# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# 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_compound_2_sq
_database_code_depnum_ccdc_archive 'CCDC 1543622'
_audit_update_record             
;
2017-04-12 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C128 H208 Co4 N40 O76 P8'
_chemical_formula_weight         4006.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_H-M_alt        'I 4 2 2'
_space_group_name_Hall           'I 4 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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   24.556(4)
_cell_length_b                   24.556(4)
_cell_length_c                   17.680(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10661(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5874
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      20.28

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_F_000             4184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    0.454
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6855
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54581
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.173
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6641
_reflns_number_gt                3395
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
'Refined as a 2-component inversion twin., SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] 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_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.28(6)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         6641
_refine_ls_number_parameters     195
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.1589
_refine_ls_R_factor_gt           0.0861
_refine_ls_wR_factor_ref         0.3228
_refine_ls_wR_factor_gt          0.2665
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.24058(6) 0.5000 0.0650(5) Uani 1 2 d S T P . .
O2 O 0.5000 0.3268(3) 0.5000 0.075(2) Uani 1 2 d S T P . .
O3 O 0.5000 0.1557(4) 0.5000 0.109(3) Uani 1 2 d S T P . .
P1 P 0.63850(12) 0.36017(11) 0.28833(12) 0.0777(7) Uani 1 1 d . . . . .
O1 O 0.6032(3) 0.3911(3) 0.3391(4) 0.0923(19) Uani 1 1 d . . . . .
N1 N 0.6732(4) 0.3137(4) 0.3349(4) 0.088(2) Uani 1 1 d . . . . .
H1 H 0.7078 0.3105 0.3225 0.105 Uiso 1 1 calc R U . . .
C11 C 0.6549(4) 0.2790(3) 0.3911(4) 0.065(2) Uani 1 1 d . . . . .
C12 C 0.6016(4) 0.2772(4) 0.4134(5) 0.069(2) Uani 1 1 d . . . . .
H12 H 0.5758 0.3001 0.3891 0.083 Uiso 1 1 calc R U . . .
N13 N 0.5847(3) 0.2435(3) 0.4693(4) 0.0699(18) Uani 1 1 d . . . . .
C14 C 0.6213(3) 0.2093(3) 0.5025(6) 0.073(2) Uani 1 1 d . . . . .
H14 H 0.6090 0.1840 0.5393 0.088 Uiso 1 1 calc R U . . .
C15 C 0.6747(4) 0.2104(4) 0.4843(10) 0.103(4) Uani 1 1 d . . . . .
H15 H 0.6995 0.1876 0.5105 0.124 Uiso 1 1 calc R U . . .
C16 C 0.6940(4) 0.2452(4) 0.4263(5) 0.070(2) Uani 1 1 d . . . . .
H16 H 0.7313 0.2459 0.4119 0.084 Uiso 1 1 calc R U . . .
N2 N 0.6843(4) 0.3943(3) 0.2460(5) 0.090(2) Uani 1 1 d . . . . .
H2 H 0.6861 0.3893 0.1967 0.108 Uiso 1 1 calc R U . . .
C21 C 0.7232(4) 0.4321(4) 0.2762(5) 0.074(2) Uani 1 1 d . . . . .
C22 C 0.7238(4) 0.4438(3) 0.3521(5) 0.071(2) Uani 1 1 d . . . . .
H22 H 0.6969 0.4282 0.3842 0.085 Uiso 1 1 calc R U . . .
N23 N 0.7620(3) 0.4771(3) 0.3821(4) 0.0639(16) Uani 1 1 d . . . . .
C24 C 0.7958(3) 0.5025(5) 0.3363(4) 0.0697(19) Uani 1 1 d . . . . .
H24 H 0.8207 0.5283 0.3564 0.084 Uiso 1 1 calc R U . . .
C25 C 0.7956(4) 0.4920(6) 0.2577(6) 0.096(3) Uani 1 1 d . . . . .
H25 H 0.8198 0.5108 0.2248 0.115 Uiso 1 1 calc R U . . .
C26 C 0.7601(4) 0.4545(4) 0.2301(5) 0.071(2) Uani 1 1 d . . . . .
H26 H 0.7615 0.4442 0.1783 0.086 Uiso 1 1 calc R U . . .
C1 C 0.5995(5) 0.3323(4) 0.2157(5) 0.108(3) Uiso 0.805(8) 1 d DG U P A 1
C2 C 0.6150(4) 0.2838(4) 0.1815(7) 0.115(3) Uiso 0.805(8) 1 d DG U P A 1
H2A H 0.6455 0.2641 0.2003 0.138 Uiso 0.805(8) 1 calc R U P A 1
C3 C 0.5860(5) 0.2640(4) 0.1199(7) 0.121(3) Uiso 0.805(8) 1 d DG U P A 1
H3 H 0.5966 0.2308 0.0965 0.145 Uiso 0.805(8) 1 calc R U P A 1
C4 C 0.5414(5) 0.2928(5) 0.0925(6) 0.128(4) Uiso 0.805(8) 1 d DG U P A 1
H4 H 0.5215 0.2792 0.0503 0.154 Uiso 0.805(8) 1 calc R U P A 1
C5 C 0.5259(4) 0.3413(4) 0.1267(6) 0.131(4) Uiso 0.805(8) 1 d DG U P A 1
H5 H 0.4954 0.3610 0.1079 0.157 Uiso 0.805(8) 1 calc R U P A 1
C6 C 0.5549(5) 0.3611(4) 0.1883(6) 0.116(3) Uiso 0.805(8) 1 d DG U P A 1
H6 H 0.5443 0.3943 0.2117 0.140 Uiso 0.805(8) 1 calc R U P A 1
C1' C 0.618(2) 0.3187(17) 0.213(3) 0.112(4) Uiso 0.195(8) 1 d DG U P A 2
C2' C 0.6447(18) 0.2695(19) 0.226(2) 0.113(4) Uiso 0.195(8) 1 d DG U P A 2
H2' H 0.6679 0.2657 0.2690 0.136 Uiso 0.195(8) 1 calc R U P A 2
C3' C 0.6371(19) 0.2258(15) 0.177(3) 0.118(4) Uiso 0.195(8) 1 d DG U P A 2
H3' H 0.6551 0.1922 0.1867 0.141 Uiso 0.195(8) 1 calc R U P A 2
C4' C 0.603(2) 0.2313(16) 0.115(2) 0.117(4) Uiso 0.195(8) 1 d DG U P A 2
H4' H 0.5979 0.2015 0.0815 0.140 Uiso 0.195(8) 1 calc R U P A 2
C5' C 0.577(2) 0.2805(19) 0.101(2) 0.122(4) Uiso 0.195(8) 1 d DG U P A 2
H5' H 0.5537 0.2843 0.0587 0.146 Uiso 0.195(8) 1 calc R U P A 2
C6' C 0.584(2) 0.3242(15) 0.150(3) 0.119(3) Uiso 0.195(8) 1 d DG U P A 2
H6' H 0.5665 0.3578 0.1410 0.143 Uiso 0.195(8) 1 calc R U P A 2
O4 O 0.5001(8) 0.3983(6) 0.6088(7) 0.096(3) Uiso 0.5 1 d . . P . .
O5 O 0.5739(10) 0.3970(11) 0.501(3) 0.202(10) Uiso 0.5 1 d . . P . .
O6 O 0.5000 0.5000 0.5000 0.214(16) Uiso 1 8 d S . 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
Co1 O3 2.084(10) . ?
Co1 O2 2.118(7) . ?
Co1 N13 2.150(7) . ?
Co1 N13 2.150(7) 5_656 ?
Co1 N23 2.160(7) 8_666 ?
Co1 N23 2.160(7) 4_565 ?
P1 O1 1.460(7) . ?
P1 N2 1.591(9) . ?
P1 N1 1.646(9) . ?
P1 C1 1.742(8) . ?
P1 C1' 1.75(3) . ?
N1 C11 1.384(12) . ?
N1 H1 0.8800 . ?
C11 C12 1.368(12) . ?
C11 C16 1.413(13) . ?
C12 N13 1.354(11) . ?
C12 H12 0.9500 . ?
N13 C14 1.364(11) . ?
C14 C15 1.350(13) . ?
C14 H14 0.9500 . ?
C15 C16 1.417(16) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
N2 C21 1.436(12) . ?
N2 H2 0.8800 . ?
C21 C26 1.337(12) . ?
C21 C22 1.372(13) . ?
C22 N23 1.353(10) . ?
C22 H22 0.9500 . ?
N23 C24 1.315(10) . ?
N23 Co1 2.161(7) 3_655 ?
C24 C25 1.413(14) . ?
C24 H24 0.9500 . ?
C25 C26 1.358(15) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C2 C3 1.3900 . ?
C2 H2A 0.9500 . ?
C3 C4 1.3900 . ?
C3 H3 0.9500 . ?
C4 C5 1.3900 . ?
C4 H4 0.9500 . ?
C5 C6 1.3900 . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C1' C2' 1.3900 . ?
C1' C6' 1.3900 . ?
C2' C3' 1.3900 . ?
C2' H2' 0.9500 . ?
C3' C4' 1.3900 . ?
C3' H3' 0.9500 . ?
C4' C5' 1.3900 . ?
C4' H4' 0.9500 . ?
C5' C6' 1.3900 . ?
C5' H5' 0.9500 . ?
C6' H6' 0.9500 . ?
O5 O5 1.01(5) 8_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Co1 O2 180.0 . . ?
O3 Co1 N13 91.90(19) . . ?
O2 Co1 N13 88.10(19) . . ?
O3 Co1 N13 91.90(19) . 5_656 ?
O2 Co1 N13 88.10(19) . 5_656 ?
N13 Co1 N13 176.2(4) . 5_656 ?
O3 Co1 N23 88.30(18) . 8_666 ?
O2 Co1 N23 91.70(18) . 8_666 ?
N13 Co1 N23 89.6(3) . 8_666 ?
N13 Co1 N23 90.5(3) 5_656 8_666 ?
O3 Co1 N23 88.30(18) . 4_565 ?
O2 Co1 N23 91.70(18) . 4_565 ?
N13 Co1 N23 90.5(3) . 4_565 ?
N13 Co1 N23 89.6(3) 5_656 4_565 ?
N23 Co1 N23 176.6(4) 8_666 4_565 ?
O1 P1 N2 115.7(5) . . ?
O1 P1 N1 111.2(4) . . ?
N2 P1 N1 103.6(5) . . ?
O1 P1 C1 109.3(5) . . ?
N2 P1 C1 104.4(5) . . ?
N1 P1 C1 112.4(5) . . ?
O1 P1 C1' 127.2(18) . . ?
N2 P1 C1' 98.4(18) . . ?
N1 P1 C1' 97.1(16) . . ?
C11 N1 P1 128.1(7) . . ?
C11 N1 H1 115.9 . . ?
P1 N1 H1 115.9 . . ?
C12 C11 N1 122.6(9) . . ?
C12 C11 C16 120.3(8) . . ?
N1 C11 C16 117.1(8) . . ?
N13 C12 C11 121.6(8) . . ?
N13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C12 N13 C14 119.2(8) . . ?
C12 N13 Co1 120.1(6) . . ?
C14 N13 Co1 120.6(6) . . ?
C15 C14 N13 121.7(10) . . ?
C15 C14 H14 119.1 . . ?
N13 C14 H14 119.1 . . ?
C14 C15 C16 120.6(10) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C11 C16 C15 116.5(8) . . ?
C11 C16 H16 121.8 . . ?
C15 C16 H16 121.8 . . ?
C21 N2 P1 129.5(7) . . ?
C21 N2 H2 115.2 . . ?
P1 N2 H2 115.2 . . ?
C26 C21 C22 120.3(8) . . ?
C26 C21 N2 119.3(8) . . ?
C22 C21 N2 120.4(8) . . ?
N23 C22 C21 121.0(8) . . ?
N23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C24 N23 C22 118.8(7) . . ?
C24 N23 Co1 119.3(5) . 3_655 ?
C22 N23 Co1 121.0(6) . 3_655 ?
N23 C24 C25 121.2(9) . . ?
N23 C24 H24 119.4 . . ?
C25 C24 H24 119.4 . . ?
C26 C25 C24 118.6(8) . . ?
C26 C25 H25 120.7 . . ?
C24 C25 H25 120.7 . . ?
C21 C26 C25 119.6(8) . . ?
C21 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C2 C1 C6 120.0 . . ?
C2 C1 P1 120.4(7) . . ?
C6 C1 P1 119.4(7) . . ?
C3 C2 C1 120.0 . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C1 120.0 . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
C2' C1' C6' 120.0 . . ?
C2' C1' P1 104(3) . . ?
C6' C1' P1 136(3) . . ?
C3' C2' C1' 120.0 . . ?
C3' C2' H2' 120.0 . . ?
C1' C2' H2' 120.0 . . ?
C4' C3' C2' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
C2' C3' H3' 120.0 . . ?
C3' C4' C5' 120.0 . . ?
C3' C4' H4' 120.0 . . ?
C5' C4' H4' 120.0 . . ?
C6' C5' C4' 120.0 . . ?
C6' C5' H5' 120.0 . . ?
C4' C5' H5' 120.0 . . ?
C5' C6' C1' 120.0 . . ?
C5' C6' H6' 120.0 . . ?
C1' C6' H6' 120.0 . . ?

_refine_diff_density_max         0.765
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.087




_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol and water'
####################################################################### 
# 
# 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_compound_Hy-Cs_2_sq
_database_code_depnum_ccdc_archive 'CCDC 1543623'
_audit_update_record             
;
2017-04-12 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C128 H206 Co4 Cs N41 O78 P8'
_chemical_formula_weight         4183.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_H-M_alt        'I 4 2 2'
_space_group_name_Hall           'I 4 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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   24.580(3)
_cell_length_b                   24.580(3)
_cell_length_c                   17.611(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10640(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9982
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      24.85

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_F_000             4336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.625
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6292
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54731
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.422
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6612
_reflns_number_gt                5213
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
'Refined as a 2-component inversion twin., SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0605P)²+6.6976P] 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_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(3)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         6612
_refine_ls_number_parameters     201
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.1133
_refine_ls_wR_factor_gt          0.1002
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.23632(2) 0.5000 0.5000 0.04491(17) Uani 1 2 d S T P . .
O2 O 0.32078(11) 0.5000 0.5000 0.0441(7) Uani 1 2 d S T P . .
O3 O 0.15076(14) 0.5000 0.5000 0.0714(11) Uani 1 2 d S T P . .
Cs1 Cs 0.5000 0.5000 0.5000 0.03952(14) Uani 1 8 d S T P . .
O4 O 0.39367(16) 0.5020(3) 0.6121(2) 0.0492(7) Uiso 0.597(3) 1 d . U P . .
O4' O 0.4234(4) 0.4979(6) 0.6498(5) 0.0492(7) Uiso 0.266(3) 1 d . U P . .
O5 O 0.4182(2) 0.3905(2) 0.5001(6) 0.0492(7) Uiso 0.386(3) 1 d . U P . .
P1 P 0.35903(6) 0.35772(5) 0.29046(5) 0.0516(2) Uani 1 1 d . . . . .
O1 O 0.39257(14) 0.38953(14) 0.34432(15) 0.0555(6) Uani 1 1 d . . . . .
N1 N 0.31267(19) 0.39315(17) 0.2448(2) 0.0648(11) Uani 1 1 d . . . . .
H1 H 0.3119 0.3892 0.1951 0.078 Uiso 1 1 calc R U . . .
C11 C 0.27428(18) 0.42885(17) 0.2759(3) 0.0519(10) Uani 1 1 d . . . . .
C12 C 0.27123(15) 0.44083(16) 0.3529(2) 0.0465(9) Uani 1 1 d . . . . .
H12 H 0.2954 0.4228 0.3866 0.056 Uiso 1 1 calc R U . . .
N13 N 0.23568(13) 0.47675(14) 0.3818(2) 0.0489(8) Uani 1 1 d . . . . .
C14 C 0.20071(15) 0.5020(3) 0.3347(2) 0.0574(9) Uani 1 1 d . . . . .
H14 H 0.1759 0.5278 0.3549 0.069 Uiso 1 1 calc R U . . .
C15 C 0.2001(2) 0.4913(3) 0.2574(3) 0.0718(16) Uani 1 1 d . . . . .
H15 H 0.1747 0.5090 0.2251 0.086 Uiso 1 1 calc R U . . .
C16 C 0.2370(2) 0.4546(2) 0.2282(3) 0.0639(12) Uani 1 1 d . . . . .
H16 H 0.2370 0.4467 0.1754 0.077 Uiso 1 1 calc R U . . .
N2 N 0.32391(16) 0.31087(16) 0.3361(2) 0.0599(10) Uani 1 1 d . . . . .
H2 H 0.2892 0.3087 0.3242 0.072 Uiso 1 1 calc R U . . .
C21 C 0.34224(17) 0.27362(17) 0.3921(3) 0.0520(10) Uani 1 1 d . . . . .
C22 C 0.39696(16) 0.27150(16) 0.4132(3) 0.0489(9) Uani 1 1 d . . . . .
H22 H 0.4224 0.2944 0.3880 0.059 Uiso 1 1 calc R U . . .
N23 N 0.41462(14) 0.23792(12) 0.4682(2) 0.0478(8) Uani 1 1 d . . . . .
C24 C 0.37827(15) 0.20550(15) 0.5025(4) 0.0615(10) Uani 1 1 d . . . . .
H24 H 0.3906 0.1817 0.5413 0.074 Uiso 1 1 calc R U . . .
C25 C 0.32368(19) 0.2052(2) 0.4839(4) 0.0723(16) Uani 1 1 d . . . . .
H25 H 0.2990 0.1816 0.5092 0.087 Uiso 1 1 calc R U . . .
C26 C 0.30595(19) 0.24011(19) 0.4275(3) 0.0632(12) Uani 1 1 d . . . . .
H26 H 0.2686 0.2408 0.4134 0.076 Uiso 1 1 calc R U . . .
C1 C 0.4042(3) 0.3344(4) 0.2166(4) 0.058(3) Uiso 0.503(18) 1 d DG U P A 1
C2 C 0.3902(3) 0.2868(4) 0.1786(5) 0.067(3) Uiso 0.503(18) 1 d DG U P A 1
H2A H 0.3593 0.2666 0.1942 0.081 Uiso 0.503(18) 1 calc R U P A 1
C3 C 0.4217(4) 0.2689(4) 0.1180(5) 0.085(4) Uiso 0.503(18) 1 d DG U P A 1
H3 H 0.4121 0.2364 0.0921 0.102 Uiso 0.503(18) 1 calc R U P A 1
C4 C 0.4670(4) 0.2985(4) 0.0953(4) 0.087(4) Uiso 0.503(18) 1 d DG U P A 1
H4 H 0.4885 0.2862 0.0538 0.104 Uiso 0.503(18) 1 calc R U P A 1
C5 C 0.4809(4) 0.3461(4) 0.1333(5) 0.083(4) Uiso 0.503(18) 1 d DG U P A 1
H5 H 0.5119 0.3663 0.1177 0.099 Uiso 0.503(18) 1 calc R U P A 1
C6 C 0.4495(4) 0.3640(3) 0.1939(5) 0.078(3) Uiso 0.503(18) 1 d DG U P A 1
H6 H 0.4590 0.3966 0.2199 0.093 Uiso 0.503(18) 1 calc R U P A 1
C1' C 0.3921(4) 0.3217(4) 0.2146(4) 0.063(3) Uiso 0.497(18) 1 d G . P A 2
C2' C 0.3752(3) 0.2715(4) 0.1870(5) 0.068(3) Uiso 0.497(18) 1 d G . P A 2
H2' H 0.3451 0.2535 0.2095 0.081 Uiso 0.497(18) 1 calc R U P A 2
C3' C 0.4026(4) 0.2476(4) 0.1265(5) 0.083(4) Uiso 0.497(18) 1 d G . P A 2
H3' H 0.3911 0.2132 0.1076 0.100 Uiso 0.497(18) 1 calc R U P A 2
C4' C 0.4467(4) 0.2739(5) 0.0935(4) 0.085(4) Uiso 0.497(18) 1 d G . P A 2
H4' H 0.4654 0.2575 0.0522 0.101 Uiso 0.497(18) 1 calc R U P A 2
C5' C 0.4635(4) 0.3241(4) 0.1211(5) 0.090(4) Uiso 0.497(18) 1 d G . P A 2
H5' H 0.4937 0.3421 0.0986 0.108 Uiso 0.497(18) 1 calc R U P A 2
C6' C 0.4362(4) 0.3480(3) 0.1816(5) 0.082(4) Uiso 0.497(18) 1 d G . P A 2
H6' H 0.4477 0.3824 0.2005 0.099 Uiso 0.497(18) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2 2.076(3) . ?
Co1 O3 2.103(4) . ?
Co1 N13 2.158(4) . ?
Co1 N13 2.158(4) 6_566 ?
Co1 N23 2.172(3) 7_556 ?
Co1 N23 2.172(3) 4_565 ?
Cs1 O4' 3.242(9) 7_556 ?
Cs1 O4' 3.242(9) 6_566 ?
Cs1 O4' 3.242(9) 4_565 ?
Cs1 O4' 3.242(9) 2_665 ?
Cs1 O4' 3.242(9) 8_666 ?
Cs1 O4' 3.242(9) 5_656 ?
Cs1 O4' 3.242(9) 3_655 ?
Cs1 O4' 3.242(9) . ?
Cs1 O4 3.276(4) 6_566 ?
Cs1 O4 3.276(4) 4_565 ?
Cs1 O4 3.276(4) 2_665 ?
Cs1 O4 3.276(4) 7_556 ?
O4 O4' 0.992(9) . ?
O5 O5 0.964(10) 7_556 ?
P1 O1 1.480(3) . ?
P1 N1 1.644(4) . ?
P1 N2 1.649(4) . ?
P1 C1' 1.797(6) . ?
P1 C1 1.803(6) . ?
N1 C11 1.400(6) . ?
N1 H1 0.8800 . ?
C11 C12 1.389(6) . ?
C11 C16 1.395(6) . ?
C12 N13 1.343(5) . ?
C12 H12 0.9500 . ?
N13 C14 1.347(5) . ?
C14 C15 1.387(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.378(8) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
N2 C21 1.419(6) . ?
N2 H2 0.8800 . ?
C21 C26 1.365(6) . ?
C21 C22 1.396(6) . ?
C22 N23 1.345(5) . ?
C22 H22 0.9500 . ?
N23 C24 1.341(5) . ?
N23 Co1 2.172(3) 3_655 ?
C24 C25 1.381(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.384(7) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C2 C3 1.3900 . ?
C2 H2A 0.9500 . ?
C3 C4 1.3900 . ?
C3 H3 0.9500 . ?
C4 C5 1.3900 . ?
C4 H4 0.9500 . ?
C5 C6 1.3900 . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C1' C2' 1.3900 . ?
C1' C6' 1.3900 . ?
C2' C3' 1.3900 . ?
C2' H2' 0.9500 . ?
C3' C4' 1.3900 . ?
C3' H3' 0.9500 . ?
C4' C5' 1.3900 . ?
C4' H4' 0.9500 . ?
C5' C6' 1.3900 . ?
C5' H5' 0.9500 . ?
C6' H6' 0.9500 . ?

