# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_exp_3649
_database_code_depnum_ccdc_archive 'CCDC 1913012'
loop_
_audit_author_name
_audit_author_address
'Mingjun Xia'
;Technical Institute of Physics and Chemistry
China
;
_audit_update_record             
;
2019-04-30 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H16 Ca K2 N12 O16'
_chemical_formula_weight         702.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   10.6818(3)
_cell_length_b                   16.2953(4)
_cell_length_c                   7.0758(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.574(3)
_cell_angle_gamma                90.00
_cell_volume                     1214.48(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             716
_exptl_absorpt_coefficient_mu    6.279
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5553
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         5.00
_diffrn_reflns_theta_max         74.39
_reflns_number_total             1279
_reflns_number_gt                1143
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1312P)²+0.2693P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1279
_refine_ls_number_parameters     113
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1732
_refine_ls_wR_factor_gt          0.1482
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.145
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.13712(8) 0.5000 0.77959(10) 0.0389(3) Uani 1 2 d S . .
Ca1 Ca 0.5000 0.5000 1.0000 0.0361(4) Uani 1 4 d S . .
O1 O 0.5000 0.10436(14) 1.0000 0.0347(6) Uani 1 2 d S . .
O2 O 0.6906(3) 0.5000 0.8661(4) 0.0367(6) Uani 1 2 d SD . .
O3 O 0.6066(3) 0.5000 1.3251(4) 0.0409(7) Uani 1 2 d SD . .
O5 O 0.30171(15) 0.34603(10) 0.8273(2) 0.0301(5) Uani 1 1 d . . .
O4 O 0.0000 0.38943(15) 0.5000 0.0347(6) Uani 1 2 d S . .
O6 O 0.19636(15) 0.14871(9) 0.6797(2) 0.0291(5) Uani 1 1 d . . .
N1 N 0.5000 0.35209(15) 0.0000 0.0233(6) Uani 1 2 d S . .
N2 N 0.0000 0.14156(15) 0.5000 0.0232(6) Uani 1 2 d S . .
N3 N 0.40067(17) 0.22532(11) 0.9090(2) 0.0244(5) Uani 1 1 d . . .
H3 H 0.3361 0.1997 0.8476 0.029 Uiso 1 1 calc R . .
N4 N 0.09915(17) 0.26851(11) 0.5916(2) 0.0240(5) Uani 1 1 d . . .
H4 H 0.1643 0.2939 0.6520 0.029 Uiso 1 1 calc R . .
C1 C 0.39811(19) 0.31027(13) 0.9102(3) 0.0216(5) Uani 1 1 d . . .
C2 C 0.10029(19) 0.18386(13) 0.5924(3) 0.0210(5) Uani 1 1 d . . .
C3 C 0.5000 0.18018(19) 0.0000 0.0231(6) Uani 1 2 d S . .
C4 C 0.0000 0.31424(18) 0.5000 0.0223(6) Uani 1 2 d S . .
H3O H 0.589(3) 0.4577(14) 1.386(4) 0.033 Uiso 1 1 d D . .
H2O H 0.700(3) 0.5414(14) 0.798(3) 0.033 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O2 2.853(3) 5_667 ?
K1 O1 2.8688(15) 7_557 ?
K1 O1 2.8688(15) 3_455 ?
K1 O4 2.8881(16) . ?
K1 O4 2.8881(16) 5_566 ?
K1 O3 2.952(3) 5_667 ?
K1 O5 3.0500(16) 6_565 ?
K1 O5 3.0500(16) . ?
K1 Ca1 3.9302(8) . ?
K1 K1 4.5145(15) 5_566 ?
K1 K1 4.6207(16) 5_567 ?
Ca1 O2 2.384(3) 5_667 ?
Ca1 O2 2.384(3) . ?
Ca1 O3 2.391(3) 5_667 ?
Ca1 O3 2.391(3) . ?
Ca1 N1 2.410(2) 1_556 ?
Ca1 N1 2.410(2) 5_666 ?
Ca1 K1 3.9302(8) 5_667 ?
O1 C3 1.235(4) 1_556 ?
O1 K1 2.8688(15) 7_557 ?
O1 K1 2.8688(15) 3_545 ?
O2 K1 2.853(3) 5_667 ?
O3 K1 2.952(3) 5_667 ?
O5 C1 1.242(3) . ?
O4 C4 1.225(4) . ?
O4 K1 2.8881(16) 5_566 ?
O6 C2 1.246(3) . ?
N1 C1 1.350(2) 1_554 ?
N1 C1 1.350(2) 2_656 ?
N1 Ca1 2.410(2) 1_554 ?
N2 C2 1.348(2) . ?
N2 C2 1.348(2) 2_556 ?
N3 C3 1.362(2) 1_556 ?
N3 C1 1.385(3) . ?
N4 C4 1.367(2) . ?
N4 C2 1.379(3) . ?
C1 N1 1.350(2) 1_556 ?
C3 O1 1.235(4) 1_554 ?
C3 N3 1.362(2) 2_656 ?
C3 N3 1.362(2) 1_554 ?
C4 N4 1.367(2) 2_556 ?

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 K1 O1 80.53(5) 5_667 7_557 ?
O2 K1 O1 80.53(5) 5_667 3_455 ?
O1 K1 O1 72.71(8) 7_557 3_455 ?
O2 K1 O4 141.40(4) 5_667 . ?
O1 K1 O4 75.87(4) 7_557 . ?
O1 K1 O4 119.71(4) 3_455 . ?
O2 K1 O4 141.40(4) 5_667 5_566 ?
O1 K1 O4 119.71(4) 7_557 5_566 ?
O1 K1 O4 75.87(4) 3_455 5_566 ?
O4 K1 O4 77.19(8) . 5_566 ?
O2 K1 O3 74.38(8) 5_667 5_667 ?
O1 K1 O3 135.64(5) 7_557 5_667 ?
O1 K1 O3 135.64(5) 3_455 5_667 ?
O4 K1 O3 102.35(5) . 5_667 ?
O4 K1 O3 102.35(5) 5_566 5_667 ?
O2 K1 O5 68.09(4) 5_667 6_565 ?
O1 K1 O5 139.86(5) 7_557 6_565 ?
O1 K1 O5 77.83(5) 3_455 6_565 ?
O4 K1 O5 143.74(5) . 6_565 ?
O4 K1 O5 77.29(5) 5_566 6_565 ?
O3 K1 O5 59.09(4) 5_667 6_565 ?
O2 K1 O5 68.09(4) 5_667 . ?
O1 K1 O5 77.83(5) 7_557 . ?
O1 K1 O5 139.86(5) 3_455 . ?
O4 K1 O5 77.29(5) . . ?
O4 K1 O5 143.74(5) 5_566 . ?
O3 K1 O5 59.09(4) 5_667 . ?
O5 K1 O5 110.70(7) 6_565 . ?
O2 K1 Ca1 37.03(6) 5_667 . ?
O1 K1 Ca1 110.08(2) 7_557 . ?
O1 K1 Ca1 110.08(2) 3_455 . ?
