# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_K(18c6)_Co(CO)4_3
_database_code_depnum_ccdc_archive 'CCDC 2093685'
loop_
_audit_author_name
_audit_author_address
'Christian Schneider'
;Philipps university Marburg
Germany
;
_audit_update_record             
;
2021-07-01 deposited with the CCDC.	2021-11-30 downloaded from the CCDC.
;
_audit_creation_date             2021-06-30
_audit_creation_method           
;
FinalCif V85 by Daniel Kratzert, Freiburg 2021,
https://github.com/dkratzert/FinalCif
;
_shelx_SHELXL_version_number     2016/6
loop_
_audit_author_email
gunnar.werncke@chemie.uni-marburg.de
christian.schneider@chemie.uni-marburg.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1(C4 Co1 O4), 1(C12 H24 K1 O6)'
_chemical_formula_sum            'C16 H24 Co K O10'
_chemical_formula_weight         474.43
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
K K 0.2009 0.2494 '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'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   13.8148(9)
_cell_length_b                   13.8148(9)
_cell_length_c                   9.9198(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1639.5(2)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    6189
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.76
_cell_measurement_theta_min      2.67
_shelx_estimated_absorpt_T_max   0.889
_shelx_estimated_absorpt_T_min   0.745
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.3557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1746 before and 0.1028 after correction. The Ratio of minimum to maximum transmission is 0.4739. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             738
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.118
_exptl_special_details           ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10135
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.109
_diffrn_reflns_theta_min         2.667
_diffrn_ambient_environment      ?
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Quest D8'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support ?
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           ?
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           ?
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1507
_reflns_number_total             1617
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.40(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1617
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0357
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0390P)²+1.0084P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0798
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Others
 Fixed U13: Co1(0) K1(0) O1(0) C1(0)
 Fixed U23: Co1(0) K1(0) O1(0) C1(0)
 Fixed Uiso: H00A(0.024) H00B(0.024) H00C(0.024) H00D(0.024) H00E(0.023)
 H00F(0.023) H00G(0.025) H00H(0.025)
 Fixed X: Co1(0.333333) K1(0.333333) H00A(0.021528) H00B(-0.043566)
 H00C(0.337902) H00D(0.313905) H00E(-0.002823) H00F(0.087222) O1(0.333333)
 H00G(0.122563) H00H(0.144516) C1(0.333333)
 Fixed Y: Co1(0.666667) K1(0.666667) H00A(0.549916) H00B(0.496441)
 H00C(0.427681) H00D(0.331638) H00E(0.352531) H00F(0.414589) O1(0.666667)
 H00G(0.287419) H00H(0.364375) C1(0.666667)
 Fixed Z: H00A(0.914657) H00B(0.776121) H00C(0.661507) H00D(0.769344)
 H00E(0.825888) H00F(0.94356) H00G(0.816992) H00H(0.686533)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.333333 0.666667 0.24709(7) 0.0197(3) Uani 1 3 d S T P . .
K1 K 0.333333 0.666667 0.83117(14) 0.0194(3) Uani 1 3 d S T P . .
O003 O 0.2614(2) 0.4358(2) 0.8281(2) 0.0169(6) Uani 1 1 d . . . . .
O004 O 0.1078(2) 0.5118(2) 0.7849(3) 0.0180(6) Uani 1 1 d . . . . .
O2 O 0.4405(2) 0.5428(3) 0.1533(3) 0.0273(7) Uani 1 1 d . . . . .
C006 C 0.0304(3) 0.5484(3) 0.8158(4) 0.0196(8) Uani 1 1 d . . . . .
H00A H 0.021528 0.549916 0.914657 0.024 Uiso 1 1 calc R . . . .
H00B H -0.043566 0.496441 0.776121 0.024 Uiso 1 1 calc R . . . .
C007 C 0.3376(3) 0.4117(3) 0.7589(4) 0.0199(8) Uani 1 1 d . . . . .
H00C H 0.337902 0.427681 0.661507 0.024 Uiso 1 1 calc R . . . .
H00D H 0.313905 0.331638 0.769344 0.024 Uiso 1 1 calc R . . . .
C008 C 0.0768(3) 0.4064(3) 0.8446(4) 0.0193(8) Uani 1 1 d . . . . .