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 Co1 O3 180.0 . . ?
O2 Co1 N13 90.42(9) . . ?
O3 Co1 N13 89.58(9) . . ?
O2 Co1 N13 90.42(9) . 6_566 ?
O3 Co1 N13 89.58(9) . 6_566 ?
N13 Co1 N13 179.16(17) . 6_566 ?
O2 Co1 N23 88.97(8) . 7_556 ?
O3 Co1 N23 91.03(8) . 7_556 ?
N13 Co1 N23 89.59(13) . 7_556 ?
N13 Co1 N23 90.42(13) 6_566 7_556 ?
O2 Co1 N23 88.97(8) . 4_565 ?
O3 Co1 N23 91.03(8) . 4_565 ?
N13 Co1 N23 90.42(13) . 4_565 ?
N13 Co1 N23 89.59(13) 6_566 4_565 ?
N23 Co1 N23 177.94(16) 7_556 4_565 ?
O4' Cs1 O4' 48.5(2) 7_556 6_566 ?
O4' Cs1 O4' 178.2(5) 7_556 4_565 ?
O4' Cs1 O4' 130.1(4) 6_566 4_565 ?
O4' Cs1 O4' 132.9(4) 7_556 2_665 ?
O4' Cs1 O4' 178.2(5) 6_566 2_665 ?
O4' Cs1 O4' 48.5(2) 4_565 2_665 ?
O4' Cs1 O4' 71.1(3) 7_556 8_666 ?
O4' Cs1 O4' 48.5(2) 6_566 8_666 ?
O4' Cs1 O4' 109.0(3) 4_565 8_666 ?
O4' Cs1 O4' 130.1(4) 2_665 8_666 ?
O4' Cs1 O4' 48.5(2) 7_556 5_656 ?
O4' Cs1 O4' 71.1(3) 6_566 5_656 ?
O4' Cs1 O4' 132.9(4) 4_565 5_656 ?
O4' Cs1 O4' 109.0(3) 2_665 5_656 ?
O4' Cs1 O4' 48.5(2) 8_666 5_656 ?
O4' Cs1 O4' 109.0(3) 7_556 3_655 ?
O4' Cs1 O4' 132.9(4) 6_566 3_655 ?
O4' Cs1 O4' 71.1(3) 4_565 3_655 ?
O4' Cs1 O4' 48.5(2) 2_665 3_655 ?
O4' Cs1 O4' 178.2(5) 8_666 3_655 ?
O4' Cs1 O4' 130.1(4) 5_656 3_655 ?
O4' Cs1 O4' 130.0(4) 7_556 . ?
O4' Cs1 O4' 109.0(3) 6_566 . ?
O4' Cs1 O4' 48.5(2) 4_565 . ?
O4' Cs1 O4' 71.1(3) 2_665 . ?
O4' Cs1 O4' 132.9(4) 8_666 . ?
O4' Cs1 O4' 178.1(5) 5_656 . ?
O4' Cs1 O4' 48.5(2) 3_655 . ?
O4' Cs1 O4 59.2(3) 7_556 6_566 ?
O4' Cs1 O4 17.50(16) 6_566 6_566 ?
O4' Cs1 O4 119.1(3) 4_565 6_566 ?
O4' Cs1 O4 162.59(15) 2_665 6_566 ?
O4' Cs1 O4 62.0(3) 8_666 6_566 ?
O4' Cs1 O4 88.44(19) 5_656 6_566 ?
O4' Cs1 O4 119.6(3) 3_655 6_566 ?
O4' Cs1 O4 91.53(19) . 6_566 ?
O4' Cs1 O4 162.59(15) 7_556 4_565 ?
O4' Cs1 O4 119.1(3) 6_566 4_565 ?
O4' Cs1 O4 17.50(16) 4_565 4_565 ?
O4' Cs1 O4 59.2(3) 2_665 4_565 ?
O4' Cs1 O4 91.53(19) 8_666 4_565 ?
O4' Cs1 O4 119.6(3) 5_656 4_565 ?
O4' Cs1 O4 88.44(19) 3_655 4_565 ?
O4' Cs1 O4 62.0(3) . 4_565 ?
O4 Cs1 O4 112.8(2) 6_566 4_565 ?
O4' Cs1 O4 119.6(3) 7_556 2_665 ?
O4' Cs1 O4 162.59(15) 6_566 2_665 ?
O4' Cs1 O4 62.0(3) 4_565 2_665 ?
O4' Cs1 O4 17.50(16) 2_665 2_665 ?
O4' Cs1 O4 119.1(3) 8_666 2_665 ?
O4' Cs1 O4 91.53(19) 5_656 2_665 ?
O4' Cs1 O4 59.2(3) 3_655 2_665 ?
O4' Cs1 O4 88.44(19) . 2_665 ?
O4 Cs1 O4 178.3(2) 6_566 2_665 ?
O4 Cs1 O4 68.70(7) 4_565 2_665 ?
O4' Cs1 O4 17.50(16) 7_556 7_556 ?
O4' Cs1 O4 62.0(3) 6_566 7_556 ?
O4' Cs1 O4 162.59(15) 4_565 7_556 ?
O4' Cs1 O4 119.6(3) 2_665 7_556 ?
O4' Cs1 O4 88.44(19) 8_666 7_556 ?
O4' Cs1 O4 59.2(3) 5_656 7_556 ?
O4' Cs1 O4 91.53(19) 3_655 7_556 ?
O4' Cs1 O4 119.1(3) . 7_556 ?
O4 Cs1 O4 68.70(7) 6_566 7_556 ?
O4 Cs1 O4 178.3(2) 4_565 7_556 ?
O4 Cs1 O4 109.8(2) 2_665 7_556 ?
O4' O4 Cs1 79.4(5) . . ?
O4 O4' Cs1 83.1(6) . . ?
O5 O5 Cs1 81.76(9) 7_556 . ?
O1 P1 N1 114.8(2) . . ?
O1 P1 N2 110.35(17) . . ?
N1 P1 N2 104.2(2) . . ?
O1 P1 C1' 119.0(4) . . ?
N1 P1 C1' 102.1(4) . . ?
N2 P1 C1' 104.8(3) . . ?
O1 P1 C1 106.7(3) . . ?
N1 P1 C1 104.0(3) . . ?
N2 P1 C1 116.9(3) . . ?
C11 N1 P1 127.4(3) . . ?
C11 N1 H1 116.3 . . ?
P1 N1 H1 116.3 . . ?
C12 C11 C16 117.1(4) . . ?
C12 C11 N1 123.4(4) . . ?
C16 C11 N1 119.4(4) . . ?
N13 C12 C11 123.0(4) . . ?
N13 C12 H12 118.5 . . ?
C11 C12 H12 118.5 . . ?
C12 N13 C14 119.0(4) . . ?
C12 N13 Co1 122.4(3) . . ?
C14 N13 Co1 118.5(3) . . ?
N13 C14 C15 121.6(5) . . ?
N13 C14 H14 119.2 . . ?
C15 C14 H14 119.2 . . ?
C16 C15 C14 118.9(4) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C11 120.3(4) . . ?
C15 C16 H16 119.9 . . ?
C11 C16 H16 119.9 . . ?
C21 N2 P1 128.6(3) . . ?
C21 N2 H2 115.7 . . ?
P1 N2 H2 115.7 . . ?
C26 C21 C22 119.0(4) . . ?
C26 C21 N2 119.9(4) . . ?
C22 C21 N2 121.0(4) . . ?
N23 C22 C21 121.7(4) . . ?
N23 C22 H22 119.1 . . ?
C21 C22 H22 119.1 . . ?
C24 N23 C22 118.3(4) . . ?
C24 N23 Co1 121.1(3) . 3_655 ?
C22 N23 Co1 120.6(3) . 3_655 ?
N23 C24 C25 123.0(5) . . ?
N23 C24 H24 118.5 . . ?
C25 C24 H24 118.5 . . ?
C24 C25 C26 118.2(5) . . ?
C24 C25 H25 120.9 . . ?
C26 C25 H25 120.9 . . ?
C21 C26 C25 119.8(4) . . ?
C21 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C2 C1 C6 120.0 . . ?
C2 C1 P1 117.6(4) . . ?
C6 C1 P1 122.3(4) . . ?
C1 C2 C3 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C3 C2 H2A 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C1 120.0 . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
C2' C1' C6' 120.0 . . ?
C2' C1' P1 124.2(5) . . ?
C6' C1' P1 115.7(5) . . ?
C1' C2' C3' 120.0 . . ?
C1' C2' H2' 120.0 . . ?
C3' C2' H2' 120.0 . . ?
C4' C3' C2' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
C2' C3' H3' 120.0 . . ?
C3' C4' C5' 120.0 . . ?
C3' C4' H4' 120.0 . . ?
C5' C4' H4' 120.0 . . ?
C4' C5' C6' 120.0 . . ?
C4' C5' H5' 120.0 . . ?
C6' C5' H5' 120.0 . . ?
C5' C6' C1' 120.0 . . ?
C5' C6' H6' 120.0 . . ?
C1' C6' H6' 120.0 . . ?

_refine_diff_density_max         0.411
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.051




_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol and water'
_exptl_crystal_preparation       ', Ferroelectric and dielectric'
####################################################################### 
# 
# 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_compound_1_sq
_database_code_depnum_ccdc_archive 'CCDC 1543626'
_audit_update_record             
;
2017-04-12 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C128 H204 N40 Ni4 O74 P8'
_chemical_formula_weight         3969.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_H-M_alt        'I 4 2 2'
_space_group_name_Hall           'I 4 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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   24.810(2)
_cell_length_b                   24.810(2)
_cell_length_c                   17.8094(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10963(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6331
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      19.99

_exptl_crystal_description       block
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_F_000             4152
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.481
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6472
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58599
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.161
_diffrn_reflns_theta_max         28.318
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6848
_reflns_number_gt                3638
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1420P)²] 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_details 
;
 Flack x determined using 1224 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.036(12)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         6848
_refine_ls_number_parameters     218
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.1308
_refine_ls_R_factor_gt           0.0668
_refine_ls_wR_factor_ref         0.2478
_refine_ls_wR_factor_gt          0.1981
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.75679(4) 0.5000 0.0633(4) Uani 1 2 d S T P . .
O2 O 0.5000 0.6731(2) 0.5000 0.0705(14) Uani 1 2 d S T P . .
O3 O 0.5000 0.8411(3) 0.5000 0.0952(19) Uani 1 2 d S T P . .
P1 P 0.36000(10) 0.64059(9) 0.70764(9) 0.0864(6) Uani 1 1 d . . . . .
O1 O 0.3968(2) 0.6073(3) 0.6603(3) 0.1043(16) Uani 1 1 d . . . . .
N1 N 0.3259(3) 0.6845(3) 0.6561(3) 0.0882(17) Uani 1 1 d . . . . .
H1A H 0.2909 0.6859 0.6636 0.106 Uiso 1 1 calc R U . . .
C11 C 0.3458(3) 0.7181(3) 0.6043(4) 0.0772(19) Uani 1 1 d . . . . .
C12 C 0.3998(3) 0.7216(3) 0.5810(4) 0.0699(17) Uani 1 1 d . . . . .
H12 H 0.4252 0.6981 0.6039 0.084 Uiso 1 1 calc R U . . .
N13 N 0.4178(2) 0.7559(2) 0.5287(3) 0.0714(14) Uani 1 1 d . . . . .
C14 C 0.3818(2) 0.7896(2) 0.4970(5) 0.0762(16) Uani 1 1 d . . . . .
H14 H 0.3940 0.8149 0.4608 0.091 Uiso 1 1 calc R U . . .
C15 C 0.3289(3) 0.7884(3) 0.5148(6) 0.091(3) Uani 1 1 d . . . . .
H15 H 0.3049 0.8120 0.4893 0.110 Uiso 1 1 calc R U . . .
C16 C 0.3082(3) 0.7535(3) 0.5700(5) 0.087(2) Uani 1 1 d . . . . .
H16 H 0.2711 0.7537 0.5836 0.104 Uiso 1 1 calc R U . . .
N2 N 0.3120(3) 0.6075(3) 0.7512(4) 0.092(2) Uani 1 1 d . . . . .
H2A H 0.3071 0.6152 0.7989 0.110 Uiso 1 1 calc R U . . .
C21 C 0.2772(3) 0.5673(3) 0.7198(4) 0.0787(19) Uani 1 1 d . . . . .
C22 C 0.2758(3) 0.5565(3) 0.6439(4) 0.0733(18) Uani 1 1 d . . . . .
H22 H 0.3001 0.5750 0.6116 0.088 Uiso 1 1 calc R U . . .
N23 N 0.2415(2) 0.5211(2) 0.6144(3) 0.0695(14) Uani 1 1 d . . . . .
C24 C 0.2068(3) 0.4963(3) 0.6596(4) 0.0744(16) Uani 1 1 d . . . . .
H24 H 0.1815 0.4718 0.6384 0.089 Uiso 1 1 calc R U . . .
C25 C 0.2061(3) 0.5051(4) 0.7379(4) 0.0832(19) Uani 1 1 d . . . . .
H25 H 0.1819 0.4859 0.7693 0.100 Uiso 1 1 calc R U . . .
C26 C 0.2413(3) 0.5422(3) 0.7678(4) 0.0768(19) Uani 1 1 d . . . . .
H26 H 0.2410 0.5503 0.8199 0.092 Uiso 1 1 calc R U . . .
C1 C 0.3999(5) 0.6669(5) 0.7820(7) 0.099(3) Uiso 0.796(7) 1 d D U P A 1
C2 C 0.3825(5) 0.7133(5) 0.8168(7) 0.106(3) Uiso 0.796(7) 1 d D U P A 1
H2 H 0.3512 0.7312 0.7992 0.128 Uiso 0.796(7) 1 calc R U P A 1
C3 C 0.4116(6) 0.7343(6) 0.8795(9) 0.113(3) Uiso 0.796(7) 1 d D U P A 1
H3 H 0.4009 0.7658 0.9059 0.136 Uiso 0.796(7) 1 calc R U P A 1
C4 C 0.4560(6) 0.7049(6) 0.8979(9) 0.124(3) Uiso 0.796(7) 1 d D U P A 1
H4 H 0.4734 0.7159 0.9429 0.149 Uiso 0.796(7) 1 calc R U P A 1
C5 C 0.4791(6) 0.6634(6) 0.8635(7) 0.130(3) Uiso 0.796(7) 1 d D U P A 1
H5 H 0.5140 0.6498 0.8745 0.156 Uiso 0.796(7) 1 calc R U P A 1
C6 C 0.4441(5) 0.6426(5) 0.8082(7) 0.115(3) Uiso 0.796(7) 1 d D U P A 1
H6 H 0.4528 0.6083 0.7878 0.139 Uiso 0.796(7) 1 calc R U P A 1
C1' C 0.3775(18) 0.6897(14) 0.782(2) 0.097(4) Uiso 0.204(7) 1 d D U P A 2
C2' C 0.3594(16) 0.7404(14) 0.787(2) 0.098(5) Uiso 0.204(7) 1 d D U P A 2
H2' H 0.3320 0.7486 0.7517 0.118 Uiso 0.204(7) 1 calc R U P A 2
C3' C 0.3731(18) 0.7845(13) 0.835(2) 0.107(4) Uiso 0.204(7) 1 d D U P A 2
H3' H 0.3641 0.8215 0.8301 0.128 Uiso 0.204(7) 1 calc R U P A 2
C4' C 0.4010(19) 0.7602(17) 0.887(2) 0.111(4) Uiso 0.204(7) 1 d D U P A 2
H4' H 0.3980 0.7777 0.9338 0.133 Uiso 0.204(7) 1 calc R U P A 2
C5' C 0.432(2) 0.7178(18) 0.890(3) 0.114(3) Uiso 0.204(7) 1 d D U P A 2
H5' H 0.4611 0.7133 0.9242 0.137 Uiso 0.204(7) 1 calc R U P A 2
C6' C 0.4171(18) 0.6785(15) 0.833(3) 0.111(3) Uiso 0.204(7) 1 d D U P A 2
H6' H 0.4350 0.6447 0.8313 0.133 Uiso 0.204(7) 1 calc R U P A 2
O4 O 0.4933(8) 0.6041(6) 0.3874(9) 0.144(5) Uiso 0.5 1 d . . P . .
O5 O 0.4197(6) 0.6096(6) 0.4958(14) 0.159(6) Uiso 0.5 1 d . . P . .
O6 O 0.5000 0.5000 0.5000 0.135(6) Uiso 1 8 d S . 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
Ni1 O2 2.075(6) . ?
Ni1 O3 2.091(7) . ?
Ni1 N13 2.103(6) . ?
Ni1 N13 2.103(6) 5_656 ?
Ni1 N23 2.104(5) 8_666 ?
Ni1 N23 2.104(5) 4_565 ?
P1 O1 1.492(6) . ?
P1 N2 1.642(6) . ?
P1 N1 1.656(7) . ?
P1 C1 1.777(12) . ?
P1 C1' 1.86(3) . ?
N1 C11 1.337(10) . ?
N1 H1A 0.8800 . ?
C11 C12 1.405(10) . ?
C11 C16 1.420(11) . ?
C12 N13 1.340(9) . ?
C12 H12 0.9500 . ?
N13 C14 1.346(8) . ?
C14 C15 1.351(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.407(12) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
N2 C21 1.431(9) . ?
N2 H2A 0.8800 . ?
C21 C22 1.379(10) . ?
C21 C26 1.383(9) . ?
C22 N23 1.332(9) . ?
C22 H22 0.9500 . ?
N23 C24 1.331(8) . ?
N23 Ni1 2.104(5) 3_655 ?
C24 C25 1.413(10) . ?
C24 H24 0.9500 . ?
C25 C26 1.375(11) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C1 C6 1.335(14) . ?
C1 C2 1.377(14) . ?
C2 C3 1.427(16) . ?
C2 H2 0.9500 . ?
C3 C4 1.363(15) . ?
C3 H3 0.9500 . ?
C4 C5 1.326(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.410(16) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C1' C2' 1.34(2) . ?
C1' C6' 1.36(2) . ?
C2' C3' 1.42(2) . ?
C2' H2' 0.9500 . ?
C3' C4' 1.30(2) . ?
C3' H3' 0.9500 . ?
C4' C5' 1.31(2) . ?
C4' H4' 0.9500 . ?
C5' C6' 1.45(2) . ?
C5' H5' 0.9500 . ?
C6' H6' 0.9500 . ?
O5 O5 1.04(3) 8_666 ?

