(10) . . . . ?
F6A P1A F1A Ca1 -66.3(10) . . . . ?
F5A P1A F1A Ca1 22.1(10) . . . . ?

####################################################################### 
# 
# 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_DW_B1_0074
_audit_block_doi                 10.5517/ccdc.csd.cc1nbx96
_database_code_depnum_ccdc_archive 'CCDC 1529828'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7CC01938F 2017
_audit_update_record             
;
2017-01-26 deposited with the CCDC.
2018-10-10 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2014/7

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.0  (Andrew D. Bond, July 2015)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Evan Keyzer'
_cambridge_user_crsid            ek406
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             enk-2-42
_cambridge_data_id               dw_b1_0074
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H22 Ca F2 O8 P +, F6 P -'
_chemical_formula_sum            'C12 H22 Ca F8 O8 P2'
_chemical_formula_weight         548.31
_chemical_absolute_configuration unk

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'
O O 0.0492 0.0322 '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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

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

_cell_length_a                   28.1056(10)
_cell_length_b                   11.9971(5)
_cell_length_c                   13.0595(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4403.5(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9964
_cell_measurement_theta_min      4.01
_cell_measurement_theta_max      58.99

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_F_000             2240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    4.827
_shelx_estimated_absorpt_T_min   0.494
_shelx_estimated_absorpt_T_max   0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5879
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22919
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.145
_diffrn_reflns_theta_max         59.103
_diffrn_reflns_theta_full        59.103
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5907
_reflns_number_gt                5140
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.900
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

_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       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          'Refined as a 2-component inversion 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)+(0.0881P)²+7.6756P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_Flack   0.52(2)
_refine_ls_abs_structure_details 'Refined as an inversion twin.'
_refine_ls_number_reflns         5907
_refine_ls_number_parameters     560
_refine_ls_number_restraints     145
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0593
_refine_ls_wR_factor_ref         0.1589
_refine_ls_wR_factor_gt          0.1521
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.102

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 0.71988(6) 0.99756(14) 0.35648(14) 0.0294(4) Uani 1 1 d . . . . .
Ca2 Ca 0.47271(6) 0.47801(14) 0.64033(13) 0.0291(4) Uani 1 1 d . . . . .
P1 P 0.72462(11) 0.4917(2) 0.6502(3) 0.0514(7) Uani 1 1 d . . . . .
P2 P 0.45437(9) 0.00869(19) 0.3932(2) 0.0395(6) Uani 1 1 d . . . . .
P3 P 0.70227(9) 1.0099(2) 0.0772(2) 0.0397(7) Uani 1 1 d . . . . .
P4 P 0.45242(8) 0.4781(2) 0.91376(18) 0.0367(6) Uani 1 1 d . . . . .
F1 F 0.7509(3) 0.6033(7) 0.6688(7) 0.105(3) Uani 1 1 d . . . . .
F2 F 0.7432(4) 0.4955(5) 0.5353(7) 0.088(3) Uani 1 1 d . . . . .
F3 F 0.6794(3) 0.5651(9) 0.6227(8) 0.123(4) Uani 1 1 d . . . . .
F4 F 0.6943(4) 0.3839(7) 0.6281(6) 0.111(3) Uani 1 1 d . . . . .
F5 F 0.7050(3) 0.4890(5) 0.7635(6) 0.069(2) Uani 1 1 d . . . . .
F6 F 0.7677(3) 0.4206(10) 0.6803(7) 0.135(4) Uani 1 1 d . . . . .
F7 F 0.4429(3) 0.0009(5) 0.5118(5) 0.0663(19) Uani 1 1 d . . . . .
F8 F 0.49053(19) -0.0940(5) 0.4040(6) 0.0640(17) Uani 1 1 d . . . . .
F9 F 0.4955(2) 0.0959(6) 0.4148(8) 0.086(2) Uani 1 1 d . . . . .
F10 F 0.4187(2) 0.1106(5) 0.3828(5) 0.0625(17) Uani 1 1 d . . . . .
F11 F 0.4661(4) 0.0153(6) 0.2748(6) 0.088(3) Uani 1 1 d . . . . .
F12 F 0.4133(2) -0.0782(5) 0.3717(5) 0.0690(18) Uani 1 1 d . . . . .
F13 F 0.6718(3) 1.1115(7) 0.0585(6) 0.102(3) Uani 1 1 d . . . . .
F14 F 0.6695(2) 0.9235(8) 0.0306(6) 0.100(3) Uani 1 1 d . . . . .
F15 F 0.4553(3) 0.3486(6) 0.9142(7) 0.109(3) Uani 1 1 d . . . . .
F16 F 0.4033(2) 0.4907(10) 0.9565(6) 0.133(5) Uani 1 1 d . . . . .
O1 O 0.7048(3) 0.9907(6) 0.1861(5) 0.0482(19) Uani 1 1 d . . . . .
O2 O 0.7450(2) 1.0179(5) 0.0129(5) 0.0406(16) Uani 1 1 d . . . . .
O3 O 0.4521(3) 0.5107(6) 0.8083(5) 0.0454(19) Uani 1 1 d . . . . .
O4 O 0.4878(2) 0.5165(5) 0.9865(5) 0.0428(17) Uani 1 1 d . . . . .
O5 O 0.6682(2) 1.1729(6) 0.3863(7) 0.064(2) Uani 1 1 d . . . . .
O6 O 0.6287(2) 0.9779(6) 0.3505(6) 0.0566(19) Uani 1 1 d . . . . .
O7 O 0.6805(2) 0.8327(7) 0.4493(7) 0.064(2) Uani 1 1 d . . . . .
O8 O 0.7596(2) 0.8112(5) 0.3371(5) 0.0475(16) Uani 1 1 d . . . . .
O9 O 0.8036(2) 0.9975(5) 0.2881(5) 0.0385(16) Uani 1 1 d . . . . .
O10 O 0.7571(2) 1.1845(5) 0.3283(5) 0.0425(15) Uani 1 1 d . . . . .
O11 O 0.4485(3) 0.6765(6) 0.6160(7) 0.073(2) Uani 1 1 d . . . . .
O12 O 0.5352(3) 0.6176(7) 0.6912(5) 0.057(2) Uani 1 1 d . . . . .
O13 O 0.5477(3) 0.4006(9) 0.7184(8) 0.091(3) Uani 1 1 d . . . . .
O14 O 0.4885(5) 0.2744(8) 0.6208(8) 0.105(4) Uani 1 1 d . . . . .
O15 O 0.4043(4) 0.3315(8) 0.6763(7) 0.085(3) Uani 1 1 d . . . . .
O16 O 0.3991(3) 0.5041(8) 0.5274(8) 0.091(3) Uani 1 1 d . . . . .
C1 C 0.6172(4) 1.1749(11) 0.3695(12) 0.079(4) Uani 1 1 d . U . . .
H1A H 0.6082 1.2422 0.3301 0.095 Uiso 1 1 calc R U . . .
H1B H 0.6001 1.1761 0.4358 0.095 Uiso 1 1 calc R U . . .
C2 C 0.6049(4) 1.0744(11) 0.3120(10) 0.066(3) Uani 1 1 d . U . . .
H2B H 0.5701 1.0625 0.3156 0.079 Uiso 1 1 calc R U . . .
H2C H 0.6136 1.0851 0.2392 0.079 Uiso 1 1 calc R U . . .
C3 C 0.6111(4) 0.9442(14) 0.4474(12) 0.087(4) Uani 1 1 d . U . . .
H3A H 0.5759 0.9434 0.4476 0.104 Uiso 1 1 calc R U . . .
H3B H 0.6223 0.9953 0.5018 0.104 Uiso 1 1 calc R U . . .
C4 C 0.6300(4) 0.8323(12) 0.4631(12) 0.088(4) Uani 1 1 d . U . . .
H4B H 0.6222 0.8065 0.5331 0.105 Uiso 1 1 calc R U . . .
H4C H 0.6152 0.7802 0.4136 0.105 Uiso 1 1 calc R U . . .
C5 C 0.6964(5) 0.7225(10) 0.4185(11) 0.079(4) Uani 1 1 d . U . . .
H5A H 0.6874 0.6669 0.4711 0.095 Uiso 1 1 calc R U . . .
H5B H 0.6812 0.7012 0.3530 0.095 Uiso 1 1 calc R U . . .
C6 C 0.7470(4) 0.7254(9) 0.4070(11) 0.070(3) Uani 1 1 d . U . . .
H6A H 0.7622 0.7395 0.4742 0.084 Uiso 1 1 calc R U . . .
H6B H 0.7585 0.6526 0.3812 0.084 Uiso 1 1 calc R U . . .