H00E H -0.002823 0.352531 0.825888 0.023 Uiso 1 1 calc R . . . .
H00F H 0.087222 0.414589 0.943560 0.023 Uiso 1 1 calc R . . . .
O1 O 0.333333 0.666667 0.5422(8) 0.0582(17) Uani 1 3 d S T P . .
C2 C 0.3982(3) 0.5916(3) 0.1902(4) 0.0203(8) Uani 1 1 d . . . . .
C00B C 0.1489(3) 0.3648(3) 0.7862(4) 0.0211(9) Uani 1 1 d . . . . .
H00G H 0.122563 0.287419 0.816992 0.025 Uiso 1 1 calc R . . . .
H00H H 0.144516 0.364375 0.686533 0.025 Uiso 1 1 calc R . . . .
C1 C 0.333333 0.666667 0.4269(8) 0.0351(19) Uani 1 3 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 C2 1.767(4) 3_565 ?
Co1 C2 1.767(4) . ?
Co1 C2 1.767(4) 2_665 ?
Co1 C1 1.784(8) . ?
K1 O003 2.827(3) 2_665 ?
K1 O003 2.827(3) 3_565 ?
K1 O003 2.827(3) . ?
K1 O004 2.798(3) . ?
K1 O004 2.798(3) 3_565 ?
K1 O004 2.798(3) 2_665 ?
O003 C007 1.429(5) . ?
O003 C00B 1.423(5) . ?
O004 C006 1.426(5) . ?
O004 C008 1.426(5) . ?
O2 C2 1.151(5) . ?
C006 C007 1.488(5) 3_565 ?
C008 C00B 1.494(5) . ?
O1 O1 0.000(15) 3_565 ?
O1 O1 0.000(15) 2_665 ?
O1 C1 1.144(10) . ?

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
C2 Co1 C2 110.32(12) 3_565 2_665 ?
C2 Co1 C2 110.32(12) 3_565 . ?
C2 Co1 C2 110.32(12) 2_665 . ?
C2 Co1 C1 108.60(12) . . ?
C2 Co1 C1 108.61(12) 3_565 . ?
C2 Co1 C1 108.61(12) 2_665 . ?
O003 K1 O003 119.990(2) 2_665 . ?
O003 K1 O003 119.987(3) 3_565 2_665 ?
O003 K1 O003 119.989(3) 3_565 . ?
O004 K1 O003 60.45(8) . . ?
O004 K1 O003 60.22(8) 2_665 . ?
O004 K1 O003 169.95(9) 2_665 3_565 ?
O004 K1 O003 169.95(9) 3_565 . ?
O004 K1 O003 60.22(8) . 3_565 ?
O004 K1 O003 169.95(9) . 2_665 ?
O004 K1 O003 60.45(8) 2_665 2_665 ?
O004 K1 O003 60.45(8) 3_565 3_565 ?
O004 K1 O003 60.22(8) 3_565 2_665 ?
O004 K1 O004 117.37(3) . 2_665 ?
O004 K1 O004 117.37(3) 3_565 2_665 ?
O004 K1 O004 117.37(3) 3_565 . ?
C007 O003 K1 112.5(2) . . ?
C00B O003 K1 115.3(2) . . ?
C00B O003 C007 112.1(3) . . ?
C006 O004 K1 116.1(2) . . ?
C006 O004 C008 112.2(3) . . ?
C008 O004 K1 111.3(2) . . ?
O004 C006 C007 108.3(3) . 3_565 ?
O003 C007 C006 109.2(3) . 2_665 ?
O004 C008 C00B 108.3(3) . . ?
O1 O1 C1 90.0(12) 2_665 . ?
O1 O1 C1 90.0(12) 3_565 . ?
O2 C2 Co1 179.9(4) . . ?
O003 C00B C008 109.3(3) . . ?
O1 C1 Co1 180.0 . . ?
O1 C1 Co1 180.0 2_665 . ?
O1 C1 Co1 180.0 3_565 . ?
O1 C1 O1 0.000(3) 3_565 . ?
O1 C1 O1 0.000(3) 3_565 2_665 ?