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 Ni1 O3 180.0 . . ?
O2 Ni1 N13 89.41(16) . . ?
O3 Ni1 N13 90.59(16) . . ?
O2 Ni1 N13 89.41(16) . 5_656 ?
O3 Ni1 N13 90.59(16) . 5_656 ?
N13 Ni1 N13 178.8(3) . 5_656 ?
O2 Ni1 N23 91.16(15) . 8_666 ?
O3 Ni1 N23 88.84(15) . 8_666 ?
N13 Ni1 N23 89.6(2) . 8_666 ?
N13 Ni1 N23 90.4(2) 5_656 8_666 ?
O2 Ni1 N23 91.16(15) . 4_565 ?
O3 Ni1 N23 88.84(15) . 4_565 ?
N13 Ni1 N23 90.4(2) . 4_565 ?
N13 Ni1 N23 89.6(2) 5_656 4_565 ?
N23 Ni1 N23 177.7(3) 8_666 4_565 ?
O1 P1 N2 115.6(4) . . ?
O1 P1 N1 111.3(3) . . ?
N2 P1 N1 102.7(4) . . ?
O1 P1 C1 106.5(5) . . ?
N2 P1 C1 103.7(5) . . ?
N1 P1 C1 117.1(5) . . ?
O1 P1 C1' 128.8(14) . . ?
N2 P1 C1' 99.2(16) . . ?
N1 P1 C1' 94.9(11) . . ?
C11 N1 P1 127.2(5) . . ?
C11 N1 H1A 116.4 . . ?
P1 N1 H1A 116.4 . . ?
N1 C11 C12 126.4(7) . . ?
N1 C11 C16 116.2(7) . . ?
C12 C11 C16 117.5(7) . . ?
N13 C12 C11 124.2(7) . . ?
N13 C12 H12 117.9 . . ?
C11 C12 H12 117.9 . . ?
C12 N13 C14 117.7(6) . . ?
C12 N13 Ni1 119.9(5) . . ?
C14 N13 Ni1 122.3(5) . . ?
N13 C14 C15 122.2(7) . . ?
N13 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C14 C15 C16 122.1(8) . . ?
C14 C15 H15 118.9 . . ?
C16 C15 H15 118.9 . . ?
C15 C16 C11 116.2(7) . . ?
C15 C16 H16 121.9 . . ?
C11 C16 H16 121.9 . . ?
C21 N2 P1 127.0(5) . . ?
C21 N2 H2A 116.5 . . ?
P1 N2 H2A 116.5 . . ?
C22 C21 C26 120.1(7) . . ?
C22 C21 N2 122.2(7) . . ?
C26 C21 N2 117.5(6) . . ?
N23 C22 C21 122.1(7) . . ?
N23 C22 H22 118.9 . . ?
C21 C22 H22 118.9 . . ?
C24 N23 C22 118.7(6) . . ?
C24 N23 Ni1 118.9(5) . 3_655 ?
C22 N23 Ni1 122.3(5) . 3_655 ?
N23 C24 C25 122.2(7) . . ?
N23 C24 H24 118.9 . . ?
C25 C24 H24 118.9 . . ?
C26 C25 C24 118.6(6) . . ?
C26 C25 H25 120.7 . . ?
C24 C25 H25 120.7 . . ?
C25 C26 C21 118.1(6) . . ?
C25 C26 H26 120.9 . . ?
C21 C26 H26 120.9 . . ?
C6 C1 C2 118.5(12) . . ?
C6 C1 P1 123.6(10) . . ?
C2 C1 P1 117.9(9) . . ?
C1 C2 C3 119.9(11) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 C2 113.7(13) . . ?
C4 C3 H3 123.2 . . ?
C2 C3 H3 123.2 . . ?
C5 C4 C3 130.7(16) . . ?
C5 C4 H4 114.6 . . ?
C3 C4 H4 114.6 . . ?
C4 C5 C6 110.0(14) . . ?
C4 C5 H5 125.0 . . ?
C6 C5 H5 125.0 . . ?
C1 C6 C5 125.8(13) . . ?
C1 C6 H6 117.1 . . ?
C5 C6 H6 117.1 . . ?
C2' C1' C6' 113(3) . . ?
C2' C1' P1 126(3) . . ?
C6' C1' P1 121(2) . . ?
C1' C2' C3' 133(3) . . ?
C1' C2' H2' 113.6 . . ?
C3' C2' H2' 113.6 . . ?
C4' C3' C2' 101(3) . . ?
C4' C3' H3' 129.4 . . ?
C2' C3' H3' 129.4 . . ?
C3' C4' C5' 136(4) . . ?
C3' C4' H4' 112.1 . . ?
C5' C4' H4' 112.1 . . ?
C4' C5' C6' 111(3) . . ?
C4' C5' H5' 124.5 . . ?
C6' C5' H5' 124.5 . . ?
C1' C6' C5' 121(3) . . ?
C1' C6' H6' 119.7 . . ?
C5' C6' H6' 119.7 . . ?

_refine_diff_density_max         0.455
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.063




_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol and water'
_exptl_crystal_preparation       ', Ferroelectric and Dielectric'
####################################################################### 
# 
# 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_compound_Hy-Na_2_sq
_database_code_depnum_ccdc_archive 'CCDC 1543624'
_audit_update_record             
;
2017-04-12 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C128 H202.50 Co4 N40.25 Na0.25 O74 P8'
_chemical_formula_weight         3978.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_H-M_alt        'I 4 2 2'
_space_group_name_Hall           'I 4 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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   24.524(12)
_cell_length_b                   24.524(12)
_cell_length_c                   17.661(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10622(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1153
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      16.84

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_F_000             4150
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.455
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5461
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26907
_diffrn_reflns_av_unetI/netI     0.1372
_diffrn_reflns_av_R_equivalents  0.2054
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.186
_diffrn_reflns_theta_max         25.014
_diffrn_reflns_theta_full        25.014
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4705
_reflns_number_gt                1996
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
'Refined as a 2-component inversion twin., SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1747P)²] 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_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.38(10)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         4705
_refine_ls_number_parameters     172
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.2055
_refine_ls_R_factor_gt           0.0879
_refine_ls_wR_factor_ref         0.3072
_refine_ls_wR_factor_gt          0.2355
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_restrained_S_all      0.944
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.76077(9) 0.5000 0.5000 0.0668(8) Uani 1 2 d S T P . .
O2 O 0.6749(4) 0.5000 0.5000 0.075(3) Uani 1 2 d S T P . .
O3 O 0.8447(5) 0.5000 0.5000 0.100(4) Uani 1 2 d S T P . .
O4 O 0.6035(7) 0.4982(11) 0.3864(9) 0.085(5) Uiso 0.5 1 d . . P . .
O5 O 0.6076(13) 0.5774(13) 0.501(3) 0.084(10) Uiso 0.25 1 d . . P . .
O7 O 0.5000 0.5000 0.441(3) 0.095(16) Uiso 0.125 4 d S . P . .
Na1 Na 0.5000 0.5000 0.441(3) 0.095(16) Uiso 0.125 4 d S . P . .
P1 P 0.6393(2) 0.35928(18) 0.71139(18) 0.0791(11) Uani 1 1 d . . . . .
O1 O 0.6049(4) 0.3909(5) 0.6616(6) 0.104(3) Uani 1 1 d . . . . .
N1 N 0.6875(6) 0.3932(5) 0.7537(7) 0.088(4) Uani 1 1 d . . . . .
H1A H 0.6911 0.3867 0.8024 0.106 Uiso 1 1 calc R U . . .
C11 C 0.7235(4) 0.4307(4) 0.7242(5) 0.075(4) Uani 1 1 d G . . . .
C12 C 0.7247(3) 0.4406(3) 0.6467(4) 0.082(5) Uani 1 1 d G . . . .
H12 H 0.7000 0.4221 0.6141 0.099 Uiso 1 1 calc R U . . .
N13 N 0.7621(3) 0.4774(3) 0.6169(3) 0.073(3) Uani 1 1 d G . . . .
C14 C 0.7982(3) 0.5044(4) 0.6645(5) 0.070(3) Uani 1 1 d G . . . .
H14 H 0.8237 0.5295 0.6442 0.084 Uiso 1 1 calc R U . . .
C15 C 0.7970(3) 0.4946(4) 0.7420(4) 0.112(6) Uani 1 1 d G . . . .
H15 H 0.8217 0.5130 0.7746 0.135 Uiso 1 1 calc R U . . .
C16 C 0.7596(4) 0.4577(5) 0.7718(3) 0.081(4) Uani 1 1 d G . . . .
H16 H 0.7588 0.4510 0.8248 0.097 Uiso 1 1 calc R U . . .
N2 N 0.6738(6) 0.3115(6) 0.6637(6) 0.091(4) Uani 1 1 d . . . . .
H2A H 0.7081 0.3073 0.6767 0.109 Uiso 1 1 calc R U . . .
C21 C 0.6559(4) 0.2787(4) 0.6082(4) 0.060(3) Uani 1 1 d G . . . .
C22 C 0.6014(3) 0.2777(3) 0.5867(4) 0.068(4) Uani 1 1 d G . . . .
H22 H 0.5760 0.3015 0.6103 0.082 Uiso 1 1 calc R U . . .
N23 N 0.5841(2) 0.2419(3) 0.5307(4) 0.069(3) Uani 1 1 d G . . . .
C24 C 0.6212(3) 0.2071(3) 0.4961(5) 0.079(4) Uani 1 1 d G . . . .
H24 H 0.6094 0.1826 0.4578 0.094 Uiso 1 1 calc R U . . .
C25 C 0.6757(3) 0.2080(4) 0.5177(6) 0.093(5) Uani 1 1 d G . . . .
H25 H 0.7011 0.1842 0.4941 0.111 Uiso 1 1 calc R U . . .
C26 C 0.6931(3) 0.2438(4) 0.5737(5) 0.074(4) Uani 1 1 d G . . . .
H26 H 0.7304 0.2445 0.5884 0.088 Uiso 1 1 calc R U . . .
C1 C 0.5937(10) 0.3372(10) 0.7798(11) 0.077(9) Uiso 0.51(3) 1 d G U P A 1
C2 C 0.5471(10) 0.3654(8) 0.8014(13) 0.116(12) Uiso 0.51(3) 1 d G U P A 1
H2 H 0.5365 0.3974 0.7747 0.139 Uiso 0.51(3) 1 calc R U P A 1
C3 C 0.5159(9) 0.3469(9) 0.8619(13) 0.099(11) Uiso 0.51(3) 1 d G U P A 1
H3 H 0.4840 0.3662 0.8766 0.119 Uiso 0.51(3) 1 calc R U P A 1
C4 C 0.5314(9) 0.3001(10) 0.9008(11) 0.097(10) Uiso 0.51(3) 1 d G U P A 1
H4 H 0.5101 0.2875 0.9422 0.117 Uiso 0.51(3) 1 calc R U P A 1
C5 C 0.5780(9) 0.2719(9) 0.8793(11) 0.079(8) Uiso 0.51(3) 1 d G U P A 1
H5 H 0.5886 0.2399 0.9059 0.095 Uiso 0.51(3) 1 calc R U P A 1
C6 C 0.6092(8) 0.2904(9) 0.8188(11) 0.072(8) Uiso 0.51(3) 1 d G U P A 1
H6 H 0.6411 0.2711 0.8041 0.087 Uiso 0.51(3) 1 calc R U P A 1
C1' C 0.6097(11) 0.3204(10) 0.7881(12) 0.077(9) Uiso 0.49(3) 1 d G U P A 2
C2' C 0.5685(11) 0.3477(8) 0.8264(14) 0.104(11) Uiso 0.49(3) 1 d G U P A 2
H2' H 0.5573 0.3829 0.8100 0.125 Uiso 0.49(3) 1 calc R U P A 2
C3' C 0.5436(9) 0.3237(10) 0.8887(13) 0.095(10) Uiso 0.49(3) 1 d G U P A 2
H3' H 0.5154 0.3424 0.9148 0.114 Uiso 0.49(3) 1 calc R U P A 2
C4' C 0.5599(10) 0.2723(10) 0.9127(11) 0.089(10) Uiso 0.49(3) 1 d G U P A 2
H4' H 0.5429 0.2558 0.9553 0.107 Uiso 0.49(3) 1 calc R U P A 2
C5' C 0.6012(9) 0.2449(9) 0.8744(12) 0.079(9) Uiso 0.49(3) 1 d G U P A 2
H5' H 0.6123 0.2097 0.8908 0.095 Uiso 0.49(3) 1 calc R U P A 2
C6' C 0.6261(9) 0.2689(10) 0.8121(12) 0.077(9) Uiso 0.49(3) 1 d G U P A 2
H6' H 0.6543 0.2502 0.7859 0.093 Uiso 0.49(3) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O3 2.059(13) . ?
Co1 O2 2.106(11) . ?
Co1 N23 2.13(3) 8_666 ?
Co1 N23 2.13(4) 3_655 ?
Co1 N13 2.137(6) 6_566 ?
Co1 N13 2.137(6) . ?
O5 O5 1.05(6) 7_556 ?
O7 Na1 2.10(11) 5_656 ?
P1 O1 1.445(11) . ?
P1 N1 1.627(13) . ?
P1 N2 1.672(13) . ?
P1 C1 1.734(15) . ?
P1 C1' 1.809(16) . ?
N1 C11 1.377(13) . ?
N1 H1A 0.8800 . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C12 N13 1.3900 . ?
C12 H12 0.9500 . ?
N13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C14 H14 0.9500 . ?
C15 C16 1.3900 . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
N2 C21 1.341(14) . ?
N2 H2A 0.8800 . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C22 N23 1.3900 . ?
C22 H22 0.9500 . ?
N23 C24 1.3900 . ?
N23 Co1 2.133(6) 4_565 ?
C24 C25 1.3900 . ?
C24 H24 0.9500 . ?
C25 C26 1.3900 . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C2 C3 1.3900 . ?
C2 H2 0.9500 . ?
C3 C4 1.3900 . ?
C3 H3 0.9500 . ?
C4 C5 1.3900 . ?
C4 H4 0.9500 . ?
C5 C6 1.3900 . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C1' C2' 1.3900 . ?
C1' C6' 1.3900 . ?
C2' C3' 1.3900 . ?
C2' H2' 0.9500 . ?
C3' C4' 1.3900 . ?
C3' H3' 0.9500 . ?
C4' C5' 1.3900 . ?
C4' H4' 0.9500 . ?
C5' C6' 1.3900 . ?
C5' H5' 0.9500 . ?
C6' H6' 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Co1 O2 180.0 . . ?
O3 Co1 N23 91.8(5) . 8_666 ?
O2 Co1 N23 88.2(5) . 8_666 ?
O3 Co1 N23 91.8(5) . 3_655 ?
O2 Co1 N23 88.2(5) . 3_655 ?
N23 Co1 N23 176.5(10) 8_666 3_655 ?
O3 Co1 N13 89.1(8) . 6_566 ?
O2 Co1 N13 90.9(8) . 6_566 ?
N23 Co1 N13 90.3(11) 8_666 6_566 ?
N23 Co1 N13 89.7(15) 3_655 6_566 ?
O3 Co1 N13 89.1(2) . . ?
O2 Co1 N13 90.9(2) . . ?
N23 Co1 N13 89.7(7) 8_666 . ?
N23 Co1 N13 90.3(13) 3_655 . ?
N13 Co1 N13 178.3(10) 6_566 . ?
O1 P1 N1 115.5(8) . . ?
O1 P1 N2 111.4(5) . . ?
N1 P1 N2 102.9(8) . . ?
O1 P1 C1 102.4(10) . . ?
N1 P1 C1 108.0(9) . . ?
N2 P1 C1 117.2(10) . . ?
O1 P1 C1' 120.3(11) . . ?
N1 P1 C1' 102.6(10) . . ?
N2 P1 C1' 102.1(9) . . ?
C11 N1 P1 129.3(9) . . ?
C11 N1 H1A 115.4 . . ?
P1 N1 H1A 115.4 . . ?
N1 C11 C12 120.2(8) . . ?
N1 C11 C16 119.8(8) . . ?
C12 C11 C16 120.0 . . ?
N13 C12 C11 120.0 . . ?
N13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C14 N13 C12 120.0 . . ?
C14 N13 Co1 118.1(4) . . ?
C12 N13 Co1 121.6(4) . . ?
N13 C14 C15 120.0 . . ?
N13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C11 120.0 . . ?
C15 C16 H16 120.0 . . ?
C11 C16 H16 120.0 . . ?
C21 N2 P1 128.6(11) . . ?
C21 N2 H2A 115.7 . . ?
P1 N2 H2A 115.7 . . ?
N2 C21 C22 121.6(9) . . ?
N2 C21 C26 118.4(9) . . ?
C22 C21 C26 120.0 . . ?
C21 C22 N23 120.0 . . ?
C21 C22 H22 120.0 . . ?
N23 C22 H22 120.0 . . ?
C24 N23 C22 120.0 . . ?
C24 N23 Co1 120.2(4) . 4_565 ?
C22 N23 Co1 119.8(4) . 4_565 ?
N23 C24 C25 120.0 . . ?
N23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C26 C25 C24 120.0 . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C21 120.0 . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
C2 C1 C6 120.0 . . ?
C2 C1 P1 124.5(13) . . ?
C6 C1 P1 115.3(13) . . ?
C3 C2 C1 120.0 . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 120.0 . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
C2' C1' C6' 120.0 . . ?
C2' C1' P1 113.6(13) . . ?
C6' C1' P1 126.3(13) . . ?
C3' C2' C1' 120.0 . . ?
C3' C2' H2' 120.0 . . ?
C1' C2' H2' 120.0 . . ?
C2' C3' C4' 120.0 . . ?
C2' C3' H3' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
C5' C4' C3' 120.0 . . ?
C5' C4' H4' 120.0 . . ?
C3' C4' H4' 120.0 . . ?
C4' C5' C6' 120.0 . . ?
C4' C5' H5' 120.0 . . ?
C6' C5' H5' 120.0 . . ?
C5' C6' C1' 120.0 . . ?
C5' C6' H6' 120.0 . . ?
C1' C6' H6' 120.0 . . ?