O4 K1 Ca1 128.77(3) . . ?
O4 K1 Ca1 128.77(3) 5_566 . ?
O3 K1 Ca1 37.36(6) 5_667 . ?
O5 K1 Ca1 56.20(3) 6_565 . ?
O5 K1 Ca1 56.20(3) . . ?
O2 K1 K1 179.73(7) 5_667 5_566 ?
O1 K1 K1 99.26(3) 7_557 5_566 ?
O1 K1 K1 99.26(3) 3_455 5_566 ?
O4 K1 K1 38.60(4) . 5_566 ?
O4 K1 K1 38.60(4) 5_566 5_566 ?
O3 K1 K1 105.89(6) 5_667 5_566 ?
O5 K1 K1 112.03(4) 6_565 5_566 ?
O5 K1 K1 112.03(4) . 5_566 ?
Ca1 K1 K1 143.24(3) . 5_566 ?
O2 K1 K1 78.21(6) 5_667 5_567 ?
O1 K1 K1 36.36(4) 7_557 5_567 ?
O1 K1 K1 36.36(4) 3_455 5_567 ?
O4 K1 K1 98.98(2) . 5_567 ?
O4 K1 K1 98.98(2) 5_566 5_567 ?
O3 K1 K1 152.59(7) 5_667 5_567 ?
O5 K1 K1 110.11(4) 6_565 5_567 ?
O5 K1 K1 110.11(4) . 5_567 ?
Ca1 K1 K1 115.23(2) . 5_567 ?
K1 K1 K1 101.52(3) 5_566 5_567 ?
O2 Ca1 O2 180.0 5_667 . ?
O2 Ca1 O3 94.64(10) 5_667 5_667 ?
O2 Ca1 O3 85.36(10) . 5_667 ?
O2 Ca1 O3 85.36(10) 5_667 . ?
O2 Ca1 O3 94.64(10) . . ?
O3 Ca1 O3 180.000(1) 5_667 . ?
O2 Ca1 N1 90.000(1) 5_667 1_556 ?
O2 Ca1 N1 90.0 . 1_556 ?
O3 Ca1 N1 90.0 5_667 1_556 ?
O3 Ca1 N1 90.0 . 1_556 ?
O2 Ca1 N1 90.0 5_667 5_666 ?
O2 Ca1 N1 90.0 . 5_666 ?
O3 Ca1 N1 90.0 5_667 5_666 ?
O3 Ca1 N1 90.0 . 5_666 ?
N1 Ca1 N1 180.0 1_556 5_666 ?
O2 Ca1 K1 133.89(7) 5_667 5_667 ?
O2 Ca1 K1 46.11(7) . 5_667 ?
O3 Ca1 K1 131.47(7) 5_667 5_667 ?
O3 Ca1 K1 48.53(7) . 5_667 ?
N1 Ca1 K1 90.0 1_556 5_667 ?
N1 Ca1 K1 90.0 5_666 5_667 ?
O2 Ca1 K1 46.11(7) 5_667 . ?
O2 Ca1 K1 133.89(7) . . ?
O3 Ca1 K1 48.53(7) 5_667 . ?
O3 Ca1 K1 131.47(7) . . ?
N1 Ca1 K1 90.0 1_556 . ?
N1 Ca1 K1 90.0 5_666 . ?
K1 Ca1 K1 180.0 5_667 . ?
C3 O1 K1 126.36(4) 1_556 7_557 ?
C3 O1 K1 126.36(4) 1_556 3_545 ?
K1 O1 K1 107.29(8) 7_557 3_545 ?
Ca1 O2 K1 96.86(9) . 5_667 ?
Ca1 O3 K1 94.11(8) . 5_667 ?
C1 O5 K1 148.81(14) . . ?
C4 O4 K1 128.60(4) . . ?
C4 O4 K1 128.60(4) . 5_566 ?
K1 O4 K1 102.81(8) . 5_566 ?
C1 N1 C1 119.4(3) 1_554 2_656 ?
C1 N1 Ca1 120.31(13) 1_554 1_554 ?
C1 N1 Ca1 120.31(13) 2_656 1_554 ?
C2 N2 C2 118.5(3) . 2_556 ?
C3 N3 C1 123.50(19) 1_556 . ?
C4 N4 C2 123.55(19) . . ?
O5 C1 N1 121.7(2) . 1_556 ?
O5 C1 N3 118.80(19) . . ?
N1 C1 N3 119.49(19) 1_556 . ?
O6 C2 N2 121.9(2) . . ?
O6 C2 N4 117.89(18) . . ?
N2 C2 N4 120.23(18) . . ?
O1 C3 N3 122.70(13) 1_554 2_656 ?
O1 C3 N3 122.70(13) 1_554 1_554 ?
N3 C3 N3 114.6(3) 2_656 1_554 ?
O4 C4 N4 123.04(13) . 2_556 ?
O4 C4 N4 123.04(13) . . ?
N4 C4 N4 113.9(3) 2_556 . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        74.39
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.892
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.125
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1913013'
loop_
_audit_author_name
_audit_author_address
'Mingjun Xia'
;Technical Institute of Physics and Chemistry
China
;
_audit_update_record             
;
2019-04-30 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H16 K2 Mg N12 O16'
_chemical_formula_weight         686.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Mg Mg 0.0486 0.0363 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   11.7623(7)
_cell_length_b                   15.9722(9)
_cell_length_c                   6.9802(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.876(6)
_cell_angle_gamma                90.00
_cell_volume                     1169.72(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             700
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6723
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         26.37
_reflns_number_total             1242
_reflns_number_gt                1126
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0838P)²+0.2476P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1242
_refine_ls_number_parameters     115
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0414
_refine_ls_wR_factor_ref         0.1106
_refine_ls_wR_factor_gt          0.1073
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.14366(5) 0.5000 0.86569(9) 0.0276(2) Uani 1 2 d S . .
Mg1 Mg 0.5000 0.5000 1.0000 0.0160(3) Uani 1 4 d S . .
O1 O 0.5000 0.10722(10) 1.0000 0.0278(4) Uani 1 2 d S . .
O2 O 0.59080(16) 0.5000 0.7978(3) 0.0218(4) Uani 1 2 d SD . .
O3 O 0.67303(16) 0.5000 1.2864(3) 0.0223(4) Uani 1 2 d SD . .
O5 O 0.29957(10) 0.35173(7) 0.9713(2) 0.0209(3) Uani 1 1 d . . .
O4 O 0.0000 0.39332(11) 0.5000 0.0286(4) Uani 1 2 d S . .
O6 O 0.19564(10) 0.14781(7) 0.5111(2) 0.0219(3) Uani 1 1 d . . .
N1 N 0.5000 0.36050(11) 1.0000 0.0144(4) Uani 1 2 d S . .
N2 N 0.0000 0.14074(12) 0.5000 0.0167(4) Uani 1 2 d S . .
N3 N 0.40005(12) 0.23039(8) 0.9882(2) 0.0174(3) Uani 1 1 d . . .
H3 H 0.3344 0.2043 0.9818 0.021 Uiso 1 1 calc R . .