O1 C1 O1 0.000(2) 2_665 . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.60(3)
2 0.40(3)

####################################################################### 
# 
# 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_Fe-CO_2_18c6
_database_code_depnum_ccdc_archive 'CCDC 2093686'
loop_
_audit_author_name
_audit_author_address
'Christian Schneider'
;Philipps university Marburg
Germany
;
_audit_update_record             
;
2021-07-01 deposited with the CCDC.	2021-11-30 downloaded from the CCDC.
;
_audit_creation_date             2021-06-30

loop_
_audit_author_email
gunnar.werncke@chemie.uni-marburg.de
christian.schneider@chemie.uni-marburg.de
_audit_creation_method           
;
FinalCif V85 by Daniel Kratzert, Freiburg 2021,
https://github.com/dkratzert/FinalCif
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C25 H60 Fe K N2 O7 Si4'
_chemical_formula_moiety         'C25 H60 Fe K N2 O7 Si4'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_chemical_formula_weight         708.06
_chemical_melting_point          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C14(H14A,H14B), C17(H17A,H17B), C15(H15A,H15B), C21(H21A,
 H21B), C25(H25A,H25B), C22(H22A,H22B), C23(H23A,H23B), C20(H20A,H20B),
 C24(H24A,H24B), C19(H19A,H19B), C18(H18A,H18B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C5(H5A,H5B,H5C),
 C11(H11A,H11B,H11C), C7(H7A,H7B,H7C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C4(H4A,
 H4B,H4C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.6181(5)
_cell_length_b                   19.9580(10)
_cell_length_c                   23.1156(12)
_cell_angle_alpha                90
_cell_angle_beta                 90.923(2)
_cell_angle_gamma                90
_cell_volume                     3975.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5698
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      26.020
_exptl_crystal_description       needle
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.475
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.114
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6639
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1228 before and 0.0575 after correction. The Ratio of minimum to maximum transmission is 0.8908. The λ/2 correction factor is Not present.'
_shelx_estimated_absorpt_T_min   0.750
_shelx_estimated_absorpt_T_max   0.930
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           ?
_diffrn_ambient_temperature      100.01
_diffrn_ambient_environment      ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  ?
_diffrn_radiation_probe          ?
_diffrn_source                   ?
_diffrn_source_type              ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_detector                 ?
_diffrn_detector_type            ?
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device       ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_measurement_specimen_support ?
_diffrn_reflns_number            29271
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_theta_min         2.223
_diffrn_reflns_theta_max         26.071
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7815
_reflns_number_gt                6058
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       ?
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0190P)²+1.1499P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         7815
_refine_ls_number_parameters     373
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0695
_refine_ls_wR_factor_gt          0.0638
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .

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'
Fe Fe 0.3463 0.8444 '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'
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_
_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
Fe1 Fe 0.19911(3) 0.24251(2) 0.59136(2) 0.01478(7) Uani 1 1 d . . . . .
K1 K 0.50170(5) 0.43593(2) 0.71673(2) 0.01616(10) Uani 1 1 d . . . . .
Si2 Si 0.29865(6) 0.08963(2) 0.58006(2) 0.01569(12) Uani 1 1 d . . . . .
Si4 Si 0.07882(6) 0.30746(3) 0.47637(2) 0.01596(12) Uani 1 1 d . . . . .
Si3 Si -0.13879(6) 0.21669(3) 0.54214(2) 0.01832(12) Uani 1 1 d . . . . .
Si1 Si 0.31801(6) 0.16005(3) 0.69694(2) 0.01545(12) Uani 1 1 d . . . . .
O2 O 0.57560(16) 0.35031(6) 0.80628(6) 0.0215(3) Uani 1 1 d . . . . .
O3 O 0.81241(15) 0.39093(6) 0.73181(6) 0.0224(3) Uani 1 1 d . . . . .
O7 O 0.31546(15) 0.43131(7) 0.81344(6) 0.0216(3) Uani 1 1 d . . . . .
O6 O 0.22027(16) 0.51009(7) 0.72010(6) 0.0247(3) Uani 1 1 d . . . . .
O5 O 0.44194(16) 0.53542(7) 0.63322(6) 0.0253(3) Uani 1 1 d . . . . .
O4 O 0.71070(16) 0.45372(7) 0.62881(6) 0.0259(3) Uani 1 1 d . . . . .
N2 N 0.03728(18) 0.25244(7) 0.53004(7) 0.0150(3) Uani 1 1 d . . . . .