_refine_diff_density_max         0.781
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.081




_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol and water'
_exptl_crystal_preparation       ', Ferroelectric and dielectric'
####################################################################### 
# 
# 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_compound_Hy-K_1_sq
_database_code_depnum_ccdc_archive 'CCDC 1543631'
_audit_update_record             
;
2017-04-12 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C128 H186 K N41 Ni4 O68 P8'
_chemical_formula_weight         3908.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_H-M_alt        'I 4 2 2'
_space_group_name_Hall           'I 4 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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   24.382(2)
_cell_length_b                   24.382(2)
_cell_length_c                   17.522(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10417(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9949
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      22.35

_exptl_crystal_description       block
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_F_000             4072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    0.522
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6412
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            65236
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.181
_diffrn_reflns_theta_max         28.365
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6531
_reflns_number_gt                4197
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0807P)²+5.1754P] 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_details 
;
 Flack x determined using 1500 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(10)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         6531
_refine_ls_number_parameters     224
_refine_ls_number_restraints     64
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1602
_refine_ls_wR_factor_gt          0.1333
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.76211(3) 0.5000 0.0542(2) Uani 1 2 d S T P . .
O2 O 0.5000 0.67700(14) 0.5000 0.0549(8) Uani 1 2 d S T P . .
O3 O 0.5000 0.84872(16) 0.5000 0.0821(13) Uani 1 2 d S T P . .
K1 K 0.5000 0.5000 0.5000 0.0785(8) Uani 1 8 d S T P . .
O4 O 0.4993(3) 0.59937(19) 0.3946(3) 0.0670(10) Uiso 0.675(4) 1 d . U P . .
O4' O 0.500(3) 0.5712(17) 0.352(2) 0.0670(10) Uiso 0.074(3) 1 d . U P . .
O5 O 0.5741(5) 0.6030(5) 0.5015(11) 0.0670(10) Uiso 0.251(3) 1 d . U P . .
P1 P 0.64008(6) 0.64127(6) 0.29098(7) 0.0653(3) Uani 1 1 d . . . . .
O1 O 0.60441(16) 0.60976(15) 0.34284(18) 0.0697(8) Uani 1 1 d . . . . .
N1 N 0.67573(19) 0.6879(2) 0.3376(2) 0.0729(12) Uani 1 1 d . . . . .
H1A H 0.7107 0.6904 0.3259 0.088 Uiso 1 1 calc R U . . .
C11 C 0.6566(2) 0.72394(19) 0.3937(3) 0.0619(12) Uani 1 1 d . . . . .
C12 C 0.60228(19) 0.72626(18) 0.4150(3) 0.0571(11) Uani 1 1 d . . . . .
H12 H 0.5768 0.7030 0.3900 0.068 Uiso 1 1 calc R U . . .
N13 N 0.58376(16) 0.76037(16) 0.4702(2) 0.0594(10) Uani 1 1 d . . . . .
C14 C 0.61963(18) 0.79421(18) 0.5006(5) 0.0692(11) Uani 1 1 d . . . . .
H14 H 0.6067 0.8204 0.5366 0.083 Uiso 1 1 calc R U . . .
C15 C 0.6745(2) 0.7941(2) 0.4837(4) 0.0739(16) Uani 1 1 d . . . . .
H15 H 0.6990 0.8176 0.5104 0.089 Uiso 1 1 calc R U . . .
C16 C 0.6935(2) 0.7597(2) 0.4279(3) 0.0707(13) Uani 1 1 d . . . . .
H16 H 0.7309 0.7603 0.4128 0.085 Uiso 1 1 calc R U . . .
N2 N 0.6865(2) 0.60572(19) 0.2459(3) 0.0770(13) Uani 1 1 d . . . . .
H2A H 0.6874 0.6095 0.1960 0.092 Uiso 1 1 calc R U . . .
C21 C 0.7256(2) 0.5695(2) 0.2776(3) 0.0629(12) Uani 1 1 d . . . . .
C22 C 0.72722(19) 0.55739(19) 0.3544(3) 0.0576(11) Uani 1 1 d . . . . .
H22 H 0.7020 0.5752 0.3875 0.069 Uiso 1 1 calc R U . . .
N23 N 0.76330(14) 0.52117(15) 0.3848(2) 0.0571(9) Uani 1 1 d . . . . .
C24 C 0.79858(18) 0.4965(3) 0.3369(3) 0.0674(12) Uani 1 1 d . . . . .
H24 H 0.8242 0.4709 0.3570 0.081 Uiso 1 1 calc R U . . .
C25 C 0.7989(2) 0.5071(3) 0.2596(3) 0.0813(16) Uani 1 1 d . . . . .
H25 H 0.8240 0.4885 0.2272 0.098 Uiso 1 1 calc R U . . .
C26 C 0.7632(2) 0.5442(2) 0.2299(3) 0.0712(14) Uani 1 1 d . . . . .
H26 H 0.7640 0.5528 0.1770 0.085 Uiso 1 1 calc R U . . .
C1 C 0.5956(5) 0.6659(4) 0.2166(6) 0.067(2) Uiso 0.558(11) 1 d D U P A 1
C2 C 0.6129(5) 0.7142(5) 0.1798(6) 0.074(3) Uiso 0.558(11) 1 d D U P A 1
H2 H 0.6453 0.7323 0.1962 0.089 Uiso 0.558(11) 1 calc R U P A 1
C3 C 0.5818(6) 0.7361(6) 0.1176(8) 0.092(3) Uiso 0.558(11) 1 d D U P A 1
H3 H 0.5906 0.7694 0.0922 0.111 Uiso 0.558(11) 1 calc R U P A 1
C4 C 0.5374(5) 0.7035(6) 0.0986(8) 0.093(3) Uiso 0.558(11) 1 d D U P A 1
H4 H 0.5179 0.7153 0.0546 0.112 Uiso 0.558(11) 1 calc R U P A 1
C5 C 0.5163(6) 0.6560(6) 0.1329(8) 0.105(4) Uiso 0.558(11) 1 d D U P A 1
H5 H 0.4837 0.6385 0.1163 0.127 Uiso 0.558(11) 1 calc R U P A 1
C6 C 0.5490(6) 0.6362(6) 0.1960(7) 0.096(3) Uiso 0.558(11) 1 d D U P A 1
H6 H 0.5389 0.6039 0.2228 0.115 Uiso 0.558(11) 1 calc R U P A 1
C1' C 0.6101(6) 0.6818(6) 0.2147(8) 0.066(3) Uiso 0.442(11) 1 d D U P A 2
C2' C 0.6273(7) 0.7335(7) 0.1917(8) 0.082(4) Uiso 0.442(11) 1 d D U P A 2
H2' H 0.6557 0.7518 0.2187 0.099 Uiso 0.442(11) 1 calc R U P A 2
C3' C 0.6019(7) 0.7592(7) 0.1269(9) 0.091(4) Uiso 0.442(11) 1 d D U P A 2
H3' H 0.6137 0.7934 0.1068 0.110 Uiso 0.442(11) 1 calc R U P A 2
C4' C 0.5577(8) 0.7288(7) 0.0957(11) 0.105(5) Uiso 0.442(11) 1 d D U P A 2
H4' H 0.5387 0.7468 0.0555 0.126 Uiso 0.442(11) 1 calc R U P A 2
C5' C 0.5375(8) 0.6775(8) 0.1137(10) 0.099(4) Uiso 0.442(11) 1 d D U P A 2
H5' H 0.5086 0.6594 0.0875 0.119 Uiso 0.442(11) 1 calc R U P A 2
C6' C 0.5674(7) 0.6551(7) 0.1787(9) 0.088(3) Uiso 0.442(11) 1 d D U P A 2
H6' H 0.5568 0.6201 0.1975 0.106 Uiso 0.442(11) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 2.075(3) . ?
Ni1 N23 2.084(4) 7_556 ?
Ni1 N23 2.084(4) 3_655 ?
Ni1 N13 2.108(4) 5_656 ?
Ni1 N13 2.109(4) . ?
Ni1 O3 2.112(4) . ?
K1 O4 3.046(4) 7_556 ?
K1 O4 3.046(4) 5_656 ?
K1 O4 3.046(4) 3_655 ?
K1 O4 3.046(4) 2_665 ?
K1 O4 3.046(4) 8_666 ?
K1 O4 3.046(4) 6_566 ?
K1 O4 3.046(4) 4_565 ?
K1 O4 3.046(4) . ?
K1 O5 3.093(12) 8_666 ?
K1 O5 3.093(12) 7_556 ?
K1 O5 3.093(12) 2_665 ?
K1 O5 3.093(12) 6_566 ?
O4 O4' 1.01(4) . ?
O5 O5 1.00(2) 7_556 ?
P1 O1 1.474(3) . ?
P1 N2 1.630(5) . ?
P1 N1 1.647(4) . ?
P1 C1 1.799(10) . ?
P1 C1' 1.816(13) . ?
N1 C11 1.400(7) . ?
N1 H1A 0.8800 . ?
C11 C12 1.376(7) . ?
C11 C16 1.388(8) . ?
C12 N13 1.353(6) . ?
C12 H12 0.9500 . ?
N13 C14 1.315(6) . ?
C14 C15 1.370(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.370(8) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
N2 C21 1.413(7) . ?
N2 H2A 0.8800 . ?
C21 C22 1.378(7) . ?
C21 C26 1.385(7) . ?
C22 N23 1.355(6) . ?
C22 H22 0.9500 . ?
N23 C24 1.344(6) . ?
N23 Ni1 2.084(4) 4_565 ?
C24 C25 1.379(8) . ?
C24 H24 0.9500 . ?
C25 C26 1.360(8) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C1 C6 1.395(14) . ?
C1 C2 1.408(13) . ?
C2 C3 1.430(14) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(16) . ?
C3 H3 0.9500 . ?
C4 C5 1.403(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.445(14) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C1' C6' 1.381(16) . ?
C1' C2' 1.388(15) . ?
C2' C3' 1.437(16) . ?
C2' H2' 0.9500 . ?
C3' C4' 1.419(18) . ?
C3' H3' 0.9500 . ?
C4' C5' 1.381(18) . ?
C4' H4' 0.9500 . ?
C5' C6' 1.458(17) . ?
C5' H5' 0.9500 . ?
C6' H6' 0.9500 . ?

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 Ni1 N23 90.80(10) . 7_556 ?
O2 Ni1 N23 90.80(10) . 3_655 ?
N23 Ni1 N23 178.40(19) 7_556 3_655 ?
O2 Ni1 N13 88.85(11) . 5_656 ?
N23 Ni1 N13 90.01(15) 7_556 5_656 ?
N23 Ni1 N13 90.02(15) 3_655 5_656 ?
O2 Ni1 N13 88.85(11) . . ?
N23 Ni1 N13 90.02(15) 7_556 . ?
N23 Ni1 N13 90.01(15) 3_655 . ?
N13 Ni1 N13 177.7(2) 5_656 . ?
O2 Ni1 O3 180.0 . . ?
N23 Ni1 O3 89.20(10) 7_556 . ?
N23 Ni1 O3 89.20(10) 3_655 . ?
N13 Ni1 O3 91.15(11) 5_656 . ?
N13 Ni1 O3 91.15(11) . . ?
O4 K1 O4 68.44(9) 7_556 5_656 ?
O4 K1 O4 179.3(3) 7_556 3_655 ?
O4 K1 O4 112.1(2) 5_656 3_655 ?
O4 K1 O4 111.0(2) 7_556 2_665 ?
O4 K1 O4 179.3(3) 5_656 2_665 ?
O4 K1 O4 68.44(9) 3_655 2_665 ?
O4 K1 O4 105.37(18) 7_556 8_666 ?
O4 K1 O4 68.44(9) 5_656 8_666 ?
O4 K1 O4 74.63(18) 3_655 8_666 ?
O4 K1 O4 112.1(2) 2_665 8_666 ?
O4 K1 O4 68.44(9) 7_556 6_566 ?
O4 K1 O4 105.37(18) 5_656 6_566 ?
O4 K1 O4 111.0(2) 3_655 6_566 ?
O4 K1 O4 74.63(18) 2_665 6_566 ?
O4 K1 O4 68.44(9) 8_666 6_566 ?
O4 K1 O4 74.63(18) 7_556 4_565 ?
O4 K1 O4 111.0(2) 5_656 4_565 ?
O4 K1 O4 105.37(18) 3_655 4_565 ?
O4 K1 O4 68.44(9) 2_665 4_565 ?
O4 K1 O4 179.3(3) 8_666 4_565 ?
O4 K1 O4 112.1(2) 6_566 4_565 ?
O4 K1 O4 112.1(2) 7_556 . ?
O4 K1 O4 74.63(18) 5_656 . ?
O4 K1 O4 68.44(9) 3_655 . ?
O4 K1 O4 105.37(18) 2_665 . ?
O4 K1 O4 111.0(2) 8_666 . ?
O4 K1 O4 179.3(3) 6_566 . ?
O4 K1 O4 68.44(9) 4_565 . ?
O4 K1 O5 130.3(3) 7_556 8_666 ?
O4 K1 O5 118.3(3) 5_656 8_666 ?
O4 K1 O5 49.1(3) 3_655 8_666 ?
O4 K1 O5 62.3(3) 2_665 8_666 ?
O4 K1 O5 50.4(3) 8_666 8_666 ?
O4 K1 O5 62.4(3) 6_566 8_666 ?
O4 K1 O5 130.1(3) 4_565 8_666 ?
O4 K1 O5 117.0(3) . 8_666 ?
O4 K1 O5 50.4(3) 7_556 7_556 ?
O4 K1 O5 62.4(3) 5_656 7_556 ?
O4 K1 O5 130.1(3) 3_655 7_556 ?
O4 K1 O5 117.0(3) 2_665 7_556 ?
O4 K1 O5 130.3(3) 8_666 7_556 ?
O4 K1 O5 118.3(3) 6_566 7_556 ?
O4 K1 O5 49.1(3) 4_565 7_556 ?
O4 K1 O5 62.3(3) . 7_556 ?
O5 K1 O5 179.0(7) 8_666 7_556 ?
O4 K1 O5 117.0(3) 7_556 2_665 ?
O4 K1 O5 130.1(3) 5_656 2_665 ?
O4 K1 O5 62.4(3) 3_655 2_665 ?
O4 K1 O5 50.4(3) 2_665 2_665 ?
O4 K1 O5 62.3(3) 8_666 2_665 ?
O4 K1 O5 49.1(3) 6_566 2_665 ?
O4 K1 O5 118.3(3) 4_565 2_665 ?
O4 K1 O5 130.4(3) . 2_665 ?
O5 K1 O5 18.6(4) 8_666 2_665 ?
O5 K1 O5 161.5(4) 7_556 2_665 ?
O4 K1 O5 62.4(3) 7_556 6_566 ?
O4 K1 O5 130.3(3) 5_656 6_566 ?
O4 K1 O5 117.0(3) 3_655 6_566 ?
O4 K1 O5 49.1(3) 2_665 6_566 ?
O4 K1 O5 118.3(3) 8_666 6_566 ?
O4 K1 O5 50.4(3) 6_566 6_566 ?
O4 K1 O5 62.3(3) 4_565 6_566 ?
O4 K1 O5 130.1(3) . 6_566 ?
O5 K1 O5 89.996(8) 8_666 6_566 ?
O5 K1 O5 89.996(9) 7_556 6_566 ?
O5 K1 O5 71.5(4) 2_665 6_566 ?
O4' O4 K1 85(2) . . ?
O4 O4' K1 76(2) . . ?
O5 O5 K1 80.7(2) 7_556 . ?
O1 P1 N2 115.6(3) . . ?
O1 P1 N1 111.43(19) . . ?
N2 P1 N1 103.9(3) . . ?
O1 P1 C1 105.4(4) . . ?
N2 P1 C1 104.2(4) . . ?
N1 P1 C1 116.6(4) . . ?
O1 P1 C1' 120.0(5) . . ?
N2 P1 C1' 102.3(5) . . ?
N1 P1 C1' 101.6(5) . . ?
C11 N1 P1 127.3(4) . . ?
C11 N1 H1A 116.4 . . ?
P1 N1 H1A 116.4 . . ?
C12 C11 C16 118.7(5) . . ?
C12 C11 N1 122.5(5) . . ?
C16 C11 N1 118.7(5) . . ?
N13 C12 C11 122.7(4) . . ?
N13 C12 H12 118.7 . . ?
C11 C12 H12 118.7 . . ?
C14 N13 C12 117.0(4) . . ?
C14 N13 Ni1 122.1(4) . . ?
C12 N13 Ni1 120.8(3) . . ?
N13 C14 C15 124.1(5) . . ?
N13 C14 H14 118.0 . . ?
C15 C14 H14 118.0 . . ?
C16 C15 C14 119.0(5) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C11 118.3(5) . . ?
C15 C16 H16 120.9 . . ?
C11 C16 H16 120.9 . . ?
C21 N2 P1 127.6(4) . . ?
C21 N2 H2A 116.2 . . ?
P1 N2 H2A 116.2 . . ?
C22 C21 C26 118.4(5) . . ?
C22 C21 N2 122.5(4) . . ?
C26 C21 N2 119.1(5) . . ?
N23 C22 C21 122.8(4) . . ?
N23 C22 H22 118.6 . . ?
C21 C22 H22 118.6 . . ?
C24 N23 C22 117.5(5) . . ?
C24 N23 Ni1 120.2(4) . 4_565 ?
C22 N23 Ni1 122.2(3) . 4_565 ?
N23 C24 C25 122.2(6) . . ?
N23 C24 H24 118.9 . . ?
C25 C24 H24 118.9 . . ?
C26 C25 C24 119.8(5) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C21 119.2(5) . . ?
C25 C26 H26 120.4 . . ?
C21 C26 H26 120.4 . . ?
C6 C1 C2 124.0(11) . . ?
C6 C1 P1 120.4(8) . . ?
C2 C1 P1 115.5(8) . . ?
C1 C2 C3 120.2(11) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C4 C3 C2 112.6(12) . . ?
C4 C3 H3 123.7 . . ?
C2 C3 H3 123.7 . . ?
C3 C4 C5 131.1(13) . . ?
C3 C4 H4 114.5 . . ?
C5 C4 H4 114.5 . . ?
C4 C5 C6 113.7(13) . . ?
C4 C5 H5 123.1 . . ?
C6 C5 H5 123.1 . . ?
C1 C6 C5 118.3(13) . . ?
C1 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
C6' C1' C2' 121.6(13) . . ?
C6' C1' P1 112.5(10) . . ?
C2' C1' P1 125.9(10) . . ?
C1' C2' C3' 119.7(14) . . ?
C1' C2' H2' 120.2 . . ?
C3' C2' H2' 120.2 . . ?
C4' C3' C2' 113.9(15) . . ?
C4' C3' H3' 123.1 . . ?
C2' C3' H3' 123.1 . . ?
C5' C4' C3' 131.0(17) . . ?
C5' C4' H4' 114.5 . . ?
C3' C4' H4' 114.5 . . ?
C4' C5' C6' 109.9(16) . . ?
C4' C5' H5' 125.1 . . ?
C6' C5' H5' 125.1 . . ?
C1' C6' C5' 123.9(15) . . ?
C1' C6' H6' 118.1 . . ?
C5' C6' H6' 118.1 . . ?