C7 C 0.8084(4) 0.8041(9) 0.3067(9) 0.055(3) Uani 1 1 d . U . . .
H7A H 0.8147 0.7322 0.2721 0.066 Uiso 1 1 calc R U . . .
H7B H 0.8296 0.8102 0.3670 0.066 Uiso 1 1 calc R U . . .
C8 C 0.8165(3) 0.8987(9) 0.2353(8) 0.050(3) Uani 1 1 d . U . . .
H8A H 0.8504 0.9018 0.2147 0.059 Uiso 1 1 calc R U . . .
H8B H 0.7968 0.8897 0.1729 0.059 Uiso 1 1 calc R U . . .
C9 C 0.8179(3) 1.0991(9) 0.2385(8) 0.047(3) Uani 1 1 d . U . . .
H9A H 0.8000 1.1093 0.1738 0.057 Uiso 1 1 calc R U . . .
H9B H 0.8523 1.0971 0.2226 0.057 Uiso 1 1 calc R U . . .
C10 C 0.8075(3) 1.1901(8) 0.3094(8) 0.048(3) Uani 1 1 d . U . . .
H10A H 0.8255 1.1806 0.3739 0.058 Uiso 1 1 calc R U . . .
H10B H 0.8161 1.2627 0.2786 0.058 Uiso 1 1 calc R U . . .
C11 C 0.7410(4) 1.2707(9) 0.3987(9) 0.058(3) Uani 1 1 d . U . . .
H11A H 0.7572 1.3422 0.3841 0.070 Uiso 1 1 calc R U . . .
H11B H 0.7478 1.2491 0.4704 0.070 Uiso 1 1 calc R U . . .
C12 C 0.6892(4) 1.2815(9) 0.3825(10) 0.063(3) Uani 1 1 d . U . . .
H12A H 0.6752 1.3295 0.4364 0.076 Uiso 1 1 calc R U . . .
H12B H 0.6828 1.3163 0.3152 0.076 Uiso 1 1 calc R U . . .
C13 C 0.4852(5) 0.7583(9) 0.6293(12) 0.079(4) Uani 1 1 d . U . . .
H13A H 0.4709 0.8313 0.6464 0.095 Uiso 1 1 calc R U . . .
H13B H 0.5034 0.7667 0.5648 0.095 Uiso 1 1 calc R U . . .
C14 C 0.5168(6) 0.7239(13) 0.7106(13) 0.097(5) Uani 1 1 d . U . . .
H14A H 0.5432 0.7780 0.7167 0.116 Uiso 1 1 calc R U . . .
H14B H 0.4992 0.7232 0.7762 0.116 Uiso 1 1 calc R U . . .
C15 C 0.5697(5) 0.5754(13) 0.7614(10) 0.082(4) Uani 1 1 d . U . . .
H15A H 0.5972 0.6269 0.7645 0.098 Uiso 1 1 calc R U . . .
H15B H 0.5556 0.5708 0.8307 0.098 Uiso 1 1 calc R U . . .
C16 C 0.5853(6) 0.4688(16) 0.7309(13) 0.096(5) Uani 1 1 d . U . . .
H16A H 0.6176 0.4482 0.7206 0.116 Uiso 1 1 calc R U . . .
C17 C 0.5624(7) 0.2942(19) 0.7031(18) 0.137(7) Uani 1 1 d . U . . .
H17A H 0.5848 0.2558 0.7446 0.164 Uiso 1 1 calc R U . . .
C18 C 0.5424(6) 0.2548(15) 0.6275(19) 0.123(6) Uani 1 1 d . U . . .
H18A H 0.5592 0.2147 0.5763 0.148 Uiso 1 1 calc R U . . .
C19 C 0.4645(6) 0.1980(13) 0.6741(14) 0.099(5) Uani 1 1 d . U . . .
H19A H 0.4705 0.2061 0.7485 0.119 Uiso 1 1 calc R U . . .
H19B H 0.4734 0.1217 0.6526 0.119 Uiso 1 1 calc R U . . .
C20 C 0.4134(4) 0.2224(10) 0.6488(10) 0.071(3) Uani 1 1 d . U . . .
H20A H 0.4077 0.2120 0.5746 0.085 Uiso 1 1 calc R U . . .
H20B H 0.3922 0.1713 0.6869 0.085 Uiso 1 1 calc R U . . .
C21 C 0.3637(6) 0.3793(15) 0.6385(14) 0.110(5) Uani 1 1 d . U . . .
H21A H 0.3367 0.3893 0.6812 0.132 Uiso 1 1 calc R U . . .
C22 C 0.3625(3) 0.4129(10) 0.5365(10) 0.060(3) Uani 1 1 d . U . . .
H22A H 0.3305 0.4411 0.5182 0.072 Uiso 1 1 calc R U . . .
H22B H 0.3705 0.3499 0.4907 0.072 Uiso 1 1 calc R U . . .
C24 C 0.4181(4) 0.6908(11) 0.5202(12) 0.088(4) Uani 1 1 d . U . . .
H24A H 0.4375 0.6775 0.4581 0.105 Uiso 1 1 calc R U . . .
H24B H 0.4052 0.7675 0.5170 0.105 Uiso 1 1 calc R U . . .
C26 C 0.3766(5) 0.6047(13) 0.5260(14) 0.102(5) Uani 1 1 d . U . . .
H26A H 0.3575 0.6156 0.5889 0.122 Uiso 1 1 calc R U . . .
H26B H 0.3555 0.6111 0.4657 0.122 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
Ca1 O1 2.267(7) . ?
Ca1 O2 2.281(7) 4_655 ?
Ca1 O10 2.501(6) . ?
Ca1 O8 2.512(6) . ?
Ca1 O9 2.516(7) . ?
Ca1 O7 2.570(7) . ?
Ca1 O6 2.576(7) . ?
Ca1 O5 2.587(7) . ?
Ca2 O4 2.296(7) 2_664 ?
Ca2 O3 2.302(7) . ?
Ca2 O14 2.496(9) . ?
Ca2 O11 2.497(7) . ?
Ca2 O12 2.517(7) . ?
Ca2 O13 2.518(8) . ?
Ca2 O16 2.560(9) . ?
Ca2 O15 2.647(10) . ?
P1 F6 1.532(8) . ?
P1 F1 1.549(8) . ?
P1 F4 1.575(8) . ?
P1 F5 1.580(8) . ?
P1 F3 1.588(8) . ?
P1 F2 1.588(8) . ?
P2 F12 1.580(6) . ?
P2 F9 1.584(6) . ?
P2 F11 1.584(8) . ?
P2 F7 1.584(7) . ?
P2 F10 1.587(6) . ?
P2 F8 1.603(6) . ?
P3 O1 1.442(7) . ?
P3 O2 1.470(7) . ?
P3 F13 1.510(7) . ?
P3 F14 1.515(8) . ?
P4 O3 1.432(7) . ?
P4 O4 1.450(7) . ?
P4 F16 1.497(7) . ?
P4 F15 1.555(8) . ?
O2 Ca1 2.281(7) 4_654 ?
O4 Ca2 2.296(7) 2_665 ?
O5 C12 1.431(13) . ?
O5 C1 1.449(13) . ?
O6 C3 1.417(15) . ?
O6 C2 1.427(14) . ?
O7 C4 1.431(13) . ?
O7 C5 1.452(15) . ?
O8 C6 1.421(13) . ?
O8 C7 1.429(12) . ?
O9 C8 1.420(12) . ?
O9 C9 1.437(11) . ?
O10 C10 1.440(11) . ?
O10 C11 1.457(12) . ?
O11 C13 1.435(15) . ?
O11 C24 1.525(16) . ?
O12 C14 1.399(17) . ?
O12 C15 1.427(15) . ?
O13 C16 1.35(2) . ?
O13 C17 1.36(2) . ?
O14 C19 1.335(18) . ?
O14 C18 1.533(19) . ?
O15 C21 1.369(16) . ?
O15 C20 1.381(14) . ?
O16 C26 1.361(15) . ?
O16 C22 1.507(14) . ?
C1 C2 1.461(18) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2B 0.9900 . ?
C2 H2C 0.9900 . ?
C3 C4 1.458(19) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4B 0.9900 . ?
C4 H4C 0.9900 . ?
C5 C6 1.432(17) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.487(16) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.460(15) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.477(15) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.44(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.41(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9500 . ?
C17 C18 1.23(3) . ?
C17 H17A 0.9500 . ?
C18 H18A 0.9500 . ?
C19 C20 1.50(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.39(2) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C24 C26 1.560(19) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 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
O1 Ca1 O2 164.6(2) . 4_655 ?
O1 Ca1 O10 88.1(2) . . ?
O2 Ca1 O10 81.7(2) 4_655 . ?