N1 N 0.27676(18) 0.15684(7) 0.62480(6) 0.0140(3) Uani 1 1 d . . . . .
O1 O 0.3210(2) 0.36997(8) 0.64020(8) 0.0416(4) Uani 1 1 d . . . . .
C2 C 0.4996(2) 0.20752(10) 0.71524(9) 0.0263(5) Uani 1 1 d . . . . .
H2A H 0.589818 0.182241 0.701973 0.039 Uiso 1 1 calc GR . . . .
H2B H 0.507513 0.213834 0.757224 0.039 Uiso 1 1 calc GR . . . .
H2C H 0.496602 0.251320 0.696094 0.039 Uiso 1 1 calc GR . . . .
C8 C -0.1434(2) 0.18206(11) 0.61739(9) 0.0250(5) Uani 1 1 d . . . . .
H8A H -0.058950 0.149655 0.622713 0.038 Uiso 1 1 calc GR . . . .
H8B H -0.243123 0.159745 0.623491 0.038 Uiso 1 1 calc GR . . . .
H8C H -0.130616 0.218644 0.645332 0.038 Uiso 1 1 calc GR . . . .
C1 C 0.2745(2) 0.31894(10) 0.62169(9) 0.0217(5) Uani 1 1 d . . . . .
C13 C 0.2928(2) 0.30909(10) 0.46169(9) 0.0267(5) Uani 1 1 d . . . . .
H13A H 0.348376 0.328363 0.495049 0.040 Uiso 1 1 calc GR . . . .
H13B H 0.311800 0.336430 0.427312 0.040 Uiso 1 1 calc GR . . . .
H13C H 0.329618 0.263317 0.455060 0.040 Uiso 1 1 calc GR . . . .
C16 C 0.8962(3) 0.38691(12) 0.67914(10) 0.0324(5) Uani 1 1 d . . . . .
H16A H 0.859542 0.348048 0.656071 0.039 Uiso 1 1 calc R . . . .
H16B H 1.008278 0.380960 0.687670 0.039 Uiso 1 1 calc R . . . .
C5 C 0.4913(3) 0.04631(10) 0.58807(10) 0.0280(5) Uani 1 1 d . . . . .
H5A H 0.574934 0.079283 0.584761 0.042 Uiso 1 1 calc GR . . . .
H5B H 0.501219 0.012500 0.557612 0.042 Uiso 1 1 calc GR . . . .
H5C H 0.498210 0.024546 0.626031 0.042 Uiso 1 1 calc GR . . . .
C14 C 0.7350(2) 0.33777(11) 0.81864(10) 0.0282(5) Uani 1 1 d . . . . .
H14A H 0.745765 0.296601 0.842264 0.034 Uiso 1 1 calc R . . . .
H14B H 0.779868 0.375606 0.840989 0.034 Uiso 1 1 calc R . . . .
C11 C 0.0175(2) 0.39585(9) 0.49372(9) 0.0233(5) Uani 1 1 d . . . . .
H11A H -0.091849 0.396089 0.504681 0.035 Uiso 1 1 calc GR . . . .
H11B H 0.031165 0.424309 0.459632 0.035 Uiso 1 1 calc GR . . . .
H11C H 0.081424 0.413067 0.525872 0.035 Uiso 1 1 calc GR . . . .
C7 C 0.2882(3) 0.11521(10) 0.50210(8) 0.0256(5) Uani 1 1 d . . . . .
H7A H 0.190491 0.138999 0.494456 0.038 Uiso 1 1 calc GR . . . .
H7B H 0.292894 0.075258 0.477547 0.038 Uiso 1 1 calc GR . . . .
H7C H 0.375647 0.144770 0.493519 0.038 Uiso 1 1 calc GR . . . .
C17 C 0.8701(2) 0.45024(12) 0.64593(10) 0.0326(6) Uani 1 1 d . . . . .
H17A H 0.897698 0.489345 0.670347 0.039 Uiso 1 1 calc R . . . .
H17B H 0.936387 0.450833 0.611341 0.039 Uiso 1 1 calc R . . . .
C15 C 0.8196(3) 0.32956(10) 0.76348(10) 0.0297(5) Uani 1 1 d . . . . .
H15A H 0.929213 0.317586 0.771763 0.036 Uiso 1 1 calc R . . . .