_refine_diff_density_max         0.747
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.051




_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol and water'
_exptl_crystal_preparation       ', Ferroelectric and Dielectric'
####################################################################### 
# 
# 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_compound_Hy-Rb_1_sq
_database_code_depnum_ccdc_archive 'CCDC 1543630'
_audit_update_record             
;
2017-04-12 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C128 H194 N41 Ni4 O72 P8 Rb'
_chemical_formula_weight         4027.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_H-M_alt        'I 4 2 2'
_space_group_name_Hall           'I 4 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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   24.570(8)
_cell_length_b                   24.570(8)
_cell_length_c                   17.699(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10685(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2500
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      16.81

_exptl_crystal_description       block
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_F_000             4188
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.719
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6752
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            53218
_diffrn_reflns_av_unetI/netI     0.1463
_diffrn_reflns_av_R_equivalents  0.1900
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.418
_diffrn_reflns_theta_max         28.304
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6634
_reflns_number_gt                2803
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0873P)²] 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_details 
;
 Flack x determined using 851 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(15)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         6634
_refine_ls_number_parameters     224
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.1893
_refine_ls_R_factor_gt           0.0618
_refine_ls_wR_factor_ref         0.1943
_refine_ls_wR_factor_gt          0.1452
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_restrained_S_all      0.963
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.76202(4) 0.5000 0.5000 0.0553(4) Uani 1 2 d S T P . .
O2 O 0.6776(2) 0.5000 0.5000 0.0529(15) Uani 1 2 d S T P . .
O3 O 0.8478(3) 0.5000 0.5000 0.085(2) Uani 1 2 d S T P . .
Rb1 Rb 0.5000 0.5000 0.5000 0.0572(5) Uani 1 8 d S T P . .
O4 O 0.6019(3) 0.5005(5) 0.6114(4) 0.0581(16) Uiso 0.623(4) 1 d . U P . .
O4' O 0.5759(10) 0.4975(14) 0.6522(14) 0.0581(16) Uiso 0.191(4) 1 d . U P . .
O5 O 0.5811(5) 0.3925(5) 0.4987(14) 0.0581(16) Uiso 0.311(4) 1 d . U P . .
P1 P 0.64108(10) 0.35818(10) 0.29197(10) 0.0638(5) Uani 1 1 d . . . . .
O1 O 0.6055(2) 0.3903(2) 0.3439(3) 0.0627(13) Uani 1 1 d . . . . .
N1 N 0.6883(3) 0.3933(3) 0.2483(4) 0.078(2) Uani 1 1 d . . . . .
H1A H 0.6903 0.3879 0.1992 0.093 Uiso 1 1 calc R U . . .
C11 C 0.7257(3) 0.4304(3) 0.2775(5) 0.061(2) Uani 1 1 d . . . . .
C12 C 0.7275(3) 0.4425(3) 0.3554(5) 0.057(2) Uani 1 1 d . . . . .
H12 H 0.7028 0.4245 0.3884 0.068 Uiso 1 1 calc R U . . .
N13 N 0.7626(3) 0.4783(3) 0.3842(4) 0.0603(18) Uani 1 1 d . . . . .
C14 C 0.7983(3) 0.5034(5) 0.3362(5) 0.067(2) Uani 1 1 d . . . . .
H14 H 0.8228 0.5297 0.3557 0.080 Uiso 1 1 calc R U . . .
C15 C 0.7996(3) 0.4915(4) 0.2608(5) 0.074(3) Uani 1 1 d . . . . .
H15 H 0.8261 0.5080 0.2293 0.089 Uiso 1 1 calc R U . . .
C16 C 0.7625(3) 0.4558(3) 0.2307(5) 0.067(2) Uani 1 1 d . . . . .
H16 H 0.7623 0.4487 0.1780 0.081 Uiso 1 1 calc R U . . .
N2 N 0.6752(3) 0.3121(3) 0.3400(4) 0.072(2) Uani 1 1 d . . . . .
H2A H 0.7102 0.3104 0.3295 0.087 Uiso 1 1 calc R U . . .
C21 C 0.6570(3) 0.2747(3) 0.3960(5) 0.059(2) Uani 1 1 d . . . . .
C22 C 0.6020(3) 0.2741(3) 0.4162(5) 0.058(2) Uani 1 1 d . . . . .
H22 H 0.5774 0.2986 0.3925 0.070 Uiso 1 1 calc R U . . .
N23 N 0.5832(3) 0.2386(3) 0.4701(4) 0.0600(18) Uani 1 1 d . . . . .
C24 C 0.6194(3) 0.2053(3) 0.5026(7) 0.070(2) Uani 1 1 d . . . . .
H24 H 0.6069 0.1805 0.5398 0.084 Uiso 1 1 calc R U . . .
C25 C 0.6746(4) 0.2054(4) 0.4842(6) 0.080(3) Uani 1 1 d . . . . .
H25 H 0.6992 0.1813 0.5088 0.096 Uiso 1 1 calc R U . . .
C26 C 0.6927(4) 0.2406(4) 0.4306(5) 0.069(2) Uani 1 1 d . . . . .
H26 H 0.7302 0.2414 0.4174 0.083 Uiso 1 1 calc R U . . .
C1 C 0.5974(7) 0.3336(7) 0.2180(10) 0.069(4) Uiso 0.555(16) 1 d D U P A 1
C2 C 0.5502(8) 0.3635(8) 0.1966(10) 0.087(5) Uiso 0.555(16) 1 d D U P A 1
H2 H 0.5397 0.3960 0.2217 0.105 Uiso 0.555(16) 1 calc R U P A 1
C3 C 0.5187(8) 0.3412(8) 0.1335(10) 0.098(5) Uiso 0.555(16) 1 d D U P A 1
H3 H 0.4862 0.3581 0.1164 0.117 Uiso 0.555(16) 1 calc R U P A 1
C4 C 0.5387(8) 0.2937(8) 0.0995(11) 0.092(5) Uiso 0.555(16) 1 d D U P A 1
H4 H 0.5171 0.2798 0.0594 0.111 Uiso 0.555(16) 1 calc R U P A 1
C5 C 0.5854(8) 0.2639(9) 0.1155(12) 0.091(4) Uiso 0.555(16) 1 d D U P A 1
H5 H 0.5974 0.2337 0.0863 0.109 Uiso 0.555(16) 1 calc R U P A 1
C6 C 0.6144(8) 0.2845(7) 0.1831(10) 0.076(4) Uiso 0.555(16) 1 d D U P A 1
H6 H 0.6443 0.2648 0.2032 0.091 Uiso 0.555(16) 1 calc R U P A 1
C1' C 0.6109(10) 0.3183(9) 0.2197(13) 0.075(5) Uiso 0.445(16) 1 d D U P A 2
C2' C 0.5701(9) 0.3480(9) 0.1787(12) 0.076(5) Uiso 0.445(16) 1 d D U P A 2
H2' H 0.5619 0.3846 0.1913 0.091 Uiso 0.445(16) 1 calc R U P A 2
C3' C 0.5407(11) 0.3198(11) 0.1159(15) 0.098(5) Uiso 0.445(16) 1 d D U P A 2
H3' H 0.5098 0.3348 0.0911 0.118 Uiso 0.445(16) 1 calc R U P A 2
C4' C 0.5627(12) 0.2703(10) 0.0974(16) 0.103(6) Uiso 0.445(16) 1 d D U P A 2
H4' H 0.5479 0.2549 0.0527 0.124 Uiso 0.445(16) 1 calc R U P A 2
C5' C 0.6018(10) 0.2386(10) 0.1306(13) 0.090(5) Uiso 0.445(16) 1 d D U P A 2
H5' H 0.6107 0.2030 0.1134 0.108 Uiso 0.445(16) 1 calc R U P A 2
C6' C 0.6294(10) 0.2654(10) 0.1972(13) 0.085(5) Uiso 0.445(16) 1 d D U P A 2
H6' H 0.6582 0.2478 0.2233 0.102 Uiso 0.445(16) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 2.074(6) . ?
Ni1 O3 2.108(7) . ?
Ni1 N23 2.112(7) 8_666 ?
Ni1 N23 2.112(7) 3_655 ?
Ni1 N13 2.119(7) . ?
Ni1 N13 2.119(7) 6_566 ?
Rb1 O4 3.187(7) 8_666 ?
Rb1 O4 3.187(7) 5_656 ?
Rb1 O4 3.187(7) 3_655 ?
Rb1 O4 3.187(7) 7_556 ?
Rb1 O4 3.187(7) 2_665 ?
Rb1 O4 3.187(7) 6_566 ?
Rb1 O4 3.187(7) 4_565 ?
Rb1 O4 3.188(7) . ?
Rb1 O4' 3.28(2) . ?
Rb1 O4' 3.28(2) 5_656 ?
Rb1 O4' 3.28(2) 8_666 ?
Rb1 O4' 3.28(2) 3_655 ?
O4 O4' 0.97(2) . ?
O5 O5 0.92(2) 8_666 ?
P1 O1 1.493(5) . ?
P1 N1 1.639(7) . ?
P1 N2 1.646(7) . ?
P1 C1' 1.77(2) . ?
P1 C1 1.799(16) . ?
N1 C11 1.395(10) . ?
N1 H1A 0.8800 . ?
C11 C16 1.375(10) . ?
C11 C12 1.411(11) . ?
C12 N13 1.333(9) . ?
C12 H12 0.9500 . ?
N13 C14 1.368(10) . ?
C14 C15 1.365(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.372(12) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
N2 C21 1.424(11) . ?
N2 H2A 0.8800 . ?
C21 C26 1.358(11) . ?
C21 C22 1.400(10) . ?
C22 N23 1.372(9) . ?
C22 H22 0.9500 . ?
N23 C24 1.337(10) . ?
N23 Ni1 2.112(7) 4_565 ?
C24 C25 1.396(11) . ?
C24 H24 0.9500 . ?
C25 C26 1.358(12) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C1 C6 1.417(17) . ?
C1 C2 1.424(17) . ?
C2 C3 1.465(17) . ?
C2 H2 0.9500 . ?
C3 C4 1.402(18) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(19) . ?
C4 H4 0.9500 . ?
C5 C6 1.482(18) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C1' C6' 1.433(19) . ?
C1' C2' 1.436(19) . ?
C2' C3' 1.495(19) . ?
C2' H2' 0.9500 . ?
C3' C4' 1.37(2) . ?
C3' H3' 0.9500 . ?
C4' C5' 1.37(2) . ?
C4' H4' 0.9500 . ?
C5' C6' 1.512(19) . ?
C5' H5' 0.9500 . ?
C6' H6' 0.9500 . ?

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 Ni1 O3 180.0 . . ?
O2 Ni1 N23 89.58(17) . 8_666 ?
O3 Ni1 N23 90.42(17) . 8_666 ?
O2 Ni1 N23 89.58(17) . 3_655 ?
O3 Ni1 N23 90.42(17) . 3_655 ?
N23 Ni1 N23 179.2(3) 8_666 3_655 ?
O2 Ni1 N13 90.41(17) . . ?
O3 Ni1 N13 89.59(17) . . ?
N23 Ni1 N13 89.9(2) 8_666 . ?
N23 Ni1 N13 90.1(2) 3_655 . ?
O2 Ni1 N13 90.41(17) . 6_566 ?
O3 Ni1 N13 89.59(17) . 6_566 ?
N23 Ni1 N13 90.1(2) 8_666 6_566 ?
N23 Ni1 N13 89.9(2) 3_655 6_566 ?
N13 Ni1 N13 179.2(4) . 6_566 ?
O4 Rb1 O4 67.50(15) 8_666 5_656 ?
O4 Rb1 O4 179.6(4) 8_666 3_655 ?
O4 Rb1 O4 112.1(4) 5_656 3_655 ?
O4 Rb1 O4 103.6(3) 8_666 7_556 ?
O4 Rb1 O4 67.50(15) 5_656 7_556 ?
O4 Rb1 O4 76.4(3) 3_655 7_556 ?
O4 Rb1 O4 112.1(4) 8_666 2_665 ?
O4 Rb1 O4 76.4(3) 5_656 2_665 ?
O4 Rb1 O4 67.50(15) 3_655 2_665 ?
O4 Rb1 O4 112.9(4) 7_556 2_665 ?
O4 Rb1 O4 67.50(15) 8_666 6_566 ?
O4 Rb1 O4 103.6(3) 5_656 6_566 ?
O4 Rb1 O4 112.9(4) 3_655 6_566 ?
O4 Rb1 O4 67.50(15) 7_556 6_566 ?
O4 Rb1 O4 179.6(4) 2_665 6_566 ?
O4 Rb1 O4 76.4(3) 8_666 4_565 ?
O4 Rb1 O4 112.9(4) 5_656 4_565 ?
O4 Rb1 O4 103.6(3) 3_655 4_565 ?
O4 Rb1 O4 179.6(4) 7_556 4_565 ?
O4 Rb1 O4 67.50(15) 2_665 4_565 ?
O4 Rb1 O4 112.1(4) 6_566 4_565 ?
O4 Rb1 O4 112.9(4) 8_666 . ?
O4 Rb1 O4 179.6(4) 5_656 . ?
O4 Rb1 O4 67.50(15) 3_655 . ?
O4 Rb1 O4 112.1(4) 7_556 . ?
O4 Rb1 O4 103.6(3) 2_665 . ?
O4 Rb1 O4 76.4(3) 6_566 . ?
O4 Rb1 O4 67.50(15) 4_565 . ?
O4 Rb1 O4' 119.7(6) 8_666 . ?
O4 Rb1 O4' 162.9(4) 5_656 . ?
O4 Rb1 O4' 60.6(6) 3_655 . ?
O4 Rb1 O4' 121.4(6) 7_556 . ?
O4 Rb1 O4' 86.5(5) 2_665 . ?
O4 Rb1 O4' 93.5(5) 6_566 . ?
O4 Rb1 O4' 58.3(7) 4_565 . ?
O4 Rb1 O4' 17.1(4) . . ?
O4 Rb1 O4' 58.3(7) 8_666 5_656 ?
O4 Rb1 O4' 17.1(4) 5_656 5_656 ?
O4 Rb1 O4' 121.4(6) 3_655 5_656 ?
O4 Rb1 O4' 60.6(6) 7_556 5_656 ?
O4 Rb1 O4' 93.5(5) 2_665 5_656 ?
O4 Rb1 O4' 86.5(5) 6_566 5_656 ?
O4 Rb1 O4' 119.7(6) 4_565 5_656 ?
O4 Rb1 O4' 162.9(4) . 5_656 ?
O4' Rb1 O4' 177.8(12) . 5_656 ?
O4 Rb1 O4' 17.1(4) 8_666 8_666 ?
O4 Rb1 O4' 60.6(6) 5_656 8_666 ?
O4 Rb1 O4' 162.9(4) 3_655 8_666 ?
O4 Rb1 O4' 86.5(5) 7_556 8_666 ?
O4 Rb1 O4' 121.4(6) 2_665 8_666 ?
O4 Rb1 O4' 58.3(7) 6_566 8_666 ?
O4 Rb1 O4' 93.5(5) 4_565 8_666 ?
O4 Rb1 O4' 119.7(6) . 8_666 ?
O4' Rb1 O4' 130.8(11) . 8_666 ?
O4' Rb1 O4' 47.5(6) 5_656 8_666 ?
O4 Rb1 O4' 162.9(4) 8_666 3_655 ?
O4 Rb1 O4' 121.4(6) 5_656 3_655 ?
O4 Rb1 O4' 17.1(4) 3_655 3_655 ?
O4 Rb1 O4' 93.5(5) 7_556 3_655 ?
O4 Rb1 O4' 60.6(6) 2_665 3_655 ?
O4 Rb1 O4' 119.7(6) 6_566 3_655 ?
O4 Rb1 O4' 86.5(5) 4_565 3_655 ?
O4 Rb1 O4' 58.3(7) . 3_655 ?
O4' Rb1 O4' 47.5(6) . 3_655 ?
O4' Rb1 O4' 134.2(11) 5_656 3_655 ?
O4' Rb1 O4' 177.8(12) 8_666 3_655 ?
O4' O4 Rb1 86.7(14) . . ?
O4 O4' Rb1 76.1(14) . . ?
O5 O5 Rb1 82.0(2) 8_666 . ?
O1 P1 N1 115.2(4) . . ?
O1 P1 N2 110.1(3) . . ?
N1 P1 N2 104.2(4) . . ?
O1 P1 C1' 119.4(9) . . ?
N1 P1 C1' 104.2(10) . . ?
N2 P1 C1' 101.9(8) . . ?
O1 P1 C1 106.0(6) . . ?
N1 P1 C1 104.8(7) . . ?
N2 P1 C1 116.7(6) . . ?
C11 N1 P1 129.5(6) . . ?
C11 N1 H1A 115.2 . . ?
P1 N1 H1A 115.2 . . ?
C16 C11 N1 120.5(8) . . ?
C16 C11 C12 118.2(8) . . ?
N1 C11 C12 121.3(7) . . ?
N13 C12 C11 122.1(8) . . ?
N13 C12 H12 118.9 . . ?
C11 C12 H12 118.9 . . ?
C12 N13 C14 118.3(7) . . ?
C12 N13 Ni1 122.1(6) . . ?
C14 N13 Ni1 119.5(6) . . ?
C15 C14 N13 121.7(9) . . ?
C15 C14 H14 119.2 . . ?
N13 C14 H14 119.2 . . ?
C14 C15 C16 120.1(9) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C11 119.5(8) . . ?
C15 C16 H16 120.2 . . ?
C11 C16 H16 120.2 . . ?
C21 N2 P1 130.1(6) . . ?
C21 N2 H2A 115.0 . . ?
P1 N2 H2A 115.0 . . ?
C26 C21 C22 120.2(8) . . ?
C26 C21 N2 120.6(8) . . ?
C22 C21 N2 119.2(8) . . ?
N23 C22 C21 120.6(8) . . ?
N23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C24 N23 C22 117.6(7) . . ?
C24 N23 Ni1 122.1(6) . 4_565 ?
C22 N23 Ni1 120.3(5) . 4_565 ?
N23 C24 C25 123.1(9) . . ?
N23 C24 H24 118.5 . . ?
C25 C24 H24 118.5 . . ?
C26 C25 C24 118.8(9) . . ?
C26 C25 H25 120.6 . . ?
C24 C25 H25 120.6 . . ?
C21 C26 C25 119.8(8) . . ?
C21 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C6 C1 C2 124.3(15) . . ?
C6 C1 P1 115.3(12) . . ?
C2 C1 P1 120.4(12) . . ?
C1 C2 C3 116.0(16) . . ?
C1 C2 H2 122.0 . . ?
C3 C2 H2 122.0 . . ?
C4 C3 C2 117.0(17) . . ?
C4 C3 H3 121.5 . . ?
C2 C3 H3 121.5 . . ?
C5 C4 C3 129.8(19) . . ?
C5 C4 H4 115.1 . . ?
C3 C4 H4 115.1 . . ?
C4 C5 C6 112.4(17) . . ?
C4 C5 H5 123.8 . . ?
C6 C5 H5 123.8 . . ?
C1 C6 C5 120.0(16) . . ?
C1 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6' C1' C2' 122.8(19) . . ?
C6' C1' P1 124.6(15) . . ?
C2' C1' P1 112.1(14) . . ?
C1' C2' C3' 118.6(19) . . ?
C1' C2' H2' 120.7 . . ?
C3' C2' H2' 120.7 . . ?
C4' C3' C2' 113(2) . . ?
C4' C3' H3' 123.3 . . ?
C2' C3' H3' 123.3 . . ?
C5' C4' C3' 133(2) . . ?
C5' C4' H4' 113.6 . . ?
C3' C4' H4' 113.6 . . ?
C4' C5' C6' 114(2) . . ?
C4' C5' H5' 123.2 . . ?
C6' C5' H5' 123.2 . . ?
C1' C6' C5' 118.0(19) . . ?
C1' C6' H6' 121.0 . . ?
C5' C6' H6' 121.0 . . ?