O1 Ca1 O8 87.3(2) . . ?
O2 Ca1 O8 89.6(2) 4_655 . ?
O10 Ca1 O8 126.7(2) . . ?
O1 Ca1 O9 80.0(2) . . ?
O2 Ca1 O9 85.1(2) 4_655 . ?
O10 Ca1 O9 63.7(2) . . ?
O8 Ca1 O9 63.2(2) . . ?
O1 Ca1 O7 110.8(3) . . ?
O2 Ca1 O7 81.1(3) 4_655 . ?
O10 Ca1 O7 159.9(3) . . ?
O8 Ca1 O7 63.5(2) . . ?
O9 Ca1 O7 124.8(2) . . ?
O1 Ca1 O6 77.3(3) . . ?
O2 Ca1 O6 117.8(3) 4_655 . ?
O10 Ca1 O6 119.5(2) . . ?
O8 Ca1 O6 111.0(2) . . ?
O9 Ca1 O6 156.9(3) . . ?
O7 Ca1 O6 61.0(2) . . ?
O1 Ca1 O5 94.1(3) . . ?
O2 Ca1 O5 91.2(3) 4_655 . ?
O10 Ca1 O5 61.8(2) . . ?
O8 Ca1 O5 171.5(2) . . ?
O9 Ca1 O5 125.4(2) . . ?
O7 Ca1 O5 108.2(3) . . ?
O6 Ca1 O5 61.3(2) . . ?
O4 Ca2 O3 161.9(3) 2_664 . ?
O4 Ca2 O14 81.5(3) 2_664 . ?
O3 Ca2 O14 108.0(3) . . ?
O4 Ca2 O11 89.6(3) 2_664 . ?
O3 Ca2 O11 83.7(3) . . ?
O14 Ca2 O11 165.7(3) . . ?
O4 Ca2 O12 82.8(2) 2_664 . ?
O3 Ca2 O12 79.1(2) . . ?
O14 Ca2 O12 123.6(4) . . ?
O11 Ca2 O12 65.7(3) . . ?
O4 Ca2 O13 87.7(3) 2_664 . ?
O3 Ca2 O13 83.6(3) . . ?
O14 Ca2 O13 62.1(4) . . ?
O11 Ca2 O13 129.1(4) . . ?
O12 Ca2 O13 63.5(3) . . ?
O4 Ca2 O16 83.3(3) 2_664 . ?
O3 Ca2 O16 108.9(3) . . ?
O14 Ca2 O16 101.8(4) . . ?
O11 Ca2 O16 65.8(3) . . ?
O12 Ca2 O16 129.4(3) . . ?
O13 Ca2 O16 162.7(4) . . ?
O4 Ca2 O15 121.7(3) 2_664 . ?
O3 Ca2 O15 76.2(3) . . ?
O14 Ca2 O15 59.9(4) . . ?
O11 Ca2 O15 117.3(3) . . ?
O12 Ca2 O15 154.4(3) . . ?
O13 Ca2 O15 106.9(3) . . ?
O16 Ca2 O15 66.2(3) . . ?
F6 P1 F1 93.7(7) . . ?
F6 P1 F4 91.0(6) . . ?
F1 P1 F4 175.3(6) . . ?
F6 P1 F5 91.4(5) . . ?
F1 P1 F5 92.1(4) . . ?
F4 P1 F5 88.0(4) . . ?
F6 P1 F3 178.1(5) . . ?
F1 P1 F3 86.4(6) . . ?
F4 P1 F3 88.9(6) . . ?
F5 P1 F3 86.8(5) . . ?
F6 P1 F2 90.0(5) . . ?
F1 P1 F2 88.1(5) . . ?
F4 P1 F2 91.6(4) . . ?
F5 P1 F2 178.6(5) . . ?
F3 P1 F2 91.9(5) . . ?
F12 P2 F9 180.0(6) . . ?
F12 P2 F11 90.6(5) . . ?
F9 P2 F11 89.3(5) . . ?
F12 P2 F7 89.2(4) . . ?
F9 P2 F7 90.8(5) . . ?
F11 P2 F7 179.4(4) . . ?
F12 P2 F10 91.8(4) . . ?
F9 P2 F10 88.2(4) . . ?
F11 P2 F10 90.5(4) . . ?
F7 P2 F10 90.1(4) . . ?
F12 P2 F8 88.4(4) . . ?
F9 P2 F8 91.7(4) . . ?
F11 P2 F8 89.6(4) . . ?
F7 P2 F8 89.9(4) . . ?
F10 P2 F8 179.8(5) . . ?
O1 P3 O2 122.3(4) . . ?
O1 P3 F13 108.5(4) . . ?
O2 P3 F13 108.6(4) . . ?
O1 P3 F14 108.4(5) . . ?
O2 P3 F14 108.2(4) . . ?
F13 P3 F14 98.2(6) . . ?
O3 P4 O4 123.3(4) . . ?
O3 P4 F16 109.0(5) . . ?
O4 P4 F16 110.8(5) . . ?
O3 P4 F15 106.1(5) . . ?
O4 P4 F15 106.2(4) . . ?
F16 P4 F15 98.5(6) . . ?
P3 O1 Ca1 166.2(5) . . ?
P3 O2 Ca1 149.1(4) . 4_654 ?
P4 O3 Ca2 150.2(5) . . ?
P4 O4 Ca2 156.1(4) . 2_665 ?
C12 O5 C1 112.8(8) . . ?
C12 O5 Ca1 120.2(6) . . ?
C1 O5 Ca1 123.1(7) . . ?
C3 O6 C2 112.5(9) . . ?
C3 O6 Ca1 110.2(6) . . ?
C2 O6 Ca1 113.7(6) . . ?
C4 O7 C5 109.6(9) . . ?
C4 O7 Ca1 119.3(7) . . ?
C5 O7 Ca1 116.0(7) . . ?
C6 O8 C7 112.0(8) . . ?
C6 O8 Ca1 118.0(6) . . ?
C7 O8 Ca1 120.5(6) . . ?
C8 O9 C9 114.7(8) . . ?
C8 O9 Ca1 114.3(5) . . ?
C9 O9 Ca1 114.9(5) . . ?
C10 O10 C11 112.4(7) . . ?
C10 O10 Ca1 118.6(5) . . ?
C11 O10 Ca1 114.4(5) . . ?
C13 O11 C24 115.2(10) . . ?
C13 O11 Ca2 116.1(7) . . ?
C24 O11 Ca2 111.4(8) . . ?
C14 O12 C15 117.4(11) . . ?
C14 O12 Ca2 113.3(8) . . ?
C15 O12 Ca2 114.0(7) . . ?
C16 O13 C17 110.5(14) . . ?
C16 O13 Ca2 118.8(9) . . ?
C17 O13 Ca2 122.9(12) . . ?
C19 O14 C18 111.4(13) . . ?
C19 O14 Ca2 121.9(10) . . ?
C18 O14 Ca2 108.6(9) . . ?
C21 O15 C20 117.2(11) . . ?
C21 O15 Ca2 105.3(10) . . ?
C20 O15 Ca2 116.6(8) . . ?
C26 O16 C22 109.2(10) . . ?
C26 O16 Ca2 119.4(9) . . ?
C22 O16 Ca2 114.6(7) . . ?
O5 C1 C2 107.3(9) . . ?
O5 C1 H1A 110.3 . . ?
C2 C1 H1A 110.3 . . ?
O5 C1 H1B 110.3 . . ?
C2 C1 H1B 110.3 . . ?
H1A C1 H1B 108.5 . . ?
O6 C2 C1 112.2(10) . . ?
O6 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
O6 C2 H2C 109.2 . . ?
C1 C2 H2C 109.2 . . ?
H2B C2 H2C 107.9 . . ?
O6 C3 C4 105.2(12) . . ?
O6 C3 H3A 110.7 . . ?
C4 C3 H3A 110.7 . . ?
O6 C3 H3B 110.7 . . ?
C4 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
O7 C4 C3 109.9(10) . . ?
O7 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
O7 C4 H4C 109.7 . . ?
C3 C4 H4C 109.7 . . ?
H4B C4 H4C 108.2 . . ?
C6 C5 O7 108.2(10) . . ?
C6 C5 H5A 110.1 . . ?
O7 C5 H5A 110.1 . . ?
C6 C5 H5B 110.1 . . ?
O7 C5 H5B 110.1 . . ?
H5A C5 H5B 108.4 . . ?
O8 C6 C5 109.4(10) . . ?
O8 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
O8 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.2 . . ?
O8 C7 C8 106.0(8) . . ?
O8 C7 H7A 110.5 . . ?
C8 C7 H7A 110.5 . . ?
O8 C7 H7B 110.5 . . ?