N4 N 0.09928(12) 0.27025(8) 0.5076(2) 0.0183(3) Uani 1 1 d . . .
H4 H 0.1649 0.2962 0.5137 0.022 Uiso 1 1 calc R . .
C1 C 0.39699(13) 0.31710(10) 0.9858(2) 0.0139(3) Uani 1 1 d . . .
C2 C 0.10047(14) 0.18374(10) 0.5060(2) 0.0150(3) Uani 1 1 d . . .
C3 C 0.5000 0.18349(14) 1.0000 0.0164(5) Uani 1 2 d S . .
C4 C 0.0000 0.31711(14) 0.5000 0.0171(5) Uani 1 2 d S . .
H3O H 0.685(3) 0.5415(14) 1.371(4) 0.051(7) Uiso 1 1 d D . .
H2O H 0.573(2) 0.5424(12) 0.717(4) 0.039(6) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O3 2.8007(18) 5_667 ?
K1 O1 2.8459(11) 3_455 ?
K1 O1 2.8459(11) 7_557 ?
K1 O5 2.8796(12) 6_565 ?
K1 O5 2.8796(12) . ?
K1 O4 2.8939(11) . ?
K1 O4 2.8939(11) 5_566 ?
K1 O2 2.9393(18) 5_667 ?
K1 Mg1 3.8592(5) . ?
K1 K1 4.5461(10) 5_567 ?
K1 K1 4.6782(12) 5_566 ?
Mg1 O3 2.1117(18) . ?
Mg1 O3 2.1117(18) 5_667 ?
Mg1 O2 2.1203(17) . ?
Mg1 O2 2.1203(17) 5_667 ?
Mg1 N1 2.2281(18) 5_667 ?
Mg1 N1 2.2281(18) . ?
Mg1 K1 3.8592(5) 5_667 ?
O1 C3 1.218(3) . ?
O1 K1 2.8459(11) 3_545 ?
O1 K1 2.8459(11) 7_557 ?
O2 K1 2.9393(18) 5_667 ?
O3 K1 2.8007(18) 5_667 ?
O5 C1 1.2347(19) . ?
O4 C4 1.217(3) . ?
O4 K1 2.8939(11) 5_566 ?
O6 C2 1.2440(19) . ?
N1 C1 1.3601(17) . ?
N1 C1 1.3601(17) 2_657 ?
N2 C2 1.3510(18) 2_556 ?
N2 C2 1.3510(18) . ?
N3 C3 1.3648(18) . ?
N3 C1 1.385(2) . ?
N4 C4 1.3679(18) . ?
N4 C2 1.382(2) . ?
C3 N3 1.3648(18) 2_657 ?
C4 N4 1.3679(18) 2_556 ?

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 K1 O1 142.97(3) 5_667 3_455 ?
O3 K1 O1 142.97(3) 5_667 7_557 ?
O1 K1 O1 73.99(5) 3_455 7_557 ?
O3 K1 O5 65.59(3) 5_667 6_565 ?
O1 K1 O5 79.92(3) 3_455 6_565 ?
O1 K1 O5 144.56(4) 7_557 6_565 ?
O3 K1 O5 65.59(3) 5_667 . ?
O1 K1 O5 144.56(4) 3_455 . ?
O1 K1 O5 79.92(3) 7_557 . ?
O5 K1 O5 110.65(5) 6_565 . ?
O3 K1 O4 84.74(3) 5_667 . ?
O1 K1 O4 116.61(3) 3_455 . ?
O1 K1 O4 74.89(2) 7_557 . ?
O5 K1 O4 139.50(4) 6_565 . ?
O5 K1 O4 77.99(4) . . ?
O3 K1 O4 84.74(3) 5_667 5_566 ?
O1 K1 O4 74.89(2) 3_455 5_566 ?
O1 K1 O4 116.61(3) 7_557 5_566 ?
O5 K1 O4 77.99(4) 6_565 5_566 ?
O5 K1 O4 139.50(4) . 5_566 ?
O4 K1 O4 72.14(6) . 5_566 ?
O3 K1 O2 65.22(5) 5_667 5_667 ?
O1 K1 O2 108.15(3) 3_455 5_667 ?
O1 K1 O2 108.15(3) 7_557 5_667 ?
O5 K1 O2 58.11(3) 6_565 5_667 ?
O5 K1 O2 58.11(3) . 5_667 ?
O4 K1 O2 133.69(3) . 5_667 ?
O4 K1 O2 133.69(3) 5_566 5_667 ?
O3 K1 Mg1 32.27(4) 5_667 . ?
O1 K1 Mg1 131.40(2) 3_455 . ?
O1 K1 Mg1 131.40(2) 7_557 . ?
O5 K1 Mg1 56.07(2) 6_565 . ?
O5 K1 Mg1 56.07(2) . . ?
O4 K1 Mg1 110.564(15) . . ?
O4 K1 Mg1 110.564(15) 5_566 . ?
O2 K1 Mg1 32.95(3) 5_667 . ?
O3 K1 K1 178.17(4) 5_667 5_567 ?
O1 K1 K1 36.99(3) 3_455 5_567 ?
O1 K1 K1 36.99(3) 7_557 5_567 ?
O5 K1 K1 113.61(3) 6_565 5_567 ?
O5 K1 K1 113.61(3) . 5_567 ?
O4 K1 K1 96.734(16) . 5_567 ?
O4 K1 K1 96.734(16) 5_566 5_567 ?
O2 K1 K1 112.95(4) 5_667 5_567 ?
Mg1 K1 K1 145.90(2) . 5_567 ?
O3 K1 K1 83.49(4) 5_667 5_566 ?
O1 K1 K1 96.654(15) 3_455 5_566 ?
O1 K1 K1 96.654(15) 7_557 5_566 ?
O5 K1 K1 109.98(3) 6_565 5_566 ?
O5 K1 K1 109.98(3) . 5_566 ?
O4 K1 K1 36.07(3) . 5_566 ?
O4 K1 K1 36.07(3) 5_566 5_566 ?
O2 K1 K1 148.71(4) 5_667 5_566 ?
Mg1 K1 K1 115.759(18) . 5_566 ?
K1 K1 K1 98.34(2) 5_567 5_566 ?
O3 Mg1 O3 180.0 . 5_667 ?
O3 Mg1 O2 94.02(7) . . ?
O3 Mg1 O2 85.98(7) 5_667 . ?
O3 Mg1 O2 85.98(7) . 5_667 ?
O3 Mg1 O2 94.02(7) 5_667 5_667 ?
O2 Mg1 O2 180.000(1) . 5_667 ?
O3 Mg1 N1 90.0 . 5_667 ?
O3 Mg1 N1 90.0 5_667 5_667 ?
O2 Mg1 N1 90.0 . 5_667 ?
O2 Mg1 N1 90.0 5_667 5_667 ?
O3 Mg1 N1 90.0 . . ?
O3 Mg1 N1 90.0 5_667 . ?
O2 Mg1 N1 90.0 . . ?
O2 Mg1 N1 90.0 5_667 . ?