_refine_diff_density_max         0.286
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.057




_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol and water'
_exptl_crystal_preparation       ', Ferroelectric and Dielectric'
####################################################################### 
# 
# 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_compound_Hy-Na_1_sq
_database_code_depnum_ccdc_archive 'CCDC 1543632'
_audit_update_record             
;
2017-04-12 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C128 H189.50 N40.25 Na0.25 Ni4 O67.50 P8'
_chemical_formula_weight         3860.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_H-M_alt        'I 4 2 2'
_space_group_name_Hall           'I 4 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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   24.399(7)
_cell_length_b                   24.399(7)
_cell_length_c                   17.576(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10463(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9943
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      21.42

_exptl_crystal_description       block
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_F_000             4028
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.500
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6795
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51429
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.601
_diffrn_reflns_theta_max         22.483
_diffrn_reflns_theta_full        22.483
_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 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3427
_reflns_number_gt                2912
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1021P)²+11.5730P] 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_details 
;
 Flack x determined using 1145 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.022(10)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         3427
_refine_ls_number_parameters     220
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1664
_refine_ls_wR_factor_gt          0.1496
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.76091(4) 0.5000 0.0649(4) Uani 1 2 d S T P . .
P1 P 0.64068(10) 0.64208(10) 0.71058(10) 0.0796(6) Uani 1 1 d . . . . .
O1 O 0.6044(3) 0.6102(3) 0.6620(3) 0.0938(16) Uani 1 1 d . . . . .
O2 O 0.5000 0.6756(2) 0.5000 0.0695(15) Uani 1 2 d S T P . .
O3 O 0.5000 0.8472(2) 0.5000 0.089(2) Uani 1 2 d S T P . .
N1 N 0.6759(3) 0.6862(3) 0.6625(3) 0.0861(19) Uani 1 1 d . . . . .
H1A H 0.7112 0.6875 0.6727 0.103 Uiso 1 1 calc R U . . .
N2 N 0.6890(3) 0.6073(3) 0.7529(4) 0.094(2) Uani 1 1 d . . . . .
H2A H 0.6930 0.6138 0.8019 0.113 Uiso 1 1 calc R U . . .
N13 N 0.5827(2) 0.7594(2) 0.5289(4) 0.0701(17) Uani 1 1 d . . . . .
N23 N 0.7622(2) 0.5213(2) 0.6159(3) 0.0660(15) Uani 1 1 d . . . . .
C1 C 0.5949(7) 0.6666(7) 0.7804(9) 0.069(5) Uiso 0.49(2) 1 d D U P A 1
C2 C 0.6097(9) 0.7136(9) 0.8170(10) 0.084(6) Uiso 0.49(2) 1 d D U P A 1
H2 H 0.6405 0.7331 0.7980 0.101 Uiso 0.49(2) 1 calc R U P A 1
C3 C 0.5820(9) 0.7357(10) 0.8827(11) 0.092(6) Uiso 0.49(2) 1 d D U P A 1
H3 H 0.5928 0.7681 0.9087 0.111 Uiso 0.49(2) 1 calc R U P A 1
C4 C 0.5368(9) 0.7032(10) 0.9031(13) 0.102(7) Uiso 0.49(2) 1 d D U P A 1
H4 H 0.5176 0.7152 0.9471 0.122 Uiso 0.49(2) 1 calc R U P A 1
C5 C 0.5149(10) 0.6543(10) 0.8678(12) 0.118(8) Uiso 0.49(2) 1 d D U P A 1
H5 H 0.4824 0.6357 0.8830 0.142 Uiso 0.49(2) 1 calc R U P A 1
C6 C 0.5500(9) 0.6382(9) 0.8059(12) 0.102(7) Uiso 0.49(2) 1 d D U P A 1
H6 H 0.5414 0.6050 0.7805 0.122 Uiso 0.49(2) 1 calc R U P A 1
C1' C 0.6121(7) 0.6838(7) 0.7877(9) 0.066(4) Uiso 0.51(2) 1 d D U P A 2
C2' C 0.6294(9) 0.7331(9) 0.8106(11) 0.097(6) Uiso 0.51(2) 1 d D U P A 2
H2' H 0.6596 0.7498 0.7857 0.116 Uiso 0.51(2) 1 calc R U P A 2
C3' C 0.6027(10) 0.7615(10) 0.8729(12) 0.115(7) Uiso 0.51(2) 1 d D U P A 2
H3' H 0.6132 0.7972 0.8889 0.138 Uiso 0.51(2) 1 calc R U P A 2
C4' C 0.5595(9) 0.7315(9) 0.9080(13) 0.107(7) Uiso 0.51(2) 1 d D U P A 2
H4' H 0.5430 0.7485 0.9509 0.129 Uiso 0.51(2) 1 calc R U P A 2
C5' C 0.5376(10) 0.6793(11) 0.8874(14) 0.120(8) Uiso 0.51(2) 1 d D U P A 2
H5' H 0.5066 0.6619 0.9097 0.145 Uiso 0.51(2) 1 calc R U P A 2
C6' C 0.5712(9) 0.6577(9) 0.8263(12) 0.109(7) Uiso 0.51(2) 1 d D U P A 2
H6' H 0.5639 0.6210 0.8115 0.131 Uiso 0.51(2) 1 calc R U P A 2
C11 C 0.6569(3) 0.7236(3) 0.6053(4) 0.071(2) Uani 1 1 d . . . . .
C12 C 0.6015(3) 0.7245(3) 0.5831(4) 0.0691(19) Uani 1 1 d . . . . .
H12 H 0.5766 0.7000 0.6068 0.083 Uiso 1 1 calc R U . . .
C14 C 0.6198(3) 0.7936(3) 0.5001(6) 0.0747(19) Uani 1 1 d . . . . .
H14 H 0.6069 0.8205 0.4653 0.090 Uiso 1 1 calc R U . . .
C15 C 0.6739(3) 0.7938(3) 0.5158(6) 0.087(3) Uani 1 1 d . . . . .
H15 H 0.6987 0.8164 0.4884 0.105 Uiso 1 1 calc R U . . .
C16 C 0.6923(3) 0.7592(4) 0.5743(5) 0.079(2) Uani 1 1 d . . . . .
H16 H 0.7291 0.7609 0.5916 0.095 Uiso 1 1 calc R U . . .
C21 C 0.7246(3) 0.5692(3) 0.7227(5) 0.078(2) Uani 1 1 d . . . . .
C22 C 0.7274(3) 0.5566(3) 0.6459(4) 0.0663(19) Uani 1 1 d . . . . .
H22 H 0.7027 0.5746 0.6126 0.080 Uiso 1 1 calc R U . . .
C24 C 0.7977(3) 0.4947(4) 0.6633(4) 0.0717(19) Uani 1 1 d . . . . .
H24 H 0.8218 0.4678 0.6432 0.086 Uiso 1 1 calc R U . . .
C25 C 0.7989(3) 0.5065(4) 0.7403(5) 0.088(2) Uani 1 1 d . . . . .
H25 H 0.8246 0.4886 0.7724 0.106 Uiso 1 1 calc R U . . .
C26 C 0.7632(3) 0.5440(4) 0.7703(4) 0.078(2) Uani 1 1 d . . . . .
H26 H 0.7645 0.5529 0.8229 0.094 Uiso 1 1 calc R U . . .
O4 O 0.4981(6) 0.6013(4) 0.6122(5) 0.080(2) Uiso 0.5 1 d . . P . .
O5 O 0.5776(8) 0.6042(8) 0.504(2) 0.100(7) Uiso 0.25 1 d . . P . .
O6 O 0.5000 0.5000 0.5000 0.086(7) Uiso 0.5 8 d S . P . .
O7 O 0.5000 0.5000 0.5722(16) 0.081(7) Uiso 0.125 4 d S . P . .
Na1 Na 0.5000 0.5000 0.5722(16) 0.081(7) Uiso 0.125 4 d S . 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
Ni1 O2 2.080(6) . ?
Ni1 N13 2.081(6) . ?
Ni1 N13 2.081(6) 5_656 ?
Ni1 N23 2.102(6) 7_556 ?
Ni1 N23 2.102(6) 3_655 ?
Ni1 O3 2.106(6) . ?
P1 O1 1.455(6) . ?
P1 N1 1.617(7) . ?
P1 N2 1.633(8) . ?
P1 C1 1.764(15) . ?
P1 C1' 1.832(15) . ?
N1 C11 1.434(11) . ?
N1 H1A 0.8800 . ?
N2 C21 1.378(11) . ?
N2 H2A 0.8800 . ?
N13 C14 1.332(9) . ?
N13 C12 1.357(10) . ?
N23 C22 1.319(9) . ?
N23 C24 1.365(9) . ?
N23 Ni1 2.101(6) 4_565 ?
C1 C2 1.365(19) . ?
C1 C6 1.370(19) . ?
C2 C3 1.44(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.41(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.45(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.44(2) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C1' C2' 1.338(19) . ?
C1' C6' 1.366(19) . ?
C2' C3' 1.45(2) . ?
C2' H2' 0.9500 . ?
C3' C4' 1.43(2) . ?
C3' H3' 0.9500 . ?
C4' C5' 1.43(2) . ?
C4' H4' 0.9500 . ?
C5' C6' 1.45(2) . ?
C5' H5' 0.9500 . ?
C6' H6' 0.9500 . ?
C11 C16 1.339(11) . ?
C11 C12 1.406(11) . ?
C12 H12 0.9500 . ?
C14 C15 1.350(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.404(12) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.386(12) . ?
C21 C26 1.401(11) . ?
C22 H22 0.9500 . ?
C24 C25 1.384(11) . ?
C24 H24 0.9500 . ?
C25 C26 1.369(12) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
O5 O5 0.93(4) 7_556 ?
O6 O7 1.27(3) . ?
O6 Na1 1.27(3) 5_656 ?
O6 O7 1.27(3) 5_656 ?
O7 Na1 2.54(6) 5_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 N13 88.96(17) . . ?
O2 Ni1 N13 88.96(17) . 5_656 ?
N13 Ni1 N13 177.9(3) . 5_656 ?
O2 Ni1 N23 90.87(15) . 7_556 ?
N13 Ni1 N23 89.9(2) . 7_556 ?
N13 Ni1 N23 90.2(2) 5_656 7_556 ?
O2 Ni1 N23 90.87(15) . 3_655 ?
N13 Ni1 N23 90.2(2) . 3_655 ?
N13 Ni1 N23 89.9(2) 5_656 3_655 ?
N23 Ni1 N23 178.3(3) 7_556 3_655 ?
O2 Ni1 O3 180.0 . . ?
N13 Ni1 O3 91.04(17) . . ?
N13 Ni1 O3 91.04(17) 5_656 . ?
N23 Ni1 O3 89.13(15) 7_556 . ?
N23 Ni1 O3 89.13(15) 3_655 . ?
O1 P1 N1 111.9(3) . . ?
O1 P1 N2 115.4(4) . . ?
N1 P1 N2 101.5(4) . . ?
O1 P1 C1 101.7(7) . . ?
N1 P1 C1 118.3(7) . . ?
N2 P1 C1 108.5(6) . . ?
O1 P1 C1' 119.9(6) . . ?
N1 P1 C1' 102.6(6) . . ?
N2 P1 C1' 103.1(6) . . ?
C11 N1 P1 128.1(6) . . ?
C11 N1 H1A 115.9 . . ?
P1 N1 H1A 115.9 . . ?
C21 N2 P1 129.0(6) . . ?
C21 N2 H2A 115.5 . . ?
P1 N2 H2A 115.5 . . ?
C14 N13 C12 115.4(7) . . ?
C14 N13 Ni1 123.7(5) . . ?
C12 N13 Ni1 120.8(5) . . ?
C22 N23 C24 118.2(7) . . ?
C22 N23 Ni1 122.6(5) . 4_565 ?
C24 N23 Ni1 119.0(5) . 4_565 ?
C2 C1 C6 118.8(17) . . ?
C2 C1 P1 116.4(13) . . ?
C6 C1 P1 124.2(13) . . ?
C1 C2 C3 124.5(19) . . ?
C1 C2 H2 117.7 . . ?
C3 C2 H2 117.7 . . ?
C4 C3 C2 111.2(19) . . ?
C4 C3 H3 124.4 . . ?
C2 C3 H3 124.4 . . ?
C3 C4 C5 130(2) . . ?
C3 C4 H4 114.9 . . ?
C5 C4 H4 114.9 . . ?
C6 C5 C4 109(2) . . ?
C6 C5 H5 125.4 . . ?
C4 C5 H5 125.4 . . ?
C1 C6 C5 126(2) . . ?
C1 C6 H6 117.1 . . ?
C5 C6 H6 117.1 . . ?
C2' C1' C6' 120.0(18) . . ?
C2' C1' P1 127.1(12) . . ?
C6' C1' P1 112.8(13) . . ?
C1' C2' C3' 121(2) . . ?
C1' C2' H2' 119.4 . . ?
C3' C2' H2' 119.4 . . ?
C4' C3' C2' 114(2) . . ?
C4' C3' H3' 122.8 . . ?
C2' C3' H3' 122.8 . . ?
C3' C4' C5' 129(2) . . ?
C3' C4' H4' 115.6 . . ?
C5' C4' H4' 115.6 . . ?
C4' C5' C6' 107(2) . . ?
C4' C5' H5' 126.3 . . ?
C6' C5' H5' 126.3 . . ?
C1' C6' C5' 128(2) . . ?
C1' C6' H6' 116.1 . . ?
C5' C6' H6' 116.1 . . ?
C16 C11 C12 119.7(7) . . ?
C16 C11 N1 119.2(7) . . ?
C12 C11 N1 121.0(7) . . ?
N13 C12 C11 122.0(7) . . ?
N13 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
N13 C14 C15 126.1(7) . . ?
N13 C14 H14 117.0 . . ?
C15 C14 H14 117.0 . . ?
C14 C15 C16 117.4(8) . . ?
C14 C15 H15 121.3 . . ?
C16 C15 H15 121.3 . . ?
C11 C16 C15 118.9(7) . . ?
C11 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
N2 C21 C22 123.8(7) . . ?
N2 C21 C26 119.2(8) . . ?
C22 C21 C26 116.8(8) . . ?
N23 C22 C21 124.5(7) . . ?
N23 C22 H22 117.7 . . ?
C21 C22 H22 117.7 . . ?
N23 C24 C25 120.8(8) . . ?
N23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C26 C25 C24 120.1(7) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C21 119.4(8) . . ?
C25 C26 H26 120.3 . . ?
C21 C26 H26 120.3 . . ?
O7 O6 Na1 180.0 . 5_656 ?
O7 O6 O7 180.0 . 5_656 ?
Na1 O6 O7 0.0 5_656 5_656 ?
O6 O7 Na1 0.000(3) . 5_656 ?

_refine_diff_density_max         0.636
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.058




_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol and water'
_exptl_crystal_preparation       ', Ferroelectric and Dielectric'
####################################################################### 
# 
# 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_compound_Hy-K_2_sq
_database_code_depnum_ccdc_archive 'CCDC 1543633'
_audit_update_record             
;
2017-04-12 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C128 H198 Co4 K N41 O74 P8'
_chemical_formula_weight         4017.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_H-M_alt        'I 4 2 2'
_space_group_name_Hall           'I 4 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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   24.404(4)
_cell_length_b                   24.404(4)
_cell_length_c                   17.589(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10476(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2492
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      17.03

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_F_000             4184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.481
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6516
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            52721
_diffrn_reflns_av_unetI/netI     0.1248
_diffrn_reflns_av_R_equivalents  0.1837
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.180
_diffrn_reflns_theta_max         28.331
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6564
_reflns_number_gt                2805
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
'Refined as a 2-component inversion twin., SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1220P)²] 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_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.23(6)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         6564
_refine_ls_number_parameters     201
_refine_ls_number_restraints     201
_refine_ls_R_factor_all          0.1907
_refine_ls_R_factor_gt           0.0692
_refine_ls_wR_factor_ref         0.2402
_refine_ls_wR_factor_gt          0.1819
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.969
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.76200(5) 0.5000 0.0531(4) Uani 1 2 d S TU P . .
O2 O 0.5000 0.6766(2) 0.5000 0.0626(18) Uani 1 2 d S TU P . .
O3 O 0.5000 0.8492(3) 0.5000 0.091(2) Uani 1 2 d S TU P . .
K1 K 0.5000 0.5000 0.5000 0.0879(17) Uani 1 8 d S T P . .
O4 O 0.4994(5) 0.5995(3) 0.3942(5) 0.0684(19) Uiso 0.650(4) 1 d . U P . .
O4' O 0.505(2) 0.5665(17) 0.349(3) 0.0684(19) Uiso 0.120(4) 1 d . U P . .
O5 O 0.5754(8) 0.6020(8) 0.501(2) 0.0684(19) Uiso 0.230(4) 1 d . U P . .
P1 P 0.35865(11) 0.63961(11) 0.70899(12) 0.0689(6) Uani 1 1 d . U . . .
O1 O 0.3916(3) 0.6057(3) 0.6572(3) 0.0774(16) Uani 1 1 d . U . . .
N1 N 0.3933(3) 0.6870(3) 0.7535(5) 0.083(2) Uani 1 1 d . U . . .
H1 H 0.3878 0.6895 0.8028 0.100 Uiso 1 1 calc R U . . .
C11 C 0.4310(4) 0.7241(4) 0.7220(6) 0.067(2) Uani 1 1 d . U . . .
C12 C 0.4438(3) 0.7254(3) 0.6472(6) 0.064(2) Uani 1 1 d . U . . .
H12 H 0.4276 0.6987 0.6150 0.077 Uiso 1 1 calc R U . . .
N13 N 0.4787(3) 0.7627(2) 0.6150(4) 0.0603(17) Uani 1 1 d . U . . .
C14 C 0.5042(4) 0.7984(3) 0.6623(5) 0.066(2) Uani 1 1 d . U . . .
H14 H 0.5306 0.8235 0.6431 0.079 Uiso 1 1 calc R U . . .
C15 C 0.4911(4) 0.7980(3) 0.7407(6) 0.078(3) Uani 1 1 d . U . . .
H15 H 0.5088 0.8235 0.7733 0.093 Uiso 1 1 calc R U . . .
C16 C 0.4548(4) 0.7629(4) 0.7707(6) 0.077(3) Uani 1 1 d . U . . .
H16 H 0.4455 0.7643 0.8231 0.092 Uiso 1 1 calc R U . . .
N2 N 0.3131(3) 0.6753(3) 0.6615(4) 0.079(2) Uani 1 1 d . U . . .
H2 H 0.3110 0.7104 0.6729 0.094 Uiso 1 1 calc R U . . .
C21 C 0.2768(3) 0.6564(3) 0.6042(5) 0.061(2) Uani 1 1 d . U . . .
C22 C 0.2745(3) 0.6012(3) 0.5870(5) 0.060(2) Uani 1 1 d . U . . .
H22 H 0.2966 0.5758 0.6142 0.072 Uiso 1 1 calc R U . . .
N23 N 0.2391(3) 0.5826(3) 0.5289(4) 0.0607(17) Uani 1 1 d . U . . .
C24 C 0.2060(3) 0.6201(3) 0.4990(7) 0.071(2) Uani 1 1 d . U . . .
H24 H 0.1806 0.6086 0.4614 0.085 Uiso 1 1 calc R U . . .
C25 C 0.2061(3) 0.6729(3) 0.5184(6) 0.071(3) Uani 1 1 d . U . . .
H25 H 0.1811 0.6974 0.4946 0.085 Uiso 1 1 calc R U . . .
C26 C 0.2412(4) 0.6922(4) 0.5714(5) 0.068(2) Uani 1 1 d . U . . .
H26 H 0.2411 0.7298 0.5854 0.082 Uiso 1 1 calc R U . . .
C1 C 0.3189(7) 0.6110(8) 0.7852(9) 0.079(5) Uiso 0.421(14) 1 d DG U P A 1
C2 C 0.2671(7) 0.6273(7) 0.8090(10) 0.079(5) Uiso 0.421(14) 1 d DG U P A 1
H2A H 0.2490 0.6566 0.7841 0.095 Uiso 0.421(14) 1 calc R U P A 1
C3 C 0.2418(6) 0.6006(7) 0.8694(10) 0.086(5) Uiso 0.421(14) 1 d DG U P A 1
H3 H 0.2064 0.6117 0.8856 0.103 Uiso 0.421(14) 1 calc R U P A 1
C4 C 0.2684(7) 0.5576(7) 0.9059(10) 0.091(6) Uiso 0.421(14) 1 d DG U P A 1
H4 H 0.2511 0.5393 0.9471 0.109 Uiso 0.421(14) 1 calc R U P A 1
C5 C 0.3202(7) 0.5413(7) 0.8821(10) 0.090(5) Uiso 0.421(14) 1 d DG U P A 1
H5 H 0.3383 0.5120 0.9071 0.108 Uiso 0.421(14) 1 calc R U P A 1
C6 C 0.3455(6) 0.5681(8) 0.8218(10) 0.082(5) Uiso 0.421(14) 1 d DG U P A 1
H6 H 0.3809 0.5569 0.8055 0.099 Uiso 0.421(14) 1 calc R U P A 1
C1' C 0.3345(5) 0.5958(5) 0.7817(7) 0.077(4) Uiso 0.579(14) 1 d DG U P A 2
C2' C 0.2872(5) 0.6117(5) 0.8197(8) 0.083(4) Uiso 0.579(14) 1 d DG U P A 2
H2' H 0.2678 0.6435 0.8037 0.099 Uiso 0.579(14) 1 calc R U P A 2
C3' C 0.2682(5) 0.5812(5) 0.8810(7) 0.096(4) Uiso 0.579(14) 1 d DG U P A 2
H3' H 0.2358 0.5921 0.9069 0.115 Uiso 0.579(14) 1 calc R U P A 2
C4' C 0.2965(6) 0.5348(5) 0.9044(7) 0.087(5) Uiso 0.579(14) 1 d DG U P A 2
H4' H 0.2835 0.5139 0.9463 0.104 Uiso 0.579(14) 1 calc R U P A 2
C5' C 0.3439(5) 0.5188(5) 0.8664(8) 0.103(5) Uiso 0.579(14) 1 d DG U P A 2
H5' H 0.3632 0.4871 0.8824 0.123 Uiso 0.579(14) 1 calc R U P A 2
C6' C 0.3629(4) 0.5493(6) 0.8051(8) 0.097(5) Uiso 0.579(14) 1 d DG U P A 2
H6' H 0.3952 0.5384 0.7792 0.116 Uiso 0.579(14) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N23 2.079(7) 8_666 ?
Co1 N23 2.079(7) 4_565 ?
Co1 O2 2.085(6) . ?
Co1 N13 2.088(8) 5_656 ?
Co1 N13 2.088(8) . ?
Co1 O3 2.128(7) . ?
K1 O4 3.060(8) 7_556 ?
K1 O4 3.060(8) 5_656 ?
K1 O4 3.060(8) 3_655 ?
K1 O4 3.060(8) 2_665 ?
K1 O4 3.060(8) 8_666 ?
K1 O4 3.060(8) 6_566 ?
K1 O4 3.060(8) 4_565 ?
K1 O4 3.060(8) . ?
K1 O5 3.10(2) . ?
K1 O5 3.10(2) 8_666 ?
K1 O5 3.10(2) 7_556 ?
K1 O5 3.10(2) 2_665 ?
O4 O4' 1.14(4) . ?
O5 O5 0.92(4) 7_556 ?
P1 O1 1.471(6) . ?
P1 N1 1.632(8) . ?
P1 N2 1.641(7) . ?
P1 C1' 1.768(9) . ?
P1 C1 1.796(13) . ?
N1 C11 1.405(11) . ?
N1 H1 0.8800 . ?
C11 C12 1.354(13) . ?
C11 C16 1.402(12) . ?
C12 N13 1.369(10) . ?
C12 H12 0.9500 . ?
N13 C14 1.357(10) . ?
C14 C15 1.415(13) . ?
C14 H14 0.9500 . ?
C15 C16 1.342(13) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
N2 C21 1.420(11) . ?
N2 H2 0.8800 . ?
C21 C26 1.361(12) . ?
C21 C22 1.383(11) . ?
C22 N23 1.413(10) . ?
C22 H22 0.9500 . ?
N23 C24 1.331(10) . ?
N23 Co1 2.079(7) 3_655 ?
C24 C25 1.333(11) . ?
C24 H24 0.9500 . ?
C25 C26 1.351(13) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C2 C3 1.3900 . ?
C2 H2A 0.9500 . ?
C3 C4 1.3900 . ?
C3 H3 0.9500 . ?
C4 C5 1.3900 . ?
C4 H4 0.9500 . ?
C5 C6 1.3900 . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C1' C2' 1.3900 . ?
C1' C6' 1.3900 . ?
C2' C3' 1.3900 . ?
C2' H2' 0.9500 . ?
C3' C4' 1.3900 . ?
C3' H3' 0.9500 . ?
C4' C5' 1.3900 . ?
C4' H4' 0.9500 . ?
C5' C6' 1.3900 . ?
C5' H5' 0.9500 . ?
C6' H6' 0.9500 . ?