C8 C7 H7B 110.5 . . ?
H7A C7 H7B 108.7 . . ?
O9 C8 C7 107.1(9) . . ?
O9 C8 H8A 110.3 . . ?
C7 C8 H8A 110.3 . . ?
O9 C8 H8B 110.3 . . ?
C7 C8 H8B 110.3 . . ?
H8A C8 H8B 108.6 . . ?
O9 C9 C10 107.0(8) . . ?
O9 C9 H9A 110.3 . . ?
C10 C9 H9A 110.3 . . ?
O9 C9 H9B 110.3 . . ?
C10 C9 H9B 110.3 . . ?
H9A C9 H9B 108.6 . . ?
O10 C10 C9 105.7(8) . . ?
O10 C10 H10A 110.6 . . ?
C9 C10 H10A 110.6 . . ?
O10 C10 H10B 110.6 . . ?
C9 C10 H10B 110.6 . . ?
H10A C10 H10B 108.7 . . ?
O10 C11 C12 106.1(9) . . ?
O10 C11 H11A 110.5 . . ?
C12 C11 H11A 110.5 . . ?
O10 C11 H11B 110.5 . . ?
C12 C11 H11B 110.5 . . ?
H11A C11 H11B 108.7 . . ?
O5 C12 C11 108.8(9) . . ?
O5 C12 H12A 109.9 . . ?
C11 C12 H12A 109.9 . . ?
O5 C12 H12B 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
O11 C13 C14 109.6(11) . . ?
O11 C13 H13A 109.8 . . ?
C14 C13 H13A 109.8 . . ?
O11 C13 H13B 109.8 . . ?
C14 C13 H13B 109.8 . . ?
H13A C13 H13B 108.2 . . ?
O12 C14 C13 110.8(12) . . ?
O12 C14 H14A 109.5 . . ?
C13 C14 H14A 109.5 . . ?
O12 C14 H14B 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C16 C15 O12 110.6(11) . . ?
C16 C15 H15A 109.5 . . ?
O12 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
O12 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
O13 C16 C15 109.9(13) . . ?
O13 C16 H16A 125.1 . . ?
C15 C16 H16A 125.1 . . ?
C18 C17 O13 109.9(18) . . ?
C18 C17 H17A 125.1 . . ?
O13 C17 H17A 125.1 . . ?
C17 C18 O14 116.0(18) . . ?
C17 C18 H18A 122.0 . . ?
O14 C18 H18A 122.0 . . ?
O14 C19 C20 103.6(13) . . ?
O14 C19 H19A 111.0 . . ?
C20 C19 H19A 111.0 . . ?
O14 C19 H19B 111.0 . . ?
C20 C19 H19B 111.0 . . ?
H19A C19 H19B 109.0 . . ?
O15 C20 C19 107.8(11) . . ?
O15 C20 H20A 110.2 . . ?
C19 C20 H20A 110.2 . . ?
O15 C20 H20B 110.2 . . ?
C19 C20 H20B 110.2 . . ?
H20A C20 H20B 108.5 . . ?
O15 C21 C22 119.2(14) . . ?
O15 C21 H21A 120.4 . . ?
C22 C21 H21A 120.4 . . ?
C21 C22 O16 105.6(11) . . ?
C21 C22 H22A 110.6 . . ?
O16 C22 H22A 110.6 . . ?
C21 C22 H22B 110.6 . . ?
O16 C22 H22B 110.6 . . ?
H22A C22 H22B 108.7 . . ?
O11 C24 C26 107.7(11) . . ?
O11 C24 H24A 110.2 . . ?
C26 C24 H24A 110.2 . . ?
O11 C24 H24B 110.2 . . ?
C26 C24 H24B 110.2 . . ?
H24A C24 H24B 108.5 . . ?
O16 C26 C24 104.0(10) . . ?
O16 C26 H26A 111.0 . . ?
C24 C26 H26A 111.0 . . ?
O16 C26 H26B 111.0 . . ?
C24 C26 H26B 111.0 . . ?
H26A C26 H26B 109.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 P3 O1 Ca1 56(2) . . . . ?
F13 P3 O1 Ca1 -72(2) . . . . ?
F14 P3 O1 Ca1 -177.4(18) . . . . ?
O1 P3 O2 Ca1 152.9(7) . . . 4_654 ?
F13 P3 O2 Ca1 -79.7(9) . . . 4_654 ?
F14 P3 O2 Ca1 25.9(9) . . . 4_654 ?
O4 P4 O3 Ca2 94.1(9) . . . . ?
F16 P4 O3 Ca2 -133.4(9) . . . . ?
F15 P4 O3 Ca2 -28.3(11) . . . . ?
O3 P4 O4 Ca2 -171.6(9) . . . 2_665 ?
F16 P4 O4 Ca2 56.7(12) . . . 2_665 ?
F15 P4 O4 Ca2 -49.3(12) . . . 2_665 ?
C12 O5 C1 C2 144.4(10) . . . . ?
Ca1 O5 C1 C2 -13.3(14) . . . . ?
C3 O6 C2 C1 70.5(13) . . . . ?
Ca1 O6 C2 C1 -55.7(11) . . . . ?
O5 C1 C2 O6 43.5(14) . . . . ?
C2 O6 C3 C4 166.3(10) . . . . ?
Ca1 O6 C3 C4 -65.7(12) . . . . ?
C5 O7 C4 C3 -154.1(12) . . . . ?
Ca1 O7 C4 C3 -17.0(15) . . . . ?
O6 C3 C4 O7 52.9(15) . . . . ?
C4 O7 C5 C6 -179.1(11) . . . . ?
Ca1 O7 C5 C6 42.2(12) . . . . ?
C7 O8 C6 C5 -168.3(11) . . . . ?
Ca1 O8 C6 C5 45.1(12) . . . . ?
O7 C5 C6 O8 -55.4(14) . . . . ?
C6 O8 C7 C8 -179.4(9) . . . . ?
Ca1 O8 C7 C8 -33.8(11) . . . . ?
C9 O9 C8 C7 168.2(8) . . . . ?
Ca1 O9 C8 C7 -56.0(9) . . . . ?
O8 C7 C8 O9 56.2(10) . . . . ?
C8 O9 C9 C10 -172.5(8) . . . . ?
Ca1 O9 C9 C10 51.9(9) . . . . ?
C11 O10 C10 C9 179.8(8) . . . . ?
Ca1 O10 C10 C9 42.6(9) . . . . ?
O9 C9 C10 O10 -59.2(10) . . . . ?
C10 O10 C11 C12 160.2(9) . . . . ?
Ca1 O10 C11 C12 -60.7(9) . . . . ?
C1 O5 C12 C11 -179.0(10) . . . . ?
Ca1 O5 C12 C11 -20.6(12) . . . . ?
O10 C11 C12 O5 49.9(12) . . . . ?
C24 O11 C13 C14 -169.1(11) . . . . ?
Ca2 O11 C13 C14 -36.3(13) . . . . ?
C15 O12 C14 C13 175.7(10) . . . . ?
Ca2 O12 C14 C13 -48.1(13) . . . . ?
O11 C13 C14 O12 55.6(15) . . . . ?
C14 O12 C15 C16 -179.1(12) . . . . ?
Ca2 O12 C15 C16 45.0(13) . . . . ?
C17 O13 C16 C15 -171.4(15) . . . . ?
Ca2 O13 C16 C15 38.5(16) . . . . ?
O12 C15 C16 O13 -54.2(16) . . . . ?
C16 O13 C17 C18 -130.3(19) . . . . ?
Ca2 O13 C17 C18 18(3) . . . . ?
O13 C17 C18 O14 -46(3) . . . . ?
C19 O14 C18 C17 -84(2) . . . . ?
Ca2 O14 C18 C17 53(2) . . . . ?
C18 O14 C19 C20 -173.7(14) . . . . ?
Ca2 O14 C19 C20 55.9(15) . . . . ?
C21 O15 C20 C19 165.0(13) . . . . ?
Ca2 O15 C20 C19 38.9(13) . . . . ?
O14 C19 C20 O15 -57.9(15) . . . . ?
C20 O15 C21 C22 -75.6(19) . . . . ?
Ca2 O15 C21 C22 55.9(17) . . . . ?
O15 C21 C22 O16 -64.1(18) . . . . ?
C26 O16 C22 C21 -102.2(14) . . . . ?
Ca2 O16 C22 C21 34.8(12) . . . . ?
C13 O11 C24 C26 -173.0(11) . . . . ?
Ca2 O11 C24 C26 52.0(12) . . . . ?
C22 O16 C26 C24 178.1(11) . . . . ?
Ca2 O16 C26 C24 43.5(15) . . . . ?
O11 C24 C26 O16 -61.3(15) . . . . ?