N1 Mg1 N1 180.0 5_667 . ?
O3 Mg1 K1 134.92(5) . . ?
O3 Mg1 K1 45.08(5) 5_667 . ?
O2 Mg1 K1 131.06(5) . . ?
O2 Mg1 K1 48.94(5) 5_667 . ?
N1 Mg1 K1 90.0 5_667 . ?
N1 Mg1 K1 90.0 . . ?
O3 Mg1 K1 45.08(5) . 5_667 ?
O3 Mg1 K1 134.92(5) 5_667 5_667 ?
O2 Mg1 K1 48.94(5) . 5_667 ?
O2 Mg1 K1 131.06(5) 5_667 5_667 ?
N1 Mg1 K1 90.0 5_667 5_667 ?
N1 Mg1 K1 90.0 . 5_667 ?
K1 Mg1 K1 180.000(16) . 5_667 ?
C3 O1 K1 126.99(3) . 3_545 ?
C3 O1 K1 126.99(3) . 7_557 ?
K1 O1 K1 106.01(5) 3_545 7_557 ?
Mg1 O2 K1 98.11(6) . 5_667 ?
Mg1 O3 K1 102.65(7) . 5_667 ?
C1 O5 K1 148.16(10) . . ?
C4 O4 K1 126.07(3) . . ?
C4 O4 K1 126.07(3) . 5_566 ?
K1 O4 K1 107.86(6) . 5_566 ?
C1 N1 C1 118.71(19) . 2_657 ?
C1 N1 Mg1 120.64(9) . . ?
C1 N1 Mg1 120.64(9) 2_657 . ?
C2 N2 C2 118.89(19) 2_556 . ?
C3 N3 C1 124.50(14) . . ?
C4 N4 C2 123.94(14) . . ?
O5 C1 N1 122.74(15) . . ?
O5 C1 N3 117.84(13) . . ?
N1 C1 N3 119.43(13) . . ?
O6 C2 N2 121.97(16) . . ?
O6 C2 N4 118.25(14) . . ?
N2 C2 N4 119.78(14) . . ?
O1 C3 N3 123.29(10) . 2_657 ?
O1 C3 N3 123.29(10) . . ?
N3 C3 N3 113.4(2) 2_657 . ?
O4 C4 N4 123.18(10) . . ?
O4 C4 N4 123.18(10) . 2_556 ?
N4 C4 N4 113.6(2) . 2_556 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.610
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.091
####################################################################### 
# 
# 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_exp_3941_pl
_database_code_depnum_ccdc_archive 'CCDC 1913015'
loop_
_audit_author_name
_audit_author_address
'Mingjun Xia'
;Technical Institute of Physics and Chemistry
China
;
_audit_update_record             
;
2019-04-30 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H28 Cs2 Mg N12 O22'
_chemical_formula_weight         982.59

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'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.7827(2)
_cell_length_b                   11.4995(3)
_cell_length_c                   11.8268(3)
_cell_angle_alpha                113.871(3)
_cell_angle_beta                 102.466(2)
_cell_angle_gamma                102.313(2)
_cell_volume                     775.58(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.104
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             482
_exptl_absorpt_coefficient_mu    2.480
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21393
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         26.37
_reflns_number_total             3169
_reflns_number_gt                2944
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0275P)²+0.2256P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3169
_refine_ls_number_parameters     253
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0212
_refine_ls_wR_factor_ref         0.0543
_refine_ls_wR_factor_gt          0.0532
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.075
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs1 Cs 0.33094(3) 0.554220(15) 0.169879(15) 0.03378(7) Uani 1 1 d . . .
Mg1 Mg 0.5000 0.5000 0.5000 0.0211(2) Uani 1 2 d S . .
C1 C 0.8555(4) 1.1921(2) 0.5533(2) 0.0242(5) Uani 1 1 d . . .
C2 C 0.8487(4) 1.1887(2) 0.3543(2) 0.0234(5) Uani 1 1 d . . .
C3 C 0.7325(4) 0.9764(2) 0.3582(2) 0.0271(5) Uani 1 1 d . . .
C4 C 0.2595(4) 1.0221(2) 0.2424(2) 0.0253(5) Uani 1 1 d . . .
C5 C 0.1600(4) 0.8072(2) 0.0486(2) 0.0258(5) Uani 1 1 d . . .
C6 C 0.2618(4) 1.0207(2) 0.0465(2) 0.0269(5) Uani 1 1 d . . .
N1 N 0.7766(3) 1.05338(19) 0.48899(19) 0.0276(4) Uani 1 1 d . . .
H1 H 0.7538 1.0127 0.5344 0.033 Uiso 1 1 calc R . .
N2 N 0.7680(3) 1.04940(19) 0.29286(18) 0.0261(4) Uani 1 1 d . . .
H2 H 0.7385 1.0062 0.2092 0.031 Uiso 1 1 calc R . .
N3 N 0.8948(3) 1.25927(19) 0.48500(18) 0.0258(4) Uani 1 1 d . . .
N4 N 0.2953(3) 1.09073(19) 0.17619(18) 0.0269(4) Uani 1 1 d . . .
N5 N 0.1900(3) 0.88270(19) 0.17823(18) 0.0272(4) Uani 1 1 d . . .
H5 H 0.1643 0.8412 0.2225 0.033 Uiso 1 1 calc R . .
N6 N 0.1941(3) 0.88115(19) -0.01418(19) 0.0285(4) Uani 1 1 d . . .
H6 H 0.1723 0.8387 -0.0970 0.034 Uiso 1 1 calc R . .
O1 O 0.6693(4) 0.85366(17) 0.30487(18) 0.0446(5) Uani 1 1 d . . .
O2 O 0.6381(5) 0.6896(2) 0.0447(3) 0.0660(8) Uani 1 1 d D . .
O3 O 0.8909(3) 1.25250(17) 0.67335(16) 0.0336(4) Uani 1 1 d . . .
O4 O 0.1968(3) 0.49785(18) 0.41625(19) 0.0330(4) Uani 1 1 d D . .
O5 O 0.2911(3) 1.07930(17) 0.36271(16) 0.0348(4) Uani 1 1 d . . .
O6 O 0.4907(3) 0.37004(18) 0.31499(18) 0.0324(4) Uani 1 1 d D . .
O7 O 0.8803(3) 1.24519(17) 0.28670(16) 0.0322(4) Uani 1 1 d . . .
O8 O 0.3647(3) 0.33963(16) 0.52836(17) 0.0277(4) Uani 1 1 d D . .
O9 O 0.1077(3) 0.68405(17) -0.00441(17) 0.0343(4) Uani 1 1 d . . .
O10 O 0.2896(4) 1.07699(18) -0.02145(17) 0.0426(5) Uani 1 1 d . . .
O11 O 0.7702(4) 0.4925(2) 0.2170(2) 0.0450(5) Uani 1 1 d D . .
H8A H 0.346(6) 0.261(2) 0.475(3) 0.068 Uiso 1 1 d D . .