H15B H 0.771894 0.293048 0.740298 0.036 Uiso 1 1 calc R . . . .
C21 C 0.2189(3) 0.56843(11) 0.68489(10) 0.0324(5) Uani 1 1 d . . . . .
H21A H 0.284219 0.603737 0.702967 0.039 Uiso 1 1 calc R . . . .
H21B H 0.111738 0.585806 0.680691 0.039 Uiso 1 1 calc R . . . .
C25 C 0.4861(3) 0.35273(11) 0.85736(9) 0.0281(5) Uani 1 1 d . . . . .
H25A H 0.526545 0.388132 0.883531 0.034 Uiso 1 1 calc R . . . .
H25B H 0.492740 0.309285 0.877932 0.034 Uiso 1 1 calc R . . . .
C3 C 0.1582(2) 0.20118(11) 0.73846(9) 0.0260(5) Uani 1 1 d . . . . .
H3A H 0.143737 0.247206 0.724621 0.039 Uiso 1 1 calc GR . . . .
H3B H 0.186036 0.201825 0.779732 0.039 Uiso 1 1 calc GR . . . .
H3C H 0.061683 0.175955 0.732668 0.039 Uiso 1 1 calc GR . . . .
C22 C 0.1670(3) 0.52218(12) 0.77708(10) 0.0336(6) Uani 1 1 d . . . . .
H22A H 0.062371 0.542616 0.775494 0.040 Uiso 1 1 calc R . . . .
H22B H 0.238241 0.553408 0.797564 0.040 Uiso 1 1 calc R . . . .
C23 C 0.1617(2) 0.45683(12) 0.80829(10) 0.0331(6) Uani 1 1 d . . . . .
H23A H 0.117418 0.463217 0.847157 0.040 Uiso 1 1 calc R . . . .
H23B H 0.095184 0.424786 0.786571 0.040 Uiso 1 1 calc R . . . .
C6 C 0.1458(3) 0.02413(10) 0.59127(10) 0.0301(5) Uani 1 1 d . . . . .
H6A H 0.150489 0.008553 0.631466 0.045 Uiso 1 1 calc GR . . . .
H6B H 0.163832 -0.013729 0.565227 0.045 Uiso 1 1 calc GR . . . .
H6C H 0.043177 0.043354 0.582968 0.045 Uiso 1 1 calc GR . . . .
C4 C 0.3454(3) 0.07498(10) 0.73155(9) 0.0269(5) Uani 1 1 d . . . . .
H4A H 0.251293 0.048151 0.725553 0.040 Uiso 1 1 calc GR . . . .
H4B H 0.365579 0.080487 0.773127 0.040 Uiso 1 1 calc GR . . . .
H4C H 0.433610 0.052192 0.713928 0.040 Uiso 1 1 calc GR . . . .
C9 C -0.3065(2) 0.27674(12) 0.53539(10) 0.0343(6) Uani 1 1 d . . . . .
H9A H -0.289036 0.314881 0.561382 0.051 Uiso 1 1 calc GR . . . .
H9B H -0.402638 0.253817 0.545867 0.051 Uiso 1 1 calc GR . . . .
H9C H -0.315255 0.292777 0.495397 0.051 Uiso 1 1 calc GR . . . .
C20 C 0.2807(3) 0.55033(11) 0.62690(10) 0.0320(5) Uani 1 1 d . . . . .
H20A H 0.224547 0.510891 0.611210 0.038 Uiso 1 1 calc R . . . .
H20B H 0.265715 0.588141 0.599656 0.038 Uiso 1 1 calc R . . . .
C10 C -0.1819(3) 0.14545(11) 0.49158(9) 0.0320(5) Uani 1 1 d . . . . .
H10A H -0.181442 0.161720 0.451583 0.048 Uiso 1 1 calc GR . . . .
H10B H -0.284104 0.126736 0.500120 0.048 Uiso 1 1 calc GR . . . .
H10C H -0.102587 0.110641 0.496599 0.048 Uiso 1 1 calc GR . . . .
C24 C 0.3209(3) 0.36735(11) 0.84085(9) 0.0280(5) Uani 1 1 d . . . . .
H24A H 0.280896 0.332474 0.814057 0.034 Uiso 1 1 calc R . . . .