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
N23 Co1 N23 178.5(3) 8_666 4_565 ?
N23 Co1 O2 89.23(17) 8_666 . ?
N23 Co1 O2 89.23(17) 4_565 . ?
N23 Co1 N13 90.3(3) 8_666 5_656 ?
N23 Co1 N13 89.7(3) 4_565 5_656 ?
O2 Co1 N13 90.48(16) . 5_656 ?
N23 Co1 N13 89.7(3) 8_666 . ?
N23 Co1 N13 90.3(3) 4_565 . ?
O2 Co1 N13 90.47(17) . . ?
N13 Co1 N13 179.0(3) 5_656 . ?
N23 Co1 O3 90.77(17) 8_666 . ?
N23 Co1 O3 90.77(17) 4_565 . ?
O2 Co1 O3 180.0 . . ?
N13 Co1 O3 89.52(17) 5_656 . ?
N13 Co1 O3 89.53(17) . . ?
O4 K1 O4 68.30(16) 7_556 5_656 ?
O4 K1 O4 179.5(4) 7_556 3_655 ?
O4 K1 O4 112.2(4) 5_656 3_655 ?
O4 K1 O4 111.2(4) 7_556 2_665 ?
O4 K1 O4 179.5(4) 5_656 2_665 ?
O4 K1 O4 68.30(16) 3_655 2_665 ?
O4 K1 O4 105.1(3) 7_556 8_666 ?
O4 K1 O4 68.30(16) 5_656 8_666 ?
O4 K1 O4 74.9(3) 3_655 8_666 ?
O4 K1 O4 112.2(4) 2_665 8_666 ?
O4 K1 O4 68.30(16) 7_556 6_566 ?
O4 K1 O4 105.1(3) 5_656 6_566 ?
O4 K1 O4 111.2(4) 3_655 6_566 ?
O4 K1 O4 74.9(3) 2_665 6_566 ?
O4 K1 O4 68.30(16) 8_666 6_566 ?
O4 K1 O4 74.9(3) 7_556 4_565 ?
O4 K1 O4 111.2(4) 5_656 4_565 ?
O4 K1 O4 105.1(3) 3_655 4_565 ?
O4 K1 O4 68.30(16) 2_665 4_565 ?
O4 K1 O4 179.5(4) 8_666 4_565 ?
O4 K1 O4 112.2(4) 6_566 4_565 ?
O4 K1 O4 112.2(4) 7_556 . ?
O4 K1 O4 74.9(3) 5_656 . ?
O4 K1 O4 68.30(16) 3_655 . ?
O4 K1 O4 105.1(3) 2_665 . ?
O4 K1 O4 111.2(4) 8_666 . ?
O4 K1 O4 179.5(4) 6_566 . ?
O4 K1 O4 68.30(16) 4_565 . ?
O4 K1 O5 61.9(6) 7_556 . ?
O4 K1 O5 49.9(6) 5_656 . ?
O4 K1 O5 118.6(6) 3_655 . ?
O4 K1 O5 129.6(6) 2_665 . ?
O4 K1 O5 117.7(6) 8_666 . ?
O4 K1 O5 129.7(6) 6_566 . ?
O4 K1 O5 61.8(6) 4_565 . ?
O4 K1 O5 50.7(6) . . ?
O4 K1 O5 129.6(6) 7_556 8_666 ?
O4 K1 O5 118.6(6) 5_656 8_666 ?
O4 K1 O5 49.9(6) 3_655 8_666 ?
O4 K1 O5 61.9(6) 2_665 8_666 ?
O4 K1 O5 50.7(6) 8_666 8_666 ?
O4 K1 O5 61.8(6) 6_566 8_666 ?
O4 K1 O5 129.7(6) 4_565 8_666 ?
O4 K1 O5 117.7(6) . 8_666 ?
O5 K1 O5 162.9(7) . 8_666 ?
O4 K1 O5 50.7(6) 7_556 7_556 ?
O4 K1 O5 61.8(6) 5_656 7_556 ?
O4 K1 O5 129.7(6) 3_655 7_556 ?
O4 K1 O5 117.7(6) 2_665 7_556 ?
O4 K1 O5 129.6(6) 8_666 7_556 ?
O4 K1 O5 118.6(6) 6_566 7_556 ?
O4 K1 O5 49.9(6) 4_565 7_556 ?
O4 K1 O5 61.9(6) . 7_556 ?
O5 K1 O5 17.1(7) . 7_556 ?
O5 K1 O5 179.6(14) 8_666 7_556 ?
O4 K1 O5 117.7(6) 7_556 2_665 ?
O4 K1 O5 129.7(6) 5_656 2_665 ?
O4 K1 O5 61.8(6) 3_655 2_665 ?
O4 K1 O5 50.7(6) 2_665 2_665 ?
O4 K1 O5 61.9(6) 8_666 2_665 ?
O4 K1 O5 49.9(6) 6_566 2_665 ?
O4 K1 O5 118.6(6) 4_565 2_665 ?
O4 K1 O5 129.6(6) . 2_665 ?
O5 K1 O5 179.6(14) . 2_665 ?
O5 K1 O5 17.1(7) 8_666 2_665 ?
O5 K1 O5 162.9(7) 7_556 2_665 ?
O4' O4 K1 82(2) . . ?
O4 O4' K1 77(2) . . ?
O5 O5 K1 81.5(3) 7_556 . ?
O1 P1 N1 114.3(5) . . ?
O1 P1 N2 110.8(4) . . ?
N1 P1 N2 102.6(5) . . ?
O1 P1 C1' 106.9(6) . . ?
N1 P1 C1' 104.7(6) . . ?
N2 P1 C1' 117.7(6) . . ?
O1 P1 C1 122.7(7) . . ?
N1 P1 C1 101.3(7) . . ?
N2 P1 C1 102.7(7) . . ?
C11 N1 P1 127.4(7) . . ?
C11 N1 H1 116.3 . . ?
P1 N1 H1 116.3 . . ?
C12 C11 C16 118.8(9) . . ?
C12 C11 N1 123.3(8) . . ?
C16 C11 N1 117.8(9) . . ?
C11 C12 N13 124.1(8) . . ?
C11 C12 H12 117.9 . . ?
N13 C12 H12 117.9 . . ?
C14 N13 C12 117.3(8) . . ?
C14 N13 Co1 119.0(6) . . ?
C12 N13 Co1 123.3(6) . . ?
N13 C14 C15 119.2(9) . . ?
N13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C16 C15 C14 122.6(9) . . ?
C16 C15 H15 118.7 . . ?
C14 C15 H15 118.7 . . ?
C15 C16 C11 117.7(10) . . ?
C15 C16 H16 121.2 . . ?
C11 C16 H16 121.2 . . ?
C21 N2 P1 127.7(7) . . ?
C21 N2 H2 116.2 . . ?
P1 N2 H2 116.2 . . ?
C26 C21 C22 120.5(8) . . ?
C26 C21 N2 119.4(8) . . ?
C22 C21 N2 119.9(8) . . ?
C21 C22 N23 119.7(8) . . ?
C21 C22 H22 120.1 . . ?
N23 C22 H22 120.1 . . ?
C24 N23 C22 115.9(7) . . ?
C24 N23 Co1 124.3(6) . 3_655 ?
C22 N23 Co1 119.7(5) . 3_655 ?
N23 C24 C25 124.3(9) . . ?
N23 C24 H24 117.9 . . ?
C25 C24 H24 117.9 . . ?
C24 C25 C26 121.0(9) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C25 C26 C21 118.2(8) . . ?
C25 C26 H26 120.9 . . ?
C21 C26 H26 120.9 . . ?
C2 C1 C6 120.0 . . ?
C2 C1 P1 127.2(9) . . ?
C6 C1 P1 112.8(9) . . ?
C3 C2 C1 120.0 . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 120.0 . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
C2' C1' C6' 120.0 . . ?
C2' C1' P1 117.0(7) . . ?
C6' C1' P1 122.8(7) . . ?
C1' C2' C3' 120.0 . . ?
C1' C2' H2' 120.0 . . ?
C3' C2' H2' 120.0 . . ?
C4' C3' C2' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
C2' C3' H3' 120.0 . . ?
C5' C4' C3' 120.0 . . ?
C5' C4' H4' 120.0 . . ?
C3' C4' H4' 120.0 . . ?
C4' C5' C6' 120.0 . . ?
C4' C5' H5' 120.0 . . ?
C6' C5' H5' 120.0 . . ?
C5' C6' C1' 120.0 . . ?
C5' C6' H6' 120.0 . . ?
C1' C6' H6' 120.0 . . ?

_refine_diff_density_max         0.322
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.066




_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol and water'
_exptl_crystal_preparation       ', Ferroelectric and Dielectric'
####################################################################### 
# 
# 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_compound_Hy-Li_2_sq
_database_code_depnum_ccdc_archive 'CCDC 1543628'
_audit_update_record             
;
2017-04-12 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C128 H200 Co4 Li N41 O75 P8'
_chemical_formula_weight         4003.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_H-M_alt        'I 4 2 2'
_space_group_name_Hall           'I 4 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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   24.507(6)
_cell_length_b                   24.507(6)
_cell_length_c                   17.716(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10640(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2400
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      22.30

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_F_000             4172
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.454
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6115
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51244
_diffrn_reflns_av_unetI/netI     0.1656
_diffrn_reflns_av_R_equivalents  0.2162
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.175
_diffrn_reflns_theta_max         28.384
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6661
_reflns_number_gt                2545
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
'Refined as a 2-component inversion twin., SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1731P)²] 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_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.58(8)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         6661
_refine_ls_number_parameters     173
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.2302
_refine_ls_R_factor_gt           0.0876
_refine_ls_wR_factor_ref         0.3234
_refine_ls_wR_factor_gt          0.2399
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_restrained_S_all      0.960
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.76062(7) 0.5000 0.5000 0.0576(6) Uani 1 2 d S T P . .
O2 O 0.6751(3) 0.5000 0.5000 0.067(2) Uani 1 2 d S T P . .
O3 O 0.8466(4) 0.5000 0.5000 0.096(3) Uani 1 2 d S T P . .
P1 P 0.64090(13) 0.36161(14) 0.28876(15) 0.0681(8) Uani 1 1 d . . . . .
O1 O 0.6097(4) 0.3955(3) 0.3400(4) 0.086(2) Uani 1 1 d . . . . .
N1 N 0.6859(5) 0.3258(5) 0.3361(5) 0.084(3) Uani 1 1 d . . . . .
H1 H 0.6878 0.2909 0.3248 0.101 Uiso 1 1 calc R U . . .
C11 C 0.7211(3) 0.3439(3) 0.3913(4) 0.056(3) Uani 1 1 d G . . . .
C12 C 0.7224(2) 0.3985(2) 0.4125(4) 0.062(3) Uani 1 1 d G . . . .
H12 H 0.6989 0.4240 0.3886 0.074 Uiso 1 1 calc R U . . .
N13 N 0.7581(3) 0.41572(19) 0.4686(4) 0.065(2) Uani 1 1 d G . . . .
C14 C 0.7925(3) 0.3784(3) 0.5035(4) 0.069(3) Uani 1 1 d G . . . .
H14 H 0.8169 0.3902 0.5419 0.083 Uiso 1 1 calc R U . . .
C15 C 0.7912(3) 0.3238(2) 0.4824(4) 0.077(4) Uani 1 1 d G . . . .
H15 H 0.8147 0.2982 0.5063 0.092 Uiso 1 1 calc R U . . .
C16 C 0.7555(3) 0.30652(19) 0.4263(4) 0.070(3) Uani 1 1 d G . . . .
H16 H 0.7546 0.2692 0.4118 0.084 Uiso 1 1 calc R U . . .
N2 N 0.6064(4) 0.3137(4) 0.2447(6) 0.078(3) Uani 1 1 d . . . . .
H2 H 0.6118 0.3108 0.1957 0.094 Uiso 1 1 calc R U . . .
C21 C 0.5693(3) 0.2773(3) 0.2770(4) 0.065(3) Uani 1 1 d G . . . .
C22 C 0.5586(2) 0.2765(2) 0.3540(4) 0.062(3) Uani 1 1 d G . . . .
H22 H 0.5762 0.3018 0.3865 0.075 Uiso 1 1 calc R U . . .
N23 N 0.5223(3) 0.2385(2) 0.3835(3) 0.059(2) Uani 1 1 d G . . . .
C24 C 0.4967(3) 0.2014(2) 0.3359(3) 0.062(2) Uani 1 1 d G . . . .
H24 H 0.4718 0.1754 0.3561 0.075 Uiso 1 1 calc R U . . .
C25 C 0.5074(3) 0.2022(3) 0.2589(3) 0.080(3) Uani 1 1 d G . . . .
H25 H 0.4898 0.1769 0.2264 0.096 Uiso 1 1 calc R U . . .
C26 C 0.5437(3) 0.2402(3) 0.2294(3) 0.078(4) Uani 1 1 d G . . . .
H26 H 0.5510 0.2408 0.1767 0.093 Uiso 1 1 calc R U . . .
C1 C 0.6650(7) 0.4043(7) 0.2204(8) 0.085(7) Uiso 0.62(2) 1 d DG U P A 1
C2 C 0.7116(7) 0.3882(6) 0.1817(9) 0.075(6) Uiso 0.62(2) 1 d DG U P A 1
H2A H 0.7308 0.3564 0.1970 0.090 Uiso 0.62(2) 1 calc R U P A 1
C3 C 0.7302(6) 0.4187(6) 0.1208(8) 0.077(6) Uiso 0.62(2) 1 d DG U P A 1
H3 H 0.7621 0.4077 0.0943 0.092 Uiso 0.62(2) 1 calc R U P A 1
C4 C 0.7021(7) 0.4653(7) 0.0985(8) 0.098(8) Uiso 0.62(2) 1 d DG U P A 1
H4 H 0.7148 0.4861 0.0568 0.117 Uiso 0.62(2) 1 calc R U P A 1
C5 C 0.6555(7) 0.4814(7) 0.1372(10) 0.105(8) Uiso 0.62(2) 1 d DG U P A 1
H5 H 0.6363 0.5132 0.1219 0.126 Uiso 0.62(2) 1 calc R U P A 1
C6 C 0.6369(6) 0.4509(8) 0.1981(10) 0.109(8) Uiso 0.62(2) 1 d DG U P A 1
H6 H 0.6050 0.4619 0.2246 0.131 Uiso 0.62(2) 1 calc R U P A 1
C1' C 0.6799(8) 0.3902(10) 0.2107(11) 0.053(7) Uiso 0.38(2) 1 d DG U P A 2
C2' C 0.7317(9) 0.3745(8) 0.1876(11) 0.058(8) Uiso 0.38(2) 1 d DG U P A 2
H2' H 0.7506 0.3465 0.2140 0.070 Uiso 0.38(2) 1 calc R U P A 2
C3' C 0.7560(8) 0.3998(9) 0.1260(12) 0.065(8) Uiso 0.38(2) 1 d DG U P A 2
H3' H 0.7915 0.3891 0.1102 0.078 Uiso 0.38(2) 1 calc R U P A 2
C4' C 0.7285(10) 0.4408(9) 0.0874(11) 0.075(10) Uiso 0.38(2) 1 d DG U P A 2
H4' H 0.7451 0.4581 0.0453 0.090 Uiso 0.38(2) 1 calc R U P A 2
C5' C 0.6766(9) 0.4564(9) 0.1105(14) 0.083(10) Uiso 0.38(2) 1 d DG U P A 2
H5' H 0.6577 0.4845 0.0842 0.100 Uiso 0.38(2) 1 calc R U P A 2
C6' C 0.6523(7) 0.4311(10) 0.1721(14) 0.098(11) Uiso 0.38(2) 1 d DG U P A 2
H6' H 0.6168 0.4418 0.1879 0.118 Uiso 0.38(2) 1 calc R U P A 2
O4 O 0.6007(6) 0.5000(9) 0.3857(9) 0.087(4) Uiso 0.5 1 d . . P . .
O5 O 0.6129(12) 0.5828(12) 0.499(3) 0.093(10) Uiso 0.25 1 d . . P . .
O6 O 0.5000 0.5000 0.5000 0.098(7) Uiso 1 8 d S . P . .
Li1 Li 0.5000 0.5000 0.401(4) 0.065(16) Uiso 0.5 4 d S . 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
Co1 O2 2.096(8) . ?
Co1 O3 2.107(10) . ?
Co1 N23 2.14(3) 8_666 ?
Co1 N23 2.14(3) 3_655 ?
Co1 N13 2.140(4) 6_566 ?
Co1 N13 2.140(4) . ?
P1 O1 1.448(8) . ?
P1 N1 1.640(10) . ?
P1 N2 1.644(10) . ?
P1 C1 1.706(11) . ?
P1 C1' 1.820(16) . ?
N1 C11 1.378(13) . ?
N1 H1 0.8800 . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C12 N13 1.3900 . ?
C12 H12 0.9500 . ?
N13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C14 H14 0.9500 . ?
C15 C16 1.3900 . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
N2 C21 1.395(11) . ?
N2 H2 0.8800 . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C22 N23 1.3900 . ?
C22 H22 0.9500 . ?
N23 C24 1.3900 . ?
N23 Co1 2.135(5) 4_565 ?
C24 C25 1.3900 . ?
C24 H24 0.9500 . ?
C25 C26 1.3900 . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C2 C3 1.3900 . ?
C2 H2A 0.9500 . ?
C3 C4 1.3900 . ?
C3 H3 0.9500 . ?
C4 C5 1.3900 . ?
C4 H4 0.9500 . ?
C5 C6 1.3900 . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C1' C2' 1.3900 . ?
C1' C6' 1.3900 . ?
C2' C3' 1.3900 . ?
C2' H2' 0.9500 . ?
C3' C4' 1.3900 . ?
C3' H3' 0.9500 . ?
C4' C5' 1.3900 . ?
C4' H4' 0.9500 . ?
C5' C6' 1.3900 . ?
C5' H5' 0.9500 . ?
C6' H6' 0.9500 . ?
O4 Li1 2.482(17) . ?
O5 O5 1.04(5) 7_556 ?
O6 Li1 1.76(7) . ?
O6 Li1 1.76(7) 5_656 ?
Li1 O4 2.482(17) 4_565 ?
Li1 O4 2.482(17) 2_665 ?
Li1 O4 2.482(17) 3_655 ?
Li1 Li1 3.52(13) 5_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O3 180.0 . . ?
O2 Co1 N23 90.6(9) . 8_666 ?
O3 Co1 N23 89.4(9) . 8_666 ?
O2 Co1 N23 90.6(7) . 3_655 ?
O3 Co1 N23 89.4(7) . 3_655 ?
N23 Co1 N23 178.8(15) 8_666 3_655 ?
O2 Co1 N13 88.4(6) . 6_566 ?
O3 Co1 N13 91.6(6) . 6_566 ?
N23 Co1 N13 89.8(10) 8_666 6_566 ?
N23 Co1 N13 90.3(10) 3_655 6_566 ?
O2 Co1 N13 88.36(18) . . ?
O3 Co1 N13 91.64(17) . . ?
N23 Co1 N13 90.3(8) 8_666 . ?
N23 Co1 N13 89.8(8) 3_655 . ?
N13 Co1 N13 176.7(7) 6_566 . ?
O1 P1 N1 110.0(5) . . ?
O1 P1 N2 115.8(6) . . ?
N1 P1 N2 102.0(7) . . ?
O1 P1 C1 106.0(8) . . ?
N1 P1 C1 117.3(8) . . ?
N2 P1 C1 106.2(7) . . ?
O1 P1 C1' 122.2(9) . . ?
N1 P1 C1' 103.9(8) . . ?
N2 P1 C1' 100.6(9) . . ?
C11 N1 P1 127.8(9) . . ?
C11 N1 H1 116.1 . . ?
P1 N1 H1 116.1 . . ?
N1 C11 C12 121.0(6) . . ?
N1 C11 C16 119.0(6) . . ?
C12 C11 C16 120.0 . . ?
C11 C12 N13 120.0 . . ?
C11 C12 H12 120.0 . . ?
N13 C12 H12 120.0 . . ?
C12 N13 C14 120.0 . . ?
C12 N13 Co1 119.8(3) . . ?
C14 N13 Co1 120.2(3) . . ?
C15 C14 N13 120.0 . . ?
C15 C14 H14 120.0 . . ?
N13 C14 H14 120.0 . . ?
C14 C15 C16 120.0 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C11 120.0 . . ?
C15 C16 H16 120.0 . . ?
C11 C16 H16 120.0 . . ?
C21 N2 P1 126.6(7) . . ?
C21 N2 H2 116.7 . . ?
P1 N2 H2 116.7 . . ?
C22 C21 C26 120.0 . . ?
C22 C21 N2 122.4(6) . . ?
C26 C21 N2 117.6(6) . . ?
C21 C22 N23 120.0 . . ?
C21 C22 H22 120.0 . . ?
N23 C22 H22 120.0 . . ?
C24 N23 C22 120.0 . . ?
C24 N23 Co1 118.5(3) . 4_565 ?
C22 N23 Co1 121.3(3) . 4_565 ?
C25 C24 N23 120.0 . . ?
C25 C24 H24 120.0 . . ?
N23 C24 H24 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C21 120.0 . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
C2 C1 C6 120.0 . . ?
C2 C1 P1 117.4(10) . . ?
C6 C1 P1 122.3(10) . . ?
C3 C2 C1 120.0 . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 120.0 . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
C2' C1' C6' 120.0 . . ?
C2' C1' P1 126.7(12) . . ?
C6' C1' P1 113.3(12) . . ?
C3' C2' C1' 120.0 . . ?
C3' C2' H2' 120.0 . . ?
C1' C2' H2' 120.0 . . ?
C2' C3' C4' 120.0 . . ?
C2' C3' H3' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
C3' C4' C5' 120.0 . . ?
C3' C4' H4' 120.0 . . ?
C5' C4' H4' 120.0 . . ?
C6' C5' C4' 120.0 . . ?
C6' C5' H5' 120.0 . . ?
C4' C5' H5' 120.0 . . ?
C5' C6' C1' 120.0 . . ?
C5' C6' H6' 120.0 . . ?
C1' C6' H6' 120.0 . . ?
Li1 O6 Li1 180.000(10) . 5_656 ?
O6 Li1 O4 96.1(16) . 4_565 ?
O6 Li1 O4 96.1(16) . 2_665 ?
O4 Li1 O4 89.3(3) 4_565 2_665 ?
O6 Li1 O4 96.1(16) . 3_655 ?
O4 Li1 O4 168(3) 4_565 3_655 ?
O4 Li1 O4 89.3(3) 2_665 3_655 ?
O6 Li1 O4 96.1(16) . . ?
O4 Li1 O4 89.3(3) 4_565 . ?
O4 Li1 O4 168(3) 2_665 . ?
O4 Li1 O4 89.3(3) 3_655 . ?
O6 Li1 Li1 0.000(4) . 5_656 ?
O4 Li1 Li1 96.1(16) 4_565 5_656 ?
O4 Li1 Li1 96.1(16) 2_665 5_656 ?
O4 Li1 Li1 96.1(16) 3_655 5_656 ?
O4 Li1 Li1 96.1(16) . 5_656 ?