H4A H 0.094(5) 0.427(3) 0.376(3) 0.068 Uiso 1 1 d D . .
H4B H 0.154(6) 0.561(3) 0.446(4) 0.068 Uiso 1 1 d D . .
H6A H 0.435(6) 0.2876(19) 0.274(3) 0.068 Uiso 1 1 d D . .
H6B H 0.586(5) 0.383(4) 0.285(4) 0.068 Uiso 1 1 d D . .
H11A H 0.862(5) 0.570(2) 0.251(4) 0.068 Uiso 1 1 d D . .
H2A H 0.650(6) 0.744(3) 0.014(4) 0.068 Uiso 1 1 d D . .
H8B H 0.247(4) 0.341(4) 0.537(4) 0.068 Uiso 1 1 d D . .
H2B H 0.689(6) 0.736(3) 0.1271(19) 0.068 Uiso 1 1 d D . .
H11B H 0.794(6) 0.438(3) 0.155(3) 0.068 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cs1 O2 3.012(2) 2_665 ?
Cs1 O9 3.1396(19) 2_565 ?
Cs1 O3 3.1521(18) 2_676 ?
Cs1 O11 3.193(2) . ?
Cs1 O1 3.2048(18) . ?
Cs1 O8 3.2723(17) 2_666 ?
Cs1 O2 3.282(2) . ?
Cs1 O9 3.2983(18) . ?
Cs1 O6 3.4240(19) . ?
Cs1 O4 3.487(2) . ?
Cs1 Mg1 4.15805(18) . ?
Cs1 Cs1 4.8605(4) 2_565 ?
Cs1 H6B 3.36(4) . ?
Cs1 H11A 3.47(4) . ?
Cs1 H2B 3.12(4) . ?
Mg1 O8 2.0658(16) 2_666 ?
Mg1 O8 2.0658(16) . ?
Mg1 O6 2.0687(17) 2_666 ?
Mg1 O6 2.0687(17) . ?
Mg1 O4 2.0711(18) 2_666 ?
Mg1 O4 2.0711(18) . ?
Mg1 Cs1 4.15805(18) 2_666 ?
C1 O3 1.241(3) . ?
C1 N3 1.353(3) . ?
C1 N1 1.374(3) . ?
C2 O7 1.242(3) . ?
C2 N3 1.347(3) . ?
C2 N2 1.380(3) . ?
C3 O1 1.216(3) . ?
C3 N1 1.358(3) . ?
C3 N2 1.371(3) . ?
C4 O5 1.247(3) . ?
C4 N4 1.339(3) . ?
C4 N5 1.381(3) . ?
C5 O9 1.223(3) . ?
C5 N6 1.353(3) . ?
C5 N5 1.363(3) . ?
C6 O10 1.239(3) . ?
C6 N4 1.351(3) . ?
C6 N6 1.383(3) . ?
N1 H1 0.8600 . ?
N2 H2 0.8600 . ?
N5 H5 0.8600 . ?
N6 H6 0.8600 . ?
O2 Cs1 3.012(2) 2_665 ?
O2 H2A 0.838(18) . ?
O2 H2B 0.841(19) . ?
O3 Cs1 3.1521(18) 2_676 ?
O4 H4A 0.824(19) . ?
O4 H4B 0.817(19) . ?
O6 H6A 0.820(19) . ?
O6 H6B 0.815(19) . ?
O8 Cs1 3.2723(17) 2_666 ?
O8 H8A 0.829(19) . ?
O8 H8B 0.828(19) . ?
O9 Cs1 3.1396(18) 2_565 ?
O11 H11A 0.838(19) . ?
O11 H11B 0.829(19) . ?

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 Cs1 O9 66.35(7) 2_665 2_565 ?
O2 Cs1 O3 157.57(7) 2_665 2_676 ?
O9 Cs1 O3 91.97(5) 2_565 2_676 ?
O2 Cs1 O11 61.93(8) 2_665 . ?
O9 Cs1 O11 120.22(5) 2_565 . ?
O3 Cs1 O11 139.43(5) 2_676 . ?
O2 Cs1 O1 124.55(7) 2_665 . ?
O9 Cs1 O1 158.61(5) 2_565 . ?
O3 Cs1 O1 74.15(5) 2_676 . ?
O11 Cs1 O1 79.75(6) . . ?
O2 Cs1 O8 117.79(7) 2_665 2_666 ?
O9 Cs1 O8 128.55(4) 2_565 2_666 ?
O3 Cs1 O8 79.70(5) 2_676 2_666 ?
O11 Cs1 O8 61.30(5) . 2_666 ?
O1 Cs1 O8 65.89(4) . 2_666 ?
O2 Cs1 O2 77.54(7) 2_665 . ?
O9 Cs1 O2 124.53(6) 2_565 . ?
O3 Cs1 O2 113.09(5) 2_676 . ?
O11 Cs1 O2 70.33(7) . . ?
O1 Cs1 O2 51.41(5) . . ?
O8 Cs1 O2 104.96(6) 2_666 . ?
O2 Cs1 O9 100.37(6) 2_665 . ?
O9 Cs1 O9 81.99(4) 2_565 . ?
O3 Cs1 O9 69.49(4) 2_676 . ?
O11 Cs1 O9 134.03(5) . . ?
O1 Cs1 O9 77.95(5) . . ?
O8 Cs1 O9 137.65(4) 2_666 . ?
O2 Cs1 O9 64.28(7) . . ?
O2 Cs1 O6 74.00(6) 2_665 . ?
O9 Cs1 O6 88.42(4) 2_565 . ?
O3 Cs1 O6 112.79(4) 2_676 . ?
O11 Cs1 O6 50.62(5) . . ?
O1 Cs1 O6 111.78(5) . . ?
O8 Cs1 O6 51.08(4) 2_666 . ?
O2 Cs1 O6 120.93(6) . . ?
O9 Cs1 O6 170.26(4) . . ?
O2 Cs1 O4 114.01(5) 2_665 . ?
O9 Cs1 O4 79.25(4) 2_565 . ?
O3 Cs1 O4 64.52(4) 2_676 . ?
O11 Cs1 O4 95.83(5) . . ?
O1 Cs1 O4 108.00(4) . . ?
O8 Cs1 O4 51.19(4) 2_666 . ?
O2 Cs1 O4 155.99(6) . . ?
O9 Cs1 O4 129.20(4) . . ?
O6 Cs1 O4 49.66(4) . . ?
O2 Cs1 Mg1 103.69(5) 2_665 . ?
O9 Cs1 Mg1 99.89(3) 2_565 . ?
O3 Cs1 Mg1 84.97(3) 2_676 . ?
O11 Cs1 Mg1 66.85(4) . . ?
O1 Cs1 Mg1 95.11(3) . . ?
O8 Cs1 Mg1 29.31(3) 2_666 . ?
O2 Cs1 Mg1 129.55(6) . . ?
O9 Cs1 Mg1 154.46(3) . . ?
O6 Cs1 Mg1 29.70(3) . . ?
O4 Cs1 Mg1 29.82(3) . . ?
O2 Cs1 Cs1 82.13(6) 2_665 2_565 ?