####################################################################### 
# 
# 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_DW_B2_0067
_audit_block_doi                 10.5517/ccdc.csd.cc1nbx85
_database_code_depnum_ccdc_archive 'CCDC 1529827'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7CC01938F 2017
_audit_update_record             
;
2017-06-13 deposited with the CCDC.
2018-10-10 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2014/7

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.0  (Andrew D. Bond, July 2015)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Evan Keyzer'
_cambridge_user_crsid            ek406
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             enk-2-49
_cambridge_data_id               DW_B2_0067
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C44 H86 Ca4 F12 N2 O20 Si2 4+, 4(F6 P -), 4(C2 H3 N)'
_chemical_formula_sum            'C52 H98 Ca4 F36 N6 O20 P4 Si2'
_chemical_formula_weight         2151.74

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'
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'
F F 0.0727 0.0534 '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'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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                   12.9890(4)
_cell_length_b                   13.1082(4)
_cell_length_c                   13.8922(4)
_cell_angle_alpha                100.3963(11)
_cell_angle_beta                 103.0857(11)
_cell_angle_gamma                91.6070(12)
_cell_volume                     2260.21(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9864
_cell_measurement_theta_min      3.44
_cell_measurement_theta_max      66.79

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             1104
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    4.267
_shelx_estimated_absorpt_T_min   0.427
_shelx_estimated_absorpt_T_max   0.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5730
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26812
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.437
_diffrn_reflns_theta_max         66.870
_diffrn_reflns_theta_full        66.870
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             7970
_reflns_number_gt                7095
_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       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_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)+(0.0987P)²+7.3801P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7970
_refine_ls_number_parameters     562
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0778
_refine_ls_wR_factor_ref         0.2075
_refine_ls_wR_factor_gt          0.2021
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.187
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.864
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.101

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 0.42875(6) 0.58975(6) 0.34216(6) 0.0254(2) Uani 1 1 d . . . . .
Ca2 Ca 0.88699(6) 0.72392(6) 0.67920(6) 0.0252(2) Uani 1 1 d . . . . .
Si1 Si 0.68919(8) 0.56387(8) 0.54662(8) 0.0243(3) Uani 1 1 d . . . . .
F1 F 0.7548(2) 0.5466(2) 0.4578(2) 0.0433(7) Uani 1 1 d . . . . .
F2 F 0.80345(19) 0.55846(19) 0.6351(2) 0.0365(6) Uani 1 1 d . . . . .
F3 F 0.66159(19) 0.43463(18) 0.53264(18) 0.0313(5) Uani 1 1 d . . . . .
F4 F 0.57583(19) 0.5756(2) 0.46389(18) 0.0359(6) Uani 1 1 d . . . . .
F5 F 0.62271(19) 0.57739(17) 0.63974(17) 0.0295(5) Uani 1 1 d . . . . .
F6 F 0.71779(18) 0.69448(18) 0.56959(18) 0.0302(5) Uani 1 1 d . . . . .
P1 P 0.38353(11) 0.79696(11) 1.00831(11) 0.0475(3) Uani 1 1 d . . . . .
F11 F 0.3924(6) 0.8139(7) 1.1239(4) 0.156(3) Uani 1 1 d . . . . .
F12 F 0.4473(3) 0.9048(3) 1.0225(4) 0.0890(14) Uani 1 1 d . . . . .
F13 F 0.3195(4) 0.6868(3) 0.9867(4) 0.0986(15) Uani 1 1 d . . . . .
F14 F 0.4903(4) 0.7424(4) 1.0262(5) 0.1069(17) Uani 1 1 d . . . . .
F15 F 0.2795(3) 0.8539(4) 0.9956(5) 0.126(2) Uani 1 1 d . . . . .
F16 F 0.3771(7) 0.7803(5) 0.8939(4) 0.138(3) Uani 1 1 d . . . . .
P2 P 0.88897(11) 0.73485(12) 0.14102(11) 0.0511(4) Uani 1 1 d . . . . .
F21 F 0.9314(4) 0.6443(4) 0.0702(4) 0.1066(18) Uani 1 1 d . . . . .
F22 F 0.8536(5) 0.7978(8) 0.0563(5) 0.185(4) Uani 1 1 d . . . . .
F23 F 0.7766(5) 0.6818(7) 0.1126(5) 0.178(4) Uani 1 1 d . . . . .
F24 F 0.9262(8) 0.6769(5) 0.2284(4) 0.166(4) Uani 1 1 d . . . . .
F25 F 0.8528(4) 0.8234(4) 0.2194(3) 0.0899(13) Uani 1 1 d . . . . .
F26 F 0.9995(3) 0.7938(3) 0.1562(5) 0.116(2) Uani 1 1 d . . . . .
O1 O 0.5361(5) 0.5094(4) 0.2273(3) 0.092(2) Uani 1 1 d D . . . .
O2 O 0.3314(4) 0.5211(5) 0.1704(3) 0.105(2) Uani 1 1 d D . . . .
O3 O 0.2571(4) 0.6606(5) 0.2863(5) 0.105(2) Uani 1 1 d D . . . .
O4 O 0.4220(5) 0.7733(3) 0.4213(3) 0.0833(17) Uani 1 1 d D . . . .
O5 O 0.5566(4) 0.7093(4) 0.3109(3) 0.0761(15) Uani 1 1 d D . . . .
C1 C 0.4878(9) 0.4674(10) 0.1281(7) 0.149(5) Uani 1 1 d D U . . .
H1A H 0.5185 0.4007 0.1085 0.179 Uiso 1 1 calc R U . . .
H1B H 0.5043 0.5151 0.0850 0.179 Uiso 1 1 calc R U . . .
C2 C 0.3751(8) 0.4492(8) 0.1086(7) 0.121(4) Uani 1 1 d D U . . .
H2A H 0.3434 0.4523 0.0374 0.145 Uiso 1 1 calc R U . . .
H2B H 0.3579 0.3785 0.1190 0.145 Uiso 1 1 calc R U . . .
C3 C 0.2254(6) 0.5315(8) 0.1401(6) 0.111(3) Uani 1 1 d D U . . .
H3A H 0.1852 0.4780 0.1617 0.134 Uiso 1 1 calc R U . . .
H3B H 0.2043 0.5212 0.0658 0.134 Uiso 1 1 calc R U . . .
C4 C 0.2011(6) 0.6333(8) 0.1835(6) 0.110(3) Uani 1 1 d D U . . .
H4A H 0.2211 0.6848 0.1457 0.132 Uiso 1 1 calc R U . . .
H4B H 0.1239 0.6342 0.1788 0.132 Uiso 1 1 calc R U . . .
C5 C 0.2440(7) 0.7559(7) 0.3504(9) 0.133(4) Uani 1 1 d D U . . .
H5A H 0.2216 0.7388 0.4095 0.159 Uiso 1 1 calc R U . . .
H5B H 0.1861 0.7914 0.3132 0.159 Uiso 1 1 calc R U . . .
C6 C 0.3371(9) 0.8274(8) 0.3860(11) 0.170(6) Uani 1 1 d D U . . .
H6A H 0.3503 0.8598 0.3303 0.204 Uiso 1 1 calc R U . . .
H6B H 0.3266 0.8833 0.4405 0.204 Uiso 1 1 calc R U . . .
C7 C 0.5203(9) 0.8369(7) 0.4282(8) 0.139(4) Uani 1 1 d D U . . .
H7A H 0.5039 0.9108 0.4360 0.167 Uiso 1 1 calc R U . . .
H7B H 0.5722 0.8292 0.4903 0.167 Uiso 1 1 calc R U . . .
C8 C 0.5673(7) 0.8153(5) 0.3507(8) 0.107(3) Uani 1 1 d D U . . .
H8A H 0.6435 0.8388 0.3740 0.129 Uiso 1 1 calc R U . . .
H8B H 0.5349 0.8537 0.2976 0.129 Uiso 1 1 calc R U . . .
C9 C 0.6304(6) 0.6746(7) 0.2558(8) 0.114(3) Uani 1 1 d D U . . .
H9A H 0.7021 0.7014 0.2962 0.137 Uiso 1 1 calc R U . . .
H9B H 0.6171 0.7046 0.1940 0.137 Uiso 1 1 calc R U . . .
C10 C 0.6293(8) 0.5663(9) 0.2279(9) 0.148(5) Uani 1 1 d D U . . .
H10A H 0.6888 0.5420 0.2745 0.178 Uiso 1 1 calc R U . . .
H10B H 0.6427 0.5498 0.1596 0.178 Uiso 1 1 calc R U . . .
O11 O 0.8726(3) 0.9036(3) 0.6466(3) 0.0525(9) Uani 1 1 d D . . . .