_refine_diff_density_max         0.594
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.092




_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol and water'
_exptl_crystal_preparation       ', Ferroelectric and Dielectric'
####################################################################### 
# 
# 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_compound_Hy-Li_1_sq
_database_code_depnum_ccdc_archive 'CCDC 1543627'
_audit_update_record             
;
2017-04-12 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C128 H183 Li N41 Ni4 O66.50 P8'
_chemical_formula_weight         3849.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_H-M_alt        'I 4 2 2'
_space_group_name_Hall           'I 4 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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   24.222(7)
_cell_length_b                   24.222(7)
_cell_length_c                   17.620(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10337(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2951
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      17.73

_exptl_crystal_description       block
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_F_000             4010
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    0.505
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6869
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            53788
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_av_R_equivalents  0.1493
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.429
_diffrn_reflns_theta_max         28.458
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6535
_reflns_number_gt                2652
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1234P)²] 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_details 
;
 Flack x determined using 846 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.048(17)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         6535
_refine_ls_number_parameters     220
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.1889
_refine_ls_R_factor_gt           0.0693
_refine_ls_wR_factor_ref         0.2468
_refine_ls_wR_factor_gt          0.1823
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.993
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.76043(5) 0.5000 0.5000 0.0740(5) Uani 1 2 d S T P . .
O2 O 0.6737(3) 0.5000 0.5000 0.0743(17) Uani 1 2 d S T P . .
O3 O 0.8471(3) 0.5000 0.5000 0.109(3) Uani 1 2 d S T P . .
P1 P 0.64204(11) 0.36005(11) 0.28961(10) 0.0842(7) Uani 1 1 d . . . . .
O1 O 0.6103(3) 0.3966(3) 0.3372(3) 0.0944(17) Uani 1 1 d . . . . .
N1 N 0.6854(4) 0.3245(4) 0.3384(3) 0.099(2) Uani 1 1 d . . . . .
H1A H 0.6857 0.2888 0.3290 0.119 Uiso 1 1 calc R U . . .
C11 C 0.7238(4) 0.3430(4) 0.3956(4) 0.078(2) Uani 1 1 d . . . . .
C12 C 0.7241(4) 0.3974(4) 0.4153(4) 0.078(2) Uani 1 1 d . . . . .
H12 H 0.7003 0.4225 0.3897 0.094 Uiso 1 1 calc R U . . .
N13 N 0.7591(3) 0.4169(3) 0.4727(4) 0.0776(19) Uani 1 1 d . . . . .
C14 C 0.7935(3) 0.3798(4) 0.4999(6) 0.084(2) Uani 1 1 d . . . . .
H14 H 0.8207 0.3923 0.5348 0.101 Uiso 1 1 calc R U . . .
C15 C 0.7935(4) 0.3273(4) 0.4830(6) 0.097(3) Uani 1 1 d . . . . .
H15 H 0.8173 0.3026 0.5093 0.116 Uiso 1 1 calc R U . . .
C16 C 0.7590(4) 0.3076(4) 0.4272(5) 0.089(3) Uani 1 1 d . . . . .
H16 H 0.7602 0.2701 0.4117 0.107 Uiso 1 1 calc R U . . .
N2 N 0.6080(4) 0.3110(4) 0.2462(4) 0.099(3) Uani 1 1 d . . . . .
H2A H 0.6146 0.3071 0.1974 0.118 Uiso 1 1 calc R U . . .
C21 C 0.5698(4) 0.2749(4) 0.2779(5) 0.080(2) Uani 1 1 d . . . . .
C22 C 0.5556(4) 0.2739(4) 0.3541(5) 0.075(2) Uani 1 1 d . . . . .
H22 H 0.5719 0.3005 0.3869 0.090 Uiso 1 1 calc R U . . .
N23 N 0.5205(3) 0.2380(3) 0.3838(4) 0.079(2) Uani 1 1 d . . . . .
C24 C 0.4932(4) 0.2021(3) 0.3377(4) 0.072(2) Uani 1 1 d . . . . .
H24 H 0.4651 0.1786 0.3569 0.086 Uiso 1 1 calc R U . . .
C25 C 0.5087(5) 0.2013(4) 0.2585(5) 0.098(3) Uani 1 1 d . . . . .
H25 H 0.4934 0.1739 0.2261 0.117 Uiso 1 1 calc R U . . .
C26 C 0.5436(4) 0.2376(4) 0.2300(5) 0.084(2) Uani 1 1 d . . . . .
H26 H 0.5508 0.2382 0.1771 0.101 Uiso 1 1 calc R U . . .
C1 C 0.6661(8) 0.4032(9) 0.2178(11) 0.084(6) Uiso 0.50(2) 1 d D U P A 1
C2 C 0.7153(10) 0.3866(9) 0.1837(10) 0.085(6) Uiso 0.50(2) 1 d D U P A 1
H2 H 0.7349 0.3556 0.2028 0.102 Uiso 0.50(2) 1 calc R U P A 1
C3 C 0.7367(10) 0.4173(9) 0.1181(11) 0.089(6) Uiso 0.50(2) 1 d D U P A 1
H3 H 0.7696 0.4070 0.0924 0.107 Uiso 0.50(2) 1 calc R U P A 1
C4 C 0.7058(10) 0.4613(9) 0.0970(13) 0.097(7) Uiso 0.50(2) 1 d D U P A 1
H4 H 0.7188 0.4814 0.0544 0.116 Uiso 0.50(2) 1 calc R U P A 1
C5 C 0.6578(10) 0.4807(9) 0.1297(11) 0.109(8) Uiso 0.50(2) 1 d D U P A 1
H5 H 0.6397 0.5128 0.1112 0.131 Uiso 0.50(2) 1 calc R U P A 1
C6 C 0.6360(11) 0.4493(10) 0.1943(13) 0.120(8) Uiso 0.50(2) 1 d D U P A 1
H6 H 0.6028 0.4599 0.2191 0.143 Uiso 0.50(2) 1 calc R U P A 1
C1' C 0.6833(9) 0.3889(8) 0.2130(11) 0.075(5) Uiso 0.50(2) 1 d D U P A 2
C2' C 0.7354(10) 0.3709(10) 0.1939(12) 0.097(7) Uiso 0.50(2) 1 d D U P A 2
H2' H 0.7529 0.3416 0.2206 0.116 Uiso 0.50(2) 1 calc R U P A 2
C3' C 0.7626(10) 0.3989(10) 0.1307(11) 0.105(7) Uiso 0.50(2) 1 d D U P A 2
H3' H 0.7983 0.3876 0.1146 0.126 Uiso 0.50(2) 1 calc R U P A 2
C4' C 0.7362(9) 0.4416(9) 0.0949(11) 0.087(6) Uiso 0.50(2) 1 d D U P A 2
H4' H 0.7558 0.4607 0.0563 0.104 Uiso 0.50(2) 1 calc R U P A 2
C5' C 0.6832(11) 0.4590(12) 0.1107(14) 0.118(9) Uiso 0.50(2) 1 d D U P A 2
H5' H 0.6654 0.4872 0.0824 0.141 Uiso 0.50(2) 1 calc R U P A 2
C6' C 0.6565(10) 0.4307(10) 0.1741(12) 0.111(7) Uiso 0.50(2) 1 d D U P A 2
H6' H 0.6203 0.4412 0.1888 0.133 Uiso 0.50(2) 1 calc R U P A 2
O4 O 0.5994(5) 0.5035(7) 0.3861(6) 0.095(3) Uiso 0.5 1 d . . P . .
O5 O 0.6014(8) 0.5796(8) 0.502(2) 0.096(7) Uiso 0.25 1 d . . P . .
O6 O 0.5000 0.5000 0.5000 0.091(4) Uiso 1 8 d S . P . .
Li1 Li 0.5000 0.5000 0.396(3) 0.102(16) Uiso 0.5 4 d S . 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
Ni1 N13 2.070(7) 6_566 ?
Ni1 N13 2.070(7) . ?
Ni1 O3 2.099(7) . ?
Ni1 O2 2.101(6) . ?
Ni1 N23 2.107(7) 8_666 ?
Ni1 N23 2.107(7) 3_655 ?
P1 O1 1.441(6) . ?
P1 N1 1.608(7) . ?
P1 N2 1.635(8) . ?
P1 C1 1.741(17) . ?
P1 C1' 1.819(19) . ?
N1 C11 1.443(12) . ?
N1 H1A 0.8800 . ?
C11 C16 1.330(12) . ?
C11 C12 1.362(13) . ?
C12 N13 1.401(10) . ?
C12 H12 0.9500 . ?
N13 C14 1.317(10) . ?
C14 C15 1.307(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.376(13) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
N2 C21 1.390(11) . ?
N2 H2A 0.8800 . ?
C21 C26 1.390(11) . ?
C21 C22 1.387(12) . ?
C22 N23 1.323(10) . ?
C22 H22 0.9500 . ?
N23 C24 1.361(10) . ?
N23 Ni1 2.107(7) 4_565 ?
C24 C25 1.446(12) . ?
C24 H24 0.9500 . ?
C25 C26 1.318(13) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C1 C2 1.393(19) . ?
C1 C6 1.40(2) . ?
C2 C3 1.469(19) . ?
C2 H2 0.9500 . ?
C3 C4 1.36(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.38(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.467(19) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C1' C2' 1.377(19) . ?
C1' C6' 1.38(2) . ?
C2' C3' 1.462(19) . ?
C2' H2' 0.9500 . ?
C3' C4' 1.37(2) . ?
C3' H3' 0.9500 . ?
C4' C5' 1.38(2) . ?
C4' H4' 0.9500 . ?
C5' C6' 1.46(2) . ?
C5' H5' 0.9500 . ?
C6' H6' 0.9500 . ?
O4 Li1 2.415(12) . ?
O5 O5 0.75(4) 7_556 ?
O6 Li1 1.83(6) 5_656 ?
O6 Li1 1.83(6) . ?
Li1 O4 2.415(12) 2_665 ?
Li1 O4 2.415(12) 4_565 ?
Li1 O4 2.415(12) 3_655 ?

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
N13 Ni1 N13 178.2(4) 6_566 . ?
N13 Ni1 O3 90.9(2) 6_566 . ?
N13 Ni1 O3 90.9(2) . . ?
N13 Ni1 O2 89.1(2) 6_566 . ?
N13 Ni1 O2 89.1(2) . . ?
O3 Ni1 O2 180.0 . . ?
N13 Ni1 N23 90.2(3) 6_566 8_666 ?
N13 Ni1 N23 89.8(3) . 8_666 ?
O3 Ni1 N23 89.00(19) . 8_666 ?
O2 Ni1 N23 91.00(19) . 8_666 ?
N13 Ni1 N23 89.8(3) 6_566 3_655 ?
N13 Ni1 N23 90.2(3) . 3_655 ?
O3 Ni1 N23 89.00(19) . 3_655 ?
O2 Ni1 N23 91.00(19) . 3_655 ?
N23 Ni1 N23 178.0(4) 8_666 3_655 ?
O1 P1 N1 111.5(3) . . ?
O1 P1 N2 116.7(5) . . ?
N1 P1 N2 101.0(5) . . ?
O1 P1 C1 103.5(8) . . ?
N1 P1 C1 119.5(8) . . ?
N2 P1 C1 105.3(8) . . ?
O1 P1 C1' 119.3(8) . . ?
N1 P1 C1' 104.1(7) . . ?
N2 P1 C1' 102.0(8) . . ?
C11 N1 P1 128.9(8) . . ?
C11 N1 H1A 115.6 . . ?
P1 N1 H1A 115.6 . . ?
C16 C11 C12 120.9(8) . . ?
C16 C11 N1 120.2(9) . . ?
C12 C11 N1 118.8(9) . . ?
C11 C12 N13 120.8(8) . . ?
C11 C12 H12 119.6 . . ?
N13 C12 H12 119.6 . . ?
C14 N13 C12 114.6(8) . . ?
C14 N13 Ni1 124.7(6) . . ?
C12 N13 Ni1 120.3(6) . . ?
C15 C14 N13 125.5(9) . . ?
C15 C14 H14 117.3 . . ?
N13 C14 H14 117.3 . . ?
C14 C15 C16 120.0(9) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C11 C16 C15 117.7(9) . . ?
C11 C16 H16 121.2 . . ?
C15 C16 H16 121.2 . . ?
C21 N2 P1 127.2(6) . . ?
C21 N2 H2A 116.4 . . ?
P1 N2 H2A 116.4 . . ?
N2 C21 C26 118.0(8) . . ?
N2 C21 C22 124.4(8) . . ?
C26 C21 C22 117.6(9) . . ?
N23 C22 C21 123.6(9) . . ?
N23 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
C22 N23 C24 119.8(7) . . ?
C22 N23 Ni1 121.6(5) . 4_565 ?
C24 N23 Ni1 118.4(6) . 4_565 ?
N23 C24 C25 117.3(9) . . ?
N23 C24 H24 121.4 . . ?
C25 C24 H24 121.4 . . ?
C26 C25 C24 121.6(8) . . ?
C26 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
C25 C26 C21 119.7(9) . . ?
C25 C26 H26 120.1 . . ?
C21 C26 H26 120.1 . . ?
C2 C1 C6 123.3(18) . . ?
C2 C1 P1 115.3(14) . . ?
C6 C1 P1 121.3(15) . . ?
C1 C2 C3 119.7(19) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C4 C3 C2 114.7(19) . . ?
C4 C3 H3 122.6 . . ?
C2 C3 H3 122.6 . . ?
C3 C4 C5 128(2) . . ?
C3 C4 H4 115.9 . . ?
C5 C4 H4 115.9 . . ?
C4 C5 C6 116.8(19) . . ?
C4 C5 H5 121.6 . . ?
C6 C5 H5 121.6 . . ?
C1 C6 C5 117(2) . . ?
C1 C6 H6 121.4 . . ?
C5 C6 H6 121.4 . . ?
C2' C1' C6' 122.7(19) . . ?
C2' C1' P1 124.3(13) . . ?
C6' C1' P1 113.0(15) . . ?
C1' C2' C3' 117(2) . . ?
C1' C2' H2' 121.6 . . ?
C3' C2' H2' 121.6 . . ?
C4' C3' C2' 119(2) . . ?
C4' C3' H3' 120.3 . . ?
C2' C3' H3' 120.3 . . ?
C3' C4' C5' 125(2) . . ?
C3' C4' H4' 117.6 . . ?
C5' C4' H4' 117.6 . . ?
C4' C5' C6' 115(2) . . ?
C4' C5' H5' 122.5 . . ?
C6' C5' H5' 122.5 . . ?
C1' C6' C5' 121(2) . . ?
C1' C6' H6' 119.5 . . ?
C5' C6' H6' 119.5 . . ?
Li1 O6 Li1 180.0 5_656 . ?
O6 Li1 O4 94.2(15) . 2_665 ?
O6 Li1 O4 94.2(15) . 4_565 ?
O4 Li1 O4 89.7(2) 2_665 4_565 ?
O6 Li1 O4 94.2(15) . 3_655 ?
O4 Li1 O4 89.7(2) 2_665 3_655 ?
O4 Li1 O4 172(3) 4_565 3_655 ?
O6 Li1 O4 94.2(15) . . ?
O4 Li1 O4 172(3) 2_665 . ?
O4 Li1 O4 89.7(2) 4_565 . ?
O4 Li1 O4 89.7(2) 3_655 . ?

_refine_diff_density_max         0.544
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.061