H24B H 0.255741 0.367556 0.875722 0.034 Uiso 1 1 calc R . . . .
C12 C -0.0192(3) 0.28478(11) 0.40576(9) 0.0282(5) Uani 1 1 d . . . . .
H12A H 0.010775 0.239251 0.394678 0.042 Uiso 1 1 calc GR . . . .
H12B H 0.012523 0.316366 0.375726 0.042 Uiso 1 1 calc GR . . . .
H12C H -0.132045 0.286914 0.410101 0.042 Uiso 1 1 calc GR . . . .
C19 C 0.5095(3) 0.51463(12) 0.58047(9) 0.0325(5) Uani 1 1 d . . . . .
H19A H 0.487925 0.548138 0.549795 0.039 Uiso 1 1 calc R . . . .
H19B H 0.464744 0.471181 0.567995 0.039 Uiso 1 1 calc R . . . .
C18 C 0.6812(3) 0.50779(12) 0.59026(9) 0.0339(6) Uani 1 1 d . . . . .
H18A H 0.732660 0.499370 0.552976 0.041 Uiso 1 1 calc R . . . .
H18B H 0.723644 0.549811 0.606866 0.041 Uiso 1 1 calc R . . . .


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
Fe1 N2 1.9824(16) . ?
Fe1 N1 1.9880(15) . ?
Fe1 C1 1.796(2) . ?
K1 O2 2.7510(14) . ?
K1 O3 2.8405(14) . ?
K1 O7 2.7745(14) . ?
K1 O6 2.8436(14) . ?
K1 O5 2.8112(14) . ?
K1 O4 2.7603(14) . ?
Si2 N1 1.7061(15) . ?
Si2 C5 1.878(2) . ?
Si2 C7 1.874(2) . ?
Si2 C6 1.877(2) . ?
Si4 N2 1.6993(16) . ?
Si4 C13 1.880(2) . ?
Si4 C11 1.8864(19) . ?
Si4 C12 1.881(2) . ?
Si3 N2 1.7039(16) . ?
Si3 C8 1.873(2) . ?
Si3 C9 1.882(2) . ?
Si3 C10 1.874(2) . ?
Si1 N1 1.7005(16) . ?
Si1 C2 1.872(2) . ?
Si1 C3 1.880(2) . ?
Si1 C4 1.890(2) . ?
O2 C14 1.421(2) . ?
O2 C25 1.422(2) . ?
O3 C16 1.428(2) . ?
O3 C15 1.428(2) . ?
O7 C23 1.423(2) . ?
O7 C24 1.426(2) . ?
O6 C21 1.420(2) . ?
O6 C22 1.422(2) . ?
O5 C20 1.426(3) . ?
O5 C19 1.421(2) . ?
O4 C17 1.425(3) . ?
O4 C18 1.420(3) . ?
O1 C1 1.173(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.494(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.488(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C20 1.495(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.496(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.491(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C18 1.500(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N1 126.34(6) . . ?
C1 Fe1 N2 116.11(8) . . ?
C1 Fe1 N1 117.47(8) . . ?
O2 K1 O3 60.32(4) . . ?
O2 K1 O7 60.20(4) . . ?
O2 K1 O6 119.34(4) . . ?
O2 K1 O5 173.26(4) . . ?
O2 K1 O4 119.21(4) . . ?
O3 K1 O6 164.59(4) . . ?
O7 K1 O3 116.56(4) . . ?
O7 K1 O6 59.37(4) . . ?
O7 K1 O5 118.35(4) . . ?
O5 K1 O3 118.00(4) . . ?
O5 K1 O6 60.28(4) . . ?
O4 K1 O3 60.40(4) . . ?
O4 K1 O7 172.04(4) . . ?
O4 K1 O6 121.34(4) . . ?
O4 K1 O5 61.18(4) . . ?
N1 Si2 C5 114.10(9) . . ?
N1 Si2 C7 111.39(8) . . ?
N1 Si2 C6 112.28(9) . . ?
C7 Si2 C5 104.43(10) . . ?
C7 Si2 C6 107.43(10) . . ?
C6 Si2 C5 106.68(10) . . ?
N2 Si4 C13 111.20(9) . . ?
N2 Si4 C11 112.71(8) . . ?