O12 O 0.9396(3) 0.7518(3) 0.5278(3) 0.0637(11) Uani 1 1 d D . . . .
O13 O 1.0370(3) 0.6236(3) 0.6363(3) 0.0497(9) Uani 1 1 d D . . . .
O14 O 0.9902(3) 0.6536(3) 0.8200(3) 0.0448(8) Uani 1 1 d D . . . .
O15 O 1.0031(3) 0.8560(3) 0.8101(2) 0.0441(8) Uani 1 1 d D . . . .
C11 C 0.8515(5) 0.9040(5) 0.5429(5) 0.0706(19) Uani 1 1 d D . . . .
H11A H 0.8540 0.9769 0.5329 0.085 Uiso 1 1 calc R U . . .
H11B H 0.7790 0.8722 0.5107 0.085 Uiso 1 1 calc R U . . .
C12 C 0.9275(6) 0.8469(5) 0.4935(4) 0.0681(19) Uani 1 1 d D . . . .
H12A H 0.9007 0.8338 0.4195 0.082 Uiso 1 1 calc R U . . .
H12B H 0.9965 0.8881 0.5110 0.082 Uiso 1 1 calc R U . . .
C13 C 1.0035(6) 0.6830(6) 0.4841(5) 0.079(2) Uani 1 1 d D . . . .
H13A H 1.0356 0.7159 0.4380 0.095 Uiso 1 1 calc R U . . .
H13B H 0.9602 0.6196 0.4444 0.095 Uiso 1 1 calc R U . . .
C14 C 1.0863(5) 0.6558(5) 0.5629(6) 0.074(2) Uani 1 1 d D . . . .
H14A H 1.1251 0.5986 0.5341 0.089 Uiso 1 1 calc R U . . .
H14B H 1.1374 0.7165 0.5947 0.089 Uiso 1 1 calc R U . . .
C15 C 1.1034(5) 0.5835(5) 0.7165(5) 0.0640(17) Uani 1 1 d D . . . .
H15A H 1.1637 0.6344 0.7519 0.077 Uiso 1 1 calc R U . . .
H15B H 1.1318 0.5181 0.6890 0.077 Uiso 1 1 calc R U . . .
C16 C 1.0392(5) 0.5640(4) 0.7864(5) 0.0630(17) Uani 1 1 d D . . . .
H16A H 0.9842 0.5070 0.7524 0.076 Uiso 1 1 calc R U . . .
H16B H 1.0849 0.5415 0.8450 0.076 Uiso 1 1 calc R U . . .
C17 C 1.0606(4) 0.7272(5) 0.9012(4) 0.0567(15) Uani 1 1 d D . . . .
H17A H 1.0651 0.7039 0.9658 0.068 Uiso 1 1 calc R U . . .
H17B H 1.1326 0.7295 0.8886 0.068 Uiso 1 1 calc R U . . .
C18 C 1.0227(4) 0.8280(5) 0.9076(4) 0.0531(14) Uani 1 1 d D . . . .
H18A H 1.0759 0.8789 0.9564 0.064 Uiso 1 1 calc R U . . .
H18B H 0.9565 0.8289 0.9316 0.064 Uiso 1 1 calc R U . . .
C19 C 0.9783(6) 0.9607(4) 0.8093(5) 0.0636(17) Uani 1 1 d D . . . .
H19A H 1.0383 1.0088 0.8516 0.076 Uiso 1 1 calc R U . . .
H19B H 0.9150 0.9750 0.8368 0.076 Uiso 1 1 calc R U . . .
C20 C 0.9575(5) 0.9760(4) 0.7049(5) 0.0648(17) Uani 1 1 d D . . . .
H20A H 0.9381 1.0480 0.7015 0.078 Uiso 1 1 calc R U . . .
H20B H 1.0217 0.9645 0.6784 0.078 Uiso 1 1 calc R U . . .
N100 N 0.7699(3) 0.7854(3) 0.7948(3) 0.0440(10) Uani 1 1 d . . . . .
C101 C 0.7193(4) 0.8250(4) 0.8454(4) 0.0429(11) Uani 1 1 d . . . . .
C102 C 0.6568(6) 0.8773(6) 0.9112(5) 0.074(2) Uani 1 1 d . . . . .
H10C H 0.7041 0.9166 0.9728 0.111 Uiso 1 1 calc R U . . .
H10D H 0.6118 0.8255 0.9286 0.111 Uiso 1 1 calc R U . . .
H10E H 0.6121 0.9250 0.8767 0.111 Uiso 1 1 calc R U . . .
N200 N 0.7845(5) 1.0677(5) 0.3707(5) 0.0788(17) Uani 1 1 d . . . . .
C201 C 0.7351(5) 1.0336(5) 0.2925(5) 0.0596(15) Uani 1 1 d . . . . .
C202 C 0.6718(7) 0.9893(6) 0.1927(5) 0.080(2) Uani 1 1 d . . . . .
H20C H 0.7048 0.9286 0.1638 0.120 Uiso 1 1 calc R U . . .
H20D H 0.6675 1.0413 0.1496 0.120 Uiso 1 1 calc R U . . .
H20E H 0.6004 0.9681 0.1971 0.120 Uiso 1 1 calc R U . . .
N300 N 0.5165(8) 0.9265(6) 0.6621(6) 0.108(3) Uani 1 1 d . . . . .
C301 C 0.4843(7) 0.8456(6) 0.6636(5) 0.0720(19) Uani 1 1 d . . . . .
C302 C 0.4430(7) 0.7443(6) 0.6666(6) 0.081(2) Uani 1 1 d . . . . .
H30A H 0.4996 0.6962 0.6679 0.122 Uiso 1 1 calc R U . . .
H30B H 0.3856 0.7199 0.6068 0.122 Uiso 1 1 calc R U . . .
H30C H 0.4158 0.7473 0.7272 0.122 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
Ca1 F4 2.284(2) . ?
Ca1 F5 2.346(2) 2_666 ?
Ca1 F3 2.368(2) 2_666 ?
Ca1 O5 2.414(4) . ?
Ca1 O2 2.429(4) . ?
Ca1 O3 2.456(4) . ?
Ca1 O1 2.466(4) . ?
Ca1 O4 2.472(4) . ?
Ca2 F2 2.312(2) . ?
Ca2 F6 2.350(2) . ?
Ca2 O12 2.436(4) . ?
Ca2 O14 2.450(3) . ?
Ca2 O15 2.460(3) . ?
Ca2 O11 2.482(3) . ?
Ca2 N100 2.501(4) . ?
Ca2 O13 2.503(3) . ?
Ca2 Si1 3.2489(13) . ?
Si1 F1 1.640(3) . ?
Si1 F4 1.680(2) . ?
Si1 F3 1.689(2) . ?
Si1 F5 1.698(2) . ?
Si1 F6 1.698(2) . ?
Si1 F2 1.712(2) . ?
F3 Ca1 2.368(2) 2_666 ?
F5 Ca1 2.346(2) 2_666 ?
P1 F16 1.547(5) . ?
P1 F15 1.552(4) . ?
P1 F11 1.558(6) . ?
P1 F14 1.568(5) . ?
P1 F12 1.575(4) . ?
P1 F13 1.590(4) . ?
P2 F23 1.534(5) . ?
P2 F24 1.540(5) . ?
P2 F22 1.551(5) . ?
P2 F26 1.564(4) . ?
P2 F21 1.594(5) . ?
P2 F25 1.600(5) . ?
O1 C1 1.383(9) . ?
O1 C10 1.401(9) . ?
O2 C3 1.364(8) . ?
O2 C2 1.381(8) . ?
O3 C4 1.423(8) . ?
O3 C5 1.436(9) . ?
O4 C6 1.372(9) . ?
O4 C7 1.481(8) . ?
O5 C8 1.391(8) . ?
O5 C9 1.394(8) . ?
C1 C2 1.432(11) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.436(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.444(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.345(10) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.400(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
O11 C11 1.404(7) . ?
O11 C20 1.426(6) . ?
O12 C13 1.394(7) . ?
O12 C12 1.414(7) . ?
O13 C15 1.436(7) . ?
O13 C14 1.437(7) . ?
O14 C16 1.408(7) . ?
O14 C17 1.460(6) . ?
O15 C19 1.420(6) . ?
O15 C18 1.437(6) . ?
C11 C12 1.473(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.454(10) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.466(9) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.417(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.466(8) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
N100 C101 1.136(6) . ?
C101 C102 1.452(7) . ?
C102 H10C 0.9800 . ?
C102 H10D 0.9800 . ?
C102 H10E 0.9800 . ?
N200 C201 1.133(9) . ?
C201 C202 1.450(10) . ?
C202 H20C 0.9800 . ?