O9 Cs1 Cs1 42.22(3) 2_565 2_565 ?
O3 Cs1 Cs1 77.56(3) 2_676 2_565 ?
O11 Cs1 Cs1 142.82(4) . 2_565 ?
O1 Cs1 Cs1 117.37(4) . 2_565 ?
O8 Cs1 Cs1 154.69(3) 2_666 2_565 ?
O2 Cs1 Cs1 94.11(6) . 2_565 ?
O9 Cs1 Cs1 39.77(3) . 2_565 ?
O6 Cs1 Cs1 130.62(3) . 2_565 ?
O4 Cs1 Cs1 107.97(3) . 2_565 ?
Mg1 Cs1 Cs1 136.321(6) . 2_565 ?
O2 Cs1 H6B 67.0(6) 2_665 . ?
O9 Cs1 H6B 96.0(6) 2_565 . ?
O3 Cs1 H6B 123.8(5) 2_676 . ?
O11 Cs1 H6B 37.1(4) . . ?
O1 Cs1 H6B 105.3(6) . . ?
O8 Cs1 H6B 52.7(7) 2_666 . ?
O2 Cs1 H6B 107.3(3) . . ?
O9 Cs1 H6B 166.7(5) . . ?
O6 Cs1 H6B 13.8(3) . . ?
O4 Cs1 H6B 62.7(4) . . ?
Mg1 Cs1 H6B 38.8(5) . . ?
Cs1 Cs1 H6B 136.7(7) 2_565 . ?
O2 Cs1 H11A 72.3(5) 2_665 . ?
O9 Cs1 H11A 133.7(4) 2_565 . ?
O3 Cs1 H11A 130.0(5) 2_676 . ?
O11 Cs1 H11A 13.7(4) . . ?
O1 Cs1 H11A 66.1(4) . . ?
O8 Cs1 H11A 57.3(6) 2_666 . ?
O2 Cs1 H11A 62.2(6) . . ?
O9 Cs1 H11A 126.3(6) . . ?
O6 Cs1 H11A 60.2(5) . . ?
O4 Cs1 H11A 100.0(6) . . ?
Mg1 Cs1 H11A 70.2(6) . . ?
Cs1 Cs1 H11A 148.0(6) 2_565 . ?
H6B Cs1 H11A 47.5(6) . . ?
O2 Cs1 H2B 88.6(6) 2_665 . ?
O9 Cs1 H2B 139.2(4) 2_565 . ?
O3 Cs1 H2B 105.8(7) 2_676 . ?
O11 Cs1 H2B 66.8(7) . . ?
O1 Cs1 H2B 37.6(5) . . ?
O8 Cs1 H2B 91.2(4) 2_666 . ?
O2 Cs1 H2B 14.8(3) . . ?
O9 Cs1 H2B 71.0(7) . . ?
O6 Cs1 H2B 116.1(7) . . ?
O4 Cs1 H2B 141.5(4) . . ?
Mg1 Cs1 H2B 117.7(5) . . ?
Cs1 Cs1 H2B 105.6(5) 2_565 . ?
H6B Cs1 H2B 103.4(8) . . ?
H11A Cs1 H2B 56.0(8) . . ?
O8 Mg1 O8 180.0 2_666 . ?
O8 Mg1 O6 91.29(7) 2_666 2_666 ?
O8 Mg1 O6 88.71(7) . 2_666 ?
O8 Mg1 O6 88.71(7) 2_666 . ?
O8 Mg1 O6 91.29(7) . . ?
O6 Mg1 O6 180.0 2_666 . ?
O8 Mg1 O4 89.95(7) 2_666 2_666 ?
O8 Mg1 O4 90.05(7) . 2_666 ?
O6 Mg1 O4 89.04(8) 2_666 2_666 ?
O6 Mg1 O4 90.96(8) . 2_666 ?
O8 Mg1 O4 90.05(7) 2_666 . ?
O8 Mg1 O4 89.95(7) . . ?
O6 Mg1 O4 90.96(8) 2_666 . ?
O6 Mg1 O4 89.04(8) . . ?
O4 Mg1 O4 180.000(1) 2_666 . ?
O8 Mg1 Cs1 50.84(5) 2_666 . ?
O8 Mg1 Cs1 129.16(5) . . ?
O6 Mg1 Cs1 124.91(5) 2_666 . ?
O6 Mg1 Cs1 55.09(5) . . ?
O4 Mg1 Cs1 123.16(6) 2_666 . ?
O4 Mg1 Cs1 56.84(5) . . ?
O8 Mg1 Cs1 129.16(5) 2_666 2_666 ?
O8 Mg1 Cs1 50.84(5) . 2_666 ?
O6 Mg1 Cs1 55.09(5) 2_666 2_666 ?
O6 Mg1 Cs1 124.91(5) . 2_666 ?
O4 Mg1 Cs1 56.84(6) 2_666 2_666 ?
O4 Mg1 Cs1 123.16(5) . 2_666 ?
Cs1 Mg1 Cs1 180.0 . 2_666 ?
O3 C1 N3 121.7(2) . . ?
O3 C1 N1 118.8(2) . . ?
N3 C1 N1 119.5(2) . . ?
O7 C2 N3 121.9(2) . . ?
O7 C2 N2 118.4(2) . . ?
N3 C2 N2 119.66(19) . . ?
O1 C3 N1 122.6(2) . . ?
O1 C3 N2 123.4(2) . . ?
N1 C3 N2 114.1(2) . . ?
O5 C4 N4 122.5(2) . . ?
O5 C4 N5 117.3(2) . . ?
N4 C4 N5 120.1(2) . . ?
O9 C5 N6 123.9(2) . . ?
O9 C5 N5 122.4(2) . . ?
N6 C5 N5 113.8(2) . . ?
O10 C6 N4 122.4(2) . . ?
O10 C6 N6 118.0(2) . . ?
N4 C6 N6 119.6(2) . . ?
C3 N1 C1 124.12(19) . . ?
C3 N1 H1 117.9 . . ?
C1 N1 H1 117.9 . . ?
C3 N2 C2 123.42(19) . . ?
C3 N2 H2 118.3 . . ?
C2 N2 H2 118.3 . . ?
C2 N3 C1 119.17(19) . . ?
C4 N4 C6 118.64(19) . . ?
C5 N5 C4 123.68(19) . . ?
C5 N5 H5 118.2 . . ?
C4 N5 H5 118.2 . . ?
C5 N6 C6 124.1(2) . . ?
C5 N6 H6 117.9 . . ?
C6 N6 H6 117.9 . . ?
C3 O1 Cs1 157.27(19) . . ?
Cs1 O2 Cs1 102.46(7) 2_665 . ?
Cs1 O2 H2A 102(3) 2_665 . ?
Cs1 O2 H2A 142(3) . . ?
Cs1 O2 H2B 139(3) 2_665 . ?
Cs1 O2 H2B 72(3) . . ?
H2A O2 H2B 107(4) . . ?
C1 O3 Cs1 129.57(16) . 2_676 ?