N2 Si4 C12 112.39(9) . . ?
C13 Si4 C11 107.52(9) . . ?
C13 Si4 C12 106.00(10) . . ?
C12 Si4 C11 106.63(10) . . ?
N2 Si3 C8 109.84(9) . . ?
N2 Si3 C9 113.86(9) . . ?
N2 Si3 C10 112.54(9) . . ?
C8 Si3 C9 106.51(10) . . ?
C8 Si3 C10 106.99(10) . . ?
C10 Si3 C9 106.69(11) . . ?
N1 Si1 C2 113.67(9) . . ?
N1 Si1 C3 111.96(9) . . ?
N1 Si1 C4 113.82(8) . . ?
C2 Si1 C3 106.28(10) . . ?
C2 Si1 C4 105.10(10) . . ?
C3 Si1 C4 105.29(10) . . ?
C14 O2 K1 118.17(12) . . ?
C14 O2 C25 112.02(16) . . ?
C25 O2 K1 118.80(11) . . ?
C16 O3 K1 113.69(12) . . ?
C16 O3 C15 111.75(15) . . ?
C15 O3 K1 111.55(11) . . ?
C23 O7 K1 118.08(12) . . ?
C23 O7 C24 112.45(15) . . ?
C24 O7 K1 111.86(11) . . ?
C21 O6 K1 114.21(11) . . ?
C21 O6 C22 113.07(16) . . ?
C22 O6 K1 113.68(12) . . ?
C20 O5 K1 112.66(12) . . ?
C19 O5 K1 108.06(12) . . ?
C19 O5 C20 112.63(16) . . ?
C17 O4 K1 115.27(12) . . ?
C18 O4 K1 116.58(12) . . ?
C18 O4 C17 111.93(16) . . ?
Si4 N2 Fe1 115.63(8) . . ?
Si4 N2 Si3 126.10(10) . . ?
Si3 N2 Fe1 117.31(8) . . ?
Si2 N1 Fe1 118.70(8) . . ?
Si1 N1 Fe1 114.36(8) . . ?
Si1 N1 Si2 126.92(9) . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si3 C8 H8A 109.5 . . ?
Si3 C8 H8B 109.5 . . ?
Si3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 C1 Fe1 177.86(19) . . ?
Si4 C13 H13A 109.5 . . ?
Si4 C13 H13B 109.5 . . ?
Si4 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O3 C16 H16A 110.0 . . ?
O3 C16 H16B 110.0 . . ?
O3 C16 C17 108.47(17) . . ?
H16A C16 H16B 108.4 . . ?
C17 C16 H16A 110.0 . . ?
C17 C16 H16B 110.0 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O2 C14 H14A 109.8 . . ?
O2 C14 H14B 109.8 . . ?
O2 C14 C15 109.42(18) . . ?
H14A C14 H14B 108.2 . . ?
C15 C14 H14A 109.8 . . ?
C15 C14 H14B 109.8 . . ?
Si4 C11 H11A 109.5 . . ?
Si4 C11 H11B 109.5 . . ?
Si4 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O4 C17 C16 108.68(17) . . ?
O4 C17 H17A 110.0 . . ?
O4 C17 H17B 110.0 . . ?
C16 C17 H17A 110.0 . . ?
C16 C17 H17B 110.0 . . ?
H17A C17 H17B 108.3 . . ?
O3 C15 C14 109.09(16) . . ?
O3 C15 H15A 109.9 . . ?
O3 C15 H15B 109.9 . . ?
C14 C15 H15A 109.9 . . ?
C14 C15 H15B 109.9 . . ?
H15A C15 H15B 108.3 . . ?
O6 C21 H21A 110.0 . . ?
O6 C21 H21B 110.0 . . ?
O6 C21 C20 108.42(17) . . ?
H21A C21 H21B 108.4 . . ?
C20 C21 H21A 110.0 . . ?
C20 C21 H21B 110.0 . . ?
O2 C25 H25A 109.9 . . ?
O2 C25 H25B 109.9 . . ?
O2 C25 C24 108.75(17) . . ?
H25A C25 H25B 108.3 . . ?
C24 C25 H25A 109.9 . . ?
C24 C25 H25B 109.9 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O6 C22 H22A 110.1 . . ?
O6 C22 H22B 110.1 . . ?