C202 H20D 0.9800 . ?
C202 H20E 0.9800 . ?
N300 C301 1.135(11) . ?
C301 C302 1.429(12) . ?
C302 H30A 0.9800 . ?
C302 H30B 0.9800 . ?
C302 H30C 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
F4 Ca1 F5 84.71(9) . 2_666 ?
F4 Ca1 F3 83.38(9) . 2_666 ?
F5 Ca1 F3 58.82(8) 2_666 2_666 ?
F4 Ca1 O5 78.16(13) . . ?
F5 Ca1 O5 150.40(14) 2_666 . ?
F3 Ca1 O5 140.70(13) 2_666 . ?
F4 Ca1 O2 144.79(17) . . ?
F5 Ca1 O2 80.60(16) 2_666 . ?
F3 Ca1 O2 114.80(15) 2_666 . ?
O5 Ca1 O2 99.81(17) . . ?
F4 Ca1 O3 151.47(17) . . ?
F5 Ca1 O3 102.02(15) 2_666 . ?
F3 Ca1 O3 76.92(16) 2_666 . ?
O5 Ca1 O3 104.56(18) . . ?
O2 Ca1 O3 63.5(2) . . ?
F4 Ca1 O1 83.38(14) . . ?
F5 Ca1 O1 88.66(14) 2_666 . ?
F3 Ca1 O1 145.82(13) 2_666 . ?
O5 Ca1 O1 65.68(18) . . ?
O2 Ca1 O1 64.55(19) . . ?
O3 Ca1 O1 124.06(19) . . ?
F4 Ca1 O4 90.25(14) . . ?
F5 Ca1 O4 139.38(14) 2_666 . ?
F3 Ca1 O4 80.56(13) 2_666 . ?
O5 Ca1 O4 65.28(18) . . ?
O2 Ca1 O4 121.24(19) . . ?
O3 Ca1 O4 66.47(19) . . ?
O1 Ca1 O4 130.82(19) . . ?
F2 Ca2 F6 60.30(8) . . ?
F2 Ca2 O12 104.37(13) . . ?
F6 Ca2 O12 82.65(12) . . ?
F2 Ca2 O14 82.59(10) . . ?
F6 Ca2 O14 138.19(10) . . ?
O12 Ca2 O14 127.97(14) . . ?
F2 Ca2 O15 147.59(11) . . ?
F6 Ca2 O15 142.73(11) . . ?
O12 Ca2 O15 101.89(14) . . ?
O14 Ca2 O15 66.26(11) . . ?
F2 Ca2 O11 143.66(11) . . ?
F6 Ca2 O11 83.49(10) . . ?
O12 Ca2 O11 65.09(14) . . ?
O14 Ca2 O11 132.24(12) . . ?
O15 Ca2 O11 66.02(12) . . ?
F2 Ca2 N100 92.46(13) . . ?
F6 Ca2 N100 77.94(12) . . ?
O12 Ca2 N100 143.47(15) . . ?
O14 Ca2 N100 85.70(14) . . ?
O15 Ca2 N100 77.10(13) . . ?
O11 Ca2 N100 82.08(14) . . ?
F2 Ca2 O13 80.78(11) . . ?
F6 Ca2 O13 120.15(11) . . ?
O12 Ca2 O13 64.06(14) . . ?
O14 Ca2 O13 66.54(12) . . ?
O15 Ca2 O13 94.11(12) . . ?
O11 Ca2 O13 118.96(13) . . ?
N100 Ca2 O13 151.99(14) . . ?
F1 Si1 F4 91.81(15) . . ?
F1 Si1 F3 91.89(13) . . ?
F4 Si1 F3 91.63(13) . . ?
F1 Si1 F5 177.81(15) . . ?
F4 Si1 F5 89.39(13) . . ?
F3 Si1 F5 86.25(12) . . ?
F1 Si1 F6 91.39(14) . . ?
F4 Si1 F6 90.66(13) . . ?
F3 Si1 F6 175.94(13) . . ?
F5 Si1 F6 90.42(12) . . ?
F1 Si1 F2 90.26(15) . . ?
F4 Si1 F2 176.72(15) . . ?
F3 Si1 F2 90.84(12) . . ?
F5 Si1 F2 88.62(13) . . ?
F6 Si1 F2 86.74(12) . . ?
Si1 F2 Ca2 106.75(12) . . ?
Si1 F3 Ca1 107.09(12) . 2_666 ?
Si1 F4 Ca1 175.67(16) . . ?
Si1 F5 Ca1 107.73(11) . 2_666 ?
Si1 F6 Ca2 105.61(11) . . ?
F16 P1 F15 91.4(4) . . ?
F16 P1 F11 178.9(4) . . ?
F15 P1 F11 89.5(4) . . ?
F16 P1 F14 90.9(4) . . ?
F15 P1 F14 177.3(3) . . ?
F11 P1 F14 88.1(4) . . ?
F16 P1 F12 89.2(3) . . ?
F15 P1 F12 88.9(3) . . ?
F11 P1 F12 90.2(4) . . ?
F14 P1 F12 89.9(3) . . ?
F16 P1 F13 87.1(3) . . ?
F15 P1 F13 91.6(3) . . ?
F11 P1 F13 93.5(4) . . ?
F14 P1 F13 89.8(3) . . ?
F12 P1 F13 176.4(3) . . ?
F23 P2 F24 93.3(5) . . ?
F23 P2 F22 88.4(5) . . ?
F24 P2 F22 177.4(5) . . ?
F23 P2 F26 172.4(4) . . ?
F24 P2 F26 94.1(5) . . ?
F22 P2 F26 84.2(4) . . ?
F23 P2 F21 92.6(3) . . ?
F24 P2 F21 88.0(3) . . ?
F22 P2 F21 93.8(4) . . ?
F26 P2 F21 85.9(3) . . ?
F23 P2 F25 89.4(3) . . ?
F24 P2 F25 87.9(3) . . ?
F22 P2 F25 90.2(4) . . ?
F26 P2 F25 92.6(3) . . ?
F21 P2 F25 175.5(3) . . ?
C1 O1 C10 107.6(7) . . ?
C1 O1 Ca1 119.8(5) . . ?
C10 O1 Ca1 116.6(4) . . ?
C3 O2 C2 116.9(6) . . ?
C3 O2 Ca1 121.2(5) . . ?
C2 O2 Ca1 120.0(5) . . ?
C4 O3 C5 122.6(7) . . ?
C4 O3 Ca1 119.7(5) . . ?
C5 O3 Ca1 113.0(5) . . ?
C6 O4 C7 108.3(7) . . ?
C6 O4 Ca1 119.6(5) . . ?
C7 O4 Ca1 112.3(5) . . ?
C8 O5 C9 114.9(6) . . ?
C8 O5 Ca1 123.6(4) . . ?
C9 O5 Ca1 121.4(4) . . ?
O1 C1 C2 114.3(7) . . ?
O1 C1 H1A 108.7 . . ?
C2 C1 H1A 108.7 . . ?
O1 C1 H1B 108.7 . . ?
C2 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
O2 C2 C1 112.0(7) . . ?
O2 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
O2 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
O2 C3 C4 109.7(7) . . ?
O2 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
O2 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
O3 C4 C3 110.2(6) . . ?
O3 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
O3 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
O3 C5 C6 115.1(7) . . ?
O3 C5 H5A 108.5 . . ?
C6 C5 H5A 108.5 . . ?
O3 C5 H5B 108.5 . . ?
C6 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
O4 C6 C5 108.5(8) . . ?
O4 C6 H6A 110.0 . . ?
C5 C6 H6A 110.0 . . ?
O4 C6 H6B 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
C8 C7 O4 116.9(8) . . ?
C8 C7 H7A 108.1 . . ?
O4 C7 H7A 108.1 . . ?
C8 C7 H7B 108.1 . . ?
O4 C7 H7B 108.1 . . ?
H7A C7 H7B 107.3 . . ?
C7 C8 O5 111.0(7) . . ?
C7 C8 H8A 109.4 . . ?
O5 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
O5 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
O5 C9 C10 114.8(6) . . ?
O5 C9 H9A 108.6 . . ?
C10 C9 H9A 108.6 . . ?
O5 C9 H9B 108.6 . . ?
C10 C9 H9B 108.6 . . ?
H9A C9 H9B 107.5 . . ?
C9 C10 O1 116.3(7) . . ?
C9 C10 H10A 108.2 . . ?
O1 C10 H10A 108.2 . . ?
C9 C10 H10B 108.2 . . ?
O1 C10 H10B 108.2 . . ?
H10A C10 H10B 107.4 . . ?
C11 O11 C20 113.6(5) . . ?
C11 O11 Ca2 111.2(3) . . ?