Mg1 O4 Cs1 93.34(6) . . ?
Mg1 O4 H4A 121(3) . . ?
Cs1 O4 H4A 104(3) . . ?
Mg1 O4 H4B 124(3) . . ?
Cs1 O4 H4B 98(3) . . ?
H4A O4 H4B 109(4) . . ?
Mg1 O6 Cs1 95.21(6) . . ?
Mg1 O6 H6A 128(3) . . ?
Cs1 O6 H6A 118(3) . . ?
Mg1 O6 H6B 124(3) . . ?
Cs1 O6 H6B 79(3) . . ?
H6A O6 H6B 102(4) . . ?
Mg1 O8 Cs1 99.86(6) . 2_666 ?
Mg1 O8 H8A 121(3) . . ?
Cs1 O8 H8A 116(3) 2_666 . ?
Mg1 O8 H8B 110(3) . . ?
Cs1 O8 H8B 102(3) 2_666 . ?
H8A O8 H8B 107(4) . . ?
C5 O9 Cs1 134.44(16) . 2_565 ?
C5 O9 Cs1 116.40(15) . . ?
Cs1 O9 Cs1 98.01(4) 2_565 . ?
Cs1 O11 H11A 102(3) . . ?
Cs1 O11 H11B 120(3) . . ?
H11A O11 H11B 111(4) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.071
####################################################################### 
# 
# 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_exp_3943
_database_code_depnum_ccdc_archive 'CCDC 1913014'
loop_
_audit_author_name
_audit_author_address
'Mingjun Xia'
;Technical Institute of Physics and Chemistry
China
;
_audit_update_record             
;
2019-04-30 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H16 Ca N12 O16 Rb2'
_chemical_formula_weight         795.39

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'
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'
Ca Ca 0.2262 0.3064 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   10.7222(8)
_cell_length_b                   16.4782(10)
_cell_length_c                   7.1339(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.950(7)
_cell_angle_gamma                90.00
_cell_volume                     1241.48(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             788
_exptl_absorpt_coefficient_mu    4.252
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6979
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         26.35
_reflns_number_total             1317
_reflns_number_gt                1204
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0647P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1317
_refine_ls_number_parameters     113
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0910
_refine_ls_wR_factor_gt          0.0894
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.090
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rb1 Rb 0.13602(3) 0.5000 0.77450(5) 0.03095(18) Uani 1 2 d S . .
Ca1 Ca 0.5000 0.5000 0.0000 0.0291(3) Uani 1 4 d S . .
O1 O 0.5000 0.10791(15) 0.0000 0.0300(6) Uani 1 2 d S . .
O2 O 0.6855(3) 0.5000 0.8610(4) 0.0329(6) Uani 1 2 d SD . .
O3 O 0.6023(3) 0.5000 0.3246(4) 0.0338(7) Uani 1 2 d SD . .
O5 O 0.30266(17) 0.34568(12) 0.8251(3) 0.0274(4) Uani 1 1 d . . .
O4 O 0.0000 0.38471(16) 0.5000 0.0322(7) Uani 1 2 d S . .
O6 O 0.19568(17) 0.14761(11) 0.6811(3) 0.0269(4) Uani 1 1 d . . .
N1 N 0.5000 0.35202(17) 1.0000 0.0200(6) Uani 1 2 d S . .
N2 N 0.0000 0.14052(18) 0.5000 0.0203(6) Uani 1 2 d S . .
N3 N 0.40109(19) 0.22703(13) 0.9089(3) 0.0213(5) Uani 1 1 d . . .
H3 H 0.3367 0.2016 0.8473 0.026 Uiso 1 1 calc R . .
N4 N 0.0988(2) 0.26578(13) 0.5914(3) 0.0219(5) Uani 1 1 d . . .
H4 H 0.1638 0.2909 0.6518 0.026 Uiso 1 1 calc R . .
C1 C 0.3978(2) 0.31073(16) 0.9092(3) 0.0196(5) Uani 1 1 d . . .
C2 C 0.1003(2) 0.18198(16) 0.5926(3) 0.0186(5) Uani 1 1 d . . .
C3 C 0.5000 0.1821(2) 0.0000 0.0199(7) Uani 1 2 d S . .
C4 C 0.0000 0.3109(2) 0.5000 0.0204(7) Uani 1 2 d S . .
H3O H 0.585(3) 0.4563(14) 0.374(4) 0.031 Uiso 1 1 d D . .
H2O H 0.701(3) 0.5411(15) 0.801(4) 0.031 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rb1 O4 2.9298(17) . ?
Rb1 O4 2.9298(17) 5_566 ?
Rb1 O1 2.9476(16) 3_456 ?
Rb1 O1 2.9476(16) 7_556 ?
Rb1 O2 2.951(3) 5_667 ?
Rb1 O3 3.010(3) 5_666 ?
Rb1 O5 3.0929(19) 6_565 ?
Rb1 O5 3.0929(19) . ?
Rb1 Ca1 3.9559(5) 1_556 ?
Rb1 Rb1 4.4609(8) 5_566 ?
Rb1 Rb1 4.7015(9) 5_567 ?
Ca1 O2 2.371(3) 5_666 ?
Ca1 O2 2.371(3) 1_554 ?
Ca1 O3 2.385(3) 5_665 ?
Ca1 O3 2.385(3) . ?
Ca1 N1 2.438(3) 5_666 ?
Ca1 N1 2.438(3) 1_554 ?
Ca1 Rb1 3.9559(5) 1_554 ?
Ca1 Rb1 3.9559(5) 5_666 ?
O1 C3 1.222(5) . ?
O1 Rb1 2.9476(16) 3_544 ?
O1 Rb1 2.9476(16) 7_556 ?
O2 Ca1 2.371(3) 1_556 ?
O2 Rb1 2.951(3) 5_667 ?
O3 Rb1 3.010(3) 5_666 ?
O5 C1 1.234(3) . ?
O4 C4 1.216(5) . ?
O4 Rb1 2.9298(17) 5_566 ?
O6 C2 1.242(3) . ?
N1 C1 1.355(3) . ?
N1 C1 1.355(3) 2_657 ?
N1 Ca1 2.438(3) 1_556 ?
N2 C2 1.347(3) 2_556 ?
N2 C2 1.347(3) . ?
N3 C3 1.363(3) 1_556 ?
N3 C1 1.380(3) . ?
N4 C4 1.365(3) . ?
N4 C2 1.381(3) . ?
C3 N3 1.363(3) 2_656 ?
C3 N3 1.363(3) 1_554 ?
C4 N4 1.365(3) 2_556 ?

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
O4 Rb1 O4 80.84(8) . 5_566 ?
O4 Rb1 O1 121.32(3) . 3_456 ?
O4 Rb1 O1 74.78(4) 5_566 3_456 ?
O4 Rb1 O1 74.78(4) . 7_556 ?
O4 Rb1 O1 121.32(3) 5_566 7_556 ?
O1 Rb1 O1 74.21(8) 3_456 7_556 ?
O4 Rb1 O2 139.58(4) . 5_667 ?