C20 O11 Ca2 114.6(3) . . ?
C13 O12 C12 116.2(5) . . ?
C13 O12 Ca2 120.3(4) . . ?
C12 O12 Ca2 122.1(4) . . ?
C15 O13 C14 117.4(5) . . ?
C15 O13 Ca2 116.5(3) . . ?
C14 O13 Ca2 117.1(3) . . ?
C16 O14 C17 113.2(4) . . ?
C16 O14 Ca2 111.8(3) . . ?
C17 O14 Ca2 117.1(3) . . ?
C19 O15 C18 114.6(4) . . ?
C19 O15 Ca2 115.8(3) . . ?
C18 O15 Ca2 112.4(3) . . ?
O11 C11 C12 112.5(5) . . ?
O11 C11 H11A 109.1 . . ?
C12 C11 H11A 109.1 . . ?
O11 C11 H11B 109.1 . . ?
C12 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
O12 C12 C11 107.5(5) . . ?
O12 C12 H12A 110.2 . . ?
C11 C12 H12A 110.2 . . ?
O12 C12 H12B 110.2 . . ?
C11 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?
O12 C13 C14 109.2(5) . . ?
O12 C13 H13A 109.8 . . ?
C14 C13 H13A 109.8 . . ?
O12 C13 H13B 109.8 . . ?
C14 C13 H13B 109.8 . . ?
H13A C13 H13B 108.3 . . ?
O13 C14 C13 108.0(5) . . ?
O13 C14 H14A 110.1 . . ?
C13 C14 H14A 110.1 . . ?
O13 C14 H14B 110.1 . . ?
C13 C14 H14B 110.1 . . ?
H14A C14 H14B 108.4 . . ?
O13 C15 C16 108.1(4) . . ?
O13 C15 H15A 110.1 . . ?
C16 C15 H15A 110.1 . . ?
O13 C15 H15B 110.1 . . ?
C16 C15 H15B 110.1 . . ?
H15A C15 H15B 108.4 . . ?
O14 C16 C15 111.3(5) . . ?
O14 C16 H16A 109.4 . . ?
C15 C16 H16A 109.4 . . ?
O14 C16 H16B 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C18 C17 O14 110.6(4) . . ?
C18 C17 H17A 109.5 . . ?
O14 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
O14 C17 H17B 109.5 . . ?
H17A C17 H17B 108.1 . . ?
C17 C18 O15 109.3(4) . . ?
C17 C18 H18A 109.8 . . ?
O15 C18 H18A 109.8 . . ?
C17 C18 H18B 109.8 . . ?
O15 C18 H18B 109.8 . . ?
H18A C18 H18B 108.3 . . ?
O15 C19 C20 108.0(4) . . ?
O15 C19 H19A 110.1 . . ?
C20 C19 H19A 110.1 . . ?
O15 C19 H19B 110.1 . . ?
C20 C19 H19B 110.1 . . ?
H19A C19 H19B 108.4 . . ?
O11 C20 C19 108.1(5) . . ?
O11 C20 H20A 110.1 . . ?
C19 C20 H20A 110.1 . . ?
O11 C20 H20B 110.1 . . ?
C19 C20 H20B 110.1 . . ?
H20A C20 H20B 108.4 . . ?
C101 N100 Ca2 171.7(4) . . ?
N100 C101 C102 178.7(6) . . ?
C101 C102 H10C 109.5 . . ?
C101 C102 H10D 109.5 . . ?
H10C C102 H10D 109.5 . . ?
C101 C102 H10E 109.5 . . ?
H10C C102 H10E 109.5 . . ?
H10D C102 H10E 109.5 . . ?
N200 C201 C202 179.5(8) . . ?
C201 C202 H20C 109.5 . . ?
C201 C202 H20D 109.5 . . ?
H20C C202 H20D 109.5 . . ?
C201 C202 H20E 109.5 . . ?
H20C C202 H20E 109.5 . . ?
H20D C202 H20E 109.5 . . ?
N300 C301 C302 179.2(9) . . ?
C301 C302 H30A 109.5 . . ?
C301 C302 H30B 109.5 . . ?
H30A C302 H30B 109.5 . . ?
C301 C302 H30C 109.5 . . ?
H30A C302 H30C 109.5 . . ?
H30B C302 H30C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F1 Si1 F2 Ca2 84.78(15) . . . . ?
F3 Si1 F2 Ca2 176.67(13) . . . . ?
F5 Si1 F2 Ca2 -97.10(13) . . . . ?
F6 Si1 F2 Ca2 -6.60(14) . . . . ?
F1 Si1 F3 Ca1 176.10(14) . . . 2_666 ?
F4 Si1 F3 Ca1 -92.03(13) . . . 2_666 ?
F5 Si1 F3 Ca1 -2.75(12) . . . 2_666 ?
F2 Si1 F3 Ca1 85.81(14) . . . 2_666 ?
F4 Si1 F5 Ca1 94.46(13) . . . 2_666 ?
F3 Si1 F5 Ca1 2.79(13) . . . 2_666 ?
F6 Si1 F5 Ca1 -174.88(12) . . . 2_666 ?
F2 Si1 F5 Ca1 -88.15(12) . . . 2_666 ?
F1 Si1 F6 Ca2 -83.73(14) . . . . ?
F4 Si1 F6 Ca2 -175.56(13) . . . . ?
F5 Si1 F6 Ca2 95.04(12) . . . . ?
F2 Si1 F6 Ca2 6.45(13) . . . . ?
C10 O1 C1 C2 -152.8(11) . . . . ?
Ca1 O1 C1 C2 -16.5(15) . . . . ?
C3 O2 C2 C1 161.0(10) . . . . ?
Ca1 O2 C2 C1 -34.5(13) . . . . ?
O1 C1 C2 O2 32.0(16) . . . . ?
C2 O2 C3 C4 -155.2(9) . . . . ?
Ca1 O2 C3 C4 40.5(10) . . . . ?
C5 O3 C4 C3 -176.7(8) . . . . ?
Ca1 O3 C4 C3 29.3(10) . . . . ?
O2 C3 C4 O3 -42.7(11) . . . . ?
C4 O3 C5 C6 -115.5(11) . . . . ?
Ca1 O3 C5 C6 40.1(12) . . . . ?
C7 O4 C6 C5 162.9(10) . . . . ?
Ca1 O4 C6 C5 32.5(14) . . . . ?
O3 C5 C6 O4 -47.5(15) . . . . ?
C6 O4 C7 C8 -97.0(12) . . . . ?
Ca1 O4 C7 C8 37.3(12) . . . . ?
O4 C7 C8 O5 -35.2(13) . . . . ?
C9 O5 C8 C7 -159.0(9) . . . . ?
Ca1 O5 C8 C7 17.0(11) . . . . ?
C8 O5 C9 C10 171.4(10) . . . . ?
Ca1 O5 C9 C10 -4.8(12) . . . . ?
O5 C9 C10 O1 20.8(16) . . . . ?
C1 O1 C10 C9 110.9(12) . . . . ?
Ca1 O1 C10 C9 -27.0(14) . . . . ?
C20 O11 C11 C12 78.3(7) . . . . ?
Ca2 O11 C11 C12 -52.7(6) . . . . ?
C13 O12 C12 C11 175.8(6) . . . . ?
Ca2 O12 C12 C11 -17.7(7) . . . . ?
O11 C11 C12 O12 45.9(7) . . . . ?
C12 O12 C13 C14 125.0(6) . . . . ?
Ca2 O12 C13 C14 -41.8(7) . . . . ?
C15 O13 C14 C13 174.2(5) . . . . ?
Ca2 O13 C14 C13 -39.7(6) . . . . ?
O12 C13 C14 O13 50.6(7) . . . . ?
C14 O13 C15 C16 175.3(5) . . . . ?
Ca2 O13 C15 C16 29.0(6) . . . . ?
C17 O14 C16 C15 -80.7(6) . . . . ?
Ca2 O14 C16 C15 54.2(5) . . . . ?
O13 C15 C16 O14 -54.6(6) . . . . ?
C16 O14 C17 C18 159.2(5) . . . . ?
Ca2 O14 C17 C18 26.9(6) . . . . ?
O14 C17 C18 O15 -51.7(6) . . . . ?
C19 O15 C18 C17 -172.0(5) . . . . ?
Ca2 O15 C18 C17 53.1(5) . . . . ?
C18 O15 C19 C20 -178.4(5) . . . . ?
Ca2 O15 C19 C20 -45.1(6) . . . . ?
C11 O11 C20 C19 -174.5(5) . . . . ?
Ca2 O11 C20 C19 -45.2(6) . . . . ?
O15 C19 C20 O11 58.3(7) . . . . ?