O4 Rb1 O2 139.58(4) 5_566 5_667 ?
O1 Rb1 O2 79.97(5) 3_456 5_667 ?
O1 Rb1 O2 79.97(5) 7_556 5_667 ?
O4 Rb1 O3 102.69(5) . 5_666 ?
O4 Rb1 O3 102.69(5) 5_566 5_666 ?
O1 Rb1 O3 134.23(4) 3_456 5_666 ?
O1 Rb1 O3 134.23(4) 7_556 5_666 ?
O2 Rb1 O3 73.62(8) 5_667 5_666 ?
O4 Rb1 O5 145.27(5) . 6_565 ?
O4 Rb1 O5 75.86(5) 5_566 6_565 ?
O1 Rb1 O5 76.74(5) 3_456 6_565 ?
O1 Rb1 O5 139.70(5) 7_556 6_565 ?
O2 Rb1 O5 67.88(5) 5_667 6_565 ?
O3 Rb1 O5 58.95(4) 5_666 6_565 ?
O4 Rb1 O5 75.86(5) . . ?
O4 Rb1 O5 145.27(5) 5_566 . ?
O1 Rb1 O5 139.70(5) 3_456 . ?
O1 Rb1 O5 76.74(5) 7_556 . ?
O2 Rb1 O5 67.88(5) 5_667 . ?
O3 Rb1 O5 58.95(4) 5_666 . ?
O5 Rb1 O5 110.61(7) 6_565 . ?
O4 Rb1 Ca1 127.88(3) . 1_556 ?
O4 Rb1 Ca1 127.88(3) 5_566 1_556 ?
O1 Rb1 Ca1 108.933(14) 3_456 1_556 ?
O1 Rb1 Ca1 108.933(14) 7_556 1_556 ?
O2 Rb1 Ca1 36.62(6) 5_667 1_556 ?
O3 Rb1 Ca1 36.99(6) 5_666 1_556 ?
O5 Rb1 Ca1 56.16(4) 6_565 1_556 ?
O5 Rb1 Ca1 56.16(4) . 1_556 ?
O4 Rb1 Rb1 40.42(4) . 5_566 ?
O4 Rb1 Rb1 40.42(4) 5_566 5_566 ?
O1 Rb1 Rb1 99.730(13) 3_456 5_566 ?
O1 Rb1 Rb1 99.730(13) 7_556 5_566 ?
O2 Rb1 Rb1 179.62(6) 5_667 5_566 ?
O3 Rb1 Rb1 106.77(6) 5_666 5_566 ?
O5 Rb1 Rb1 112.29(4) 6_565 5_566 ?
O5 Rb1 Rb1 112.29(4) . 5_566 ?
Ca1 Rb1 Rb1 143.758(16) 1_556 5_566 ?
O4 Rb1 Rb1 99.284(13) . 5_567 ?
O4 Rb1 Rb1 99.284(13) 5_566 5_567 ?
O1 Rb1 Rb1 37.11(4) 3_456 5_567 ?
O1 Rb1 Rb1 37.11(4) 7_556 5_567 ?
O2 Rb1 Rb1 77.38(6) 5_667 5_567 ?
O3 Rb1 Rb1 151.00(6) 5_666 5_567 ?
O5 Rb1 Rb1 109.54(4) 6_565 5_567 ?
O5 Rb1 Rb1 109.54(4) . 5_567 ?
Ca1 Rb1 Rb1 114.007(13) 1_556 5_567 ?
Rb1 Rb1 Rb1 102.235(16) 5_566 5_567 ?
O2 Ca1 O2 180.0 5_666 1_554 ?
O2 Ca1 O3 97.35(11) 5_666 5_665 ?
O2 Ca1 O3 82.65(11) 1_554 5_665 ?
O2 Ca1 O3 82.65(11) 5_666 . ?
O2 Ca1 O3 97.35(11) 1_554 . ?
O3 Ca1 O3 180.0 5_665 . ?
O2 Ca1 N1 90.0 5_666 5_666 ?
O2 Ca1 N1 90.0 1_554 5_666 ?
O3 Ca1 N1 90.0 5_665 5_666 ?
O3 Ca1 N1 90.0 . 5_666 ?
O2 Ca1 N1 90.0 5_666 1_554 ?
O2 Ca1 N1 90.0 1_554 1_554 ?
O3 Ca1 N1 90.0 5_665 1_554 ?
O3 Ca1 N1 90.0 . 1_554 ?
N1 Ca1 N1 180.0 5_666 1_554 ?
O2 Ca1 Rb1 47.95(7) 5_666 1_554 ?
O2 Ca1 Rb1 132.05(7) 1_554 1_554 ?
O3 Ca1 Rb1 49.40(8) 5_665 1_554 ?
O3 Ca1 Rb1 130.60(8) . 1_554 ?
N1 Ca1 Rb1 90.0 5_666 1_554 ?
N1 Ca1 Rb1 90.0 1_554 1_554 ?
O2 Ca1 Rb1 132.05(7) 5_666 5_666 ?
O2 Ca1 Rb1 47.95(7) 1_554 5_666 ?
O3 Ca1 Rb1 130.60(8) 5_665 5_666 ?
O3 Ca1 Rb1 49.40(8) . 5_666 ?
N1 Ca1 Rb1 90.0 5_666 5_666 ?
N1 Ca1 Rb1 90.0 1_554 5_666 ?
Rb1 Ca1 Rb1 180.0 1_554 5_666 ?
C3 O1 Rb1 127.11(4) . 3_544 ?
C3 O1 Rb1 127.11(4) . 7_556 ?
Rb1 O1 Rb1 105.79(8) 3_544 7_556 ?
Ca1 O2 Rb1 95.43(10) 1_556 5_667 ?
Ca1 O3 Rb1 93.60(10) . 5_666 ?
C1 O5 Rb1 148.55(17) . . ?
C4 O4 Rb1 130.42(4) . . ?
C4 O4 Rb1 130.42(4) . 5_566 ?
Rb1 O4 Rb1 99.16(8) . 5_566 ?
C1 N1 C1 119.7(3) . 2_657 ?
C1 N1 Ca1 120.13(15) . 1_556 ?
C1 N1 Ca1 120.13(15) 2_657 1_556 ?
C2 N2 C2 119.0(3) 2_556 . ?
C3 N3 C1 124.1(2) 1_556 . ?
C4 N4 C2 123.7(2) . . ?
O5 C1 N1 122.0(3) . . ?
O5 C1 N3 119.0(2) . . ?
N1 C1 N3 119.0(2) . . ?
O6 C2 N2 122.4(3) . . ?
O6 C2 N4 117.8(2) . . ?
N2 C2 N4 119.8(2) . . ?
O1 C3 N3 122.92(15) . 2_656 ?
O1 C3 N3 122.92(15) . 1_554 ?
N3 C3 N3 114.2(3) 2_656 1_554 ?
O4 C4 N4 123.04(16) . . ?
O4 C4 N4 123.04(16) . 2_556 ?
N4 C4 N4 113.9(3) . 2_556 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.35
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.350
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.106