O6 C22 C23 108.22(17) . . ?
H22A C22 H22B 108.4 . . ?
C23 C22 H22A 110.1 . . ?
C23 C22 H22B 110.1 . . ?
O7 C23 C22 108.51(17) . . ?
O7 C23 H23A 110.0 . . ?
O7 C23 H23B 110.0 . . ?
C22 C23 H23A 110.0 . . ?
C22 C23 H23B 110.0 . . ?
H23A C23 H23B 108.4 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
K1 C4 H4A 85.2 2_646 . ?
K1 C4 H4B 71.0 2_646 . ?
K1 C4 H4C 56.7 2_646 . ?
Si1 C4 K1 163.43(11) . 2_646 ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si3 C9 H9A 109.5 . . ?
Si3 C9 H9B 109.5 . . ?
Si3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O5 C20 C21 108.62(18) . . ?
O5 C20 H20A 110.0 . . ?
O5 C20 H20B 110.0 . . ?
C21 C20 H20A 110.0 . . ?
C21 C20 H20B 110.0 . . ?
H20A C20 H20B 108.3 . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O7 C24 C25 108.21(16) . . ?
O7 C24 H24A 110.1 . . ?
O7 C24 H24B 110.1 . . ?
C25 C24 H24A 110.1 . . ?
C25 C24 H24B 110.1 . . ?
H24A C24 H24B 108.4 . . ?
Si4 C12 H12A 109.5 . . ?
Si4 C12 H12B 109.5 . . ?
Si4 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O5 C19 H19A 110.0 . . ?
O5 C19 H19B 110.0 . . ?
O5 C19 C18 108.29(18) . . ?
H19A C19 H19B 108.4 . . ?
C18 C19 H19A 110.0 . . ?
C18 C19 H19B 110.0 . . ?
O4 C18 C19 109.29(17) . . ?
O4 C18 H18A 109.8 . . ?
O4 C18 H18B 109.8 . . ?
C19 C18 H18A 109.8 . . ?
C19 C18 H18B 109.8 . . ?
H18A C18 H18B 108.3 . . ?

####################################################################### 
# 
# 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_Co_CO_1_crypt
_database_code_depnum_ccdc_archive 'CCDC 2093687'
loop_
_audit_author_name
_audit_author_address
'Christian Schneider'
;Philipps university Marburg
Germany
;
_audit_update_record             
;
2021-07-01 deposited with the CCDC.	2021-11-30 downloaded from the CCDC.
;
_audit_creation_date             2021-06-30

loop_
_audit_author_email
gunnar.werncke@chemie.uni-marburg.de
christian.schneider@chemie.uni-marburg.de
_audit_creation_method           
;
FinalCif V85 by Daniel Kratzert, Freiburg 2021,
https://github.com/dkratzert/FinalCif
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C31 H72 Co K N4 O7 Si4'
_chemical_formula_moiety         'C13 H36 Co N2 O Si4, C18 H36 K N2 O6'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_chemical_formula_weight         823.31
_chemical_melting_point          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C21(H21A,H21B), C27(H27A,H27B), C24(H24A,H24B), C28(H28A,
 H28B), C25(H25A,H25B), C22(H22A,H22B), C29(H29A,H29B), C14(H14A,H14B),
 C15(H15A,H15B), C20(H20A,H20B), C30(H30A,H30B), C31(H31A,H31B), C16(H16A,H16B),
  C19(H19A,H19B), C17(H17A,H17B), C18(H18A,H18B), C26(H26A,H26B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C5(H5A,H5B,H5C),
 C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C4(H4A,
 H4B,H4C), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C2(H2A,H2B,H2C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_space_group_crystal_system      triclinic
_publ_section_exptl              
;
Any special experimental details
;
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.5496(5)
_cell_length_b                   13.9247(6)
_cell_length_c                   15.1024(6)
_cell_angle_alpha                111.7110(10)
_cell_angle_beta                 92.9320(10)
_cell_angle_gamma                108.9010(10)
_cell_volume                     2275.40(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9903
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      26.02
_exptl_crystal_description       plank
_exptl_crystal_colour            'clear light green'
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.117
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_correction_T_min  0.6881
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1085 before and 0.0511 after correction. The Ratio of minimum to maximum transmission is 0.9233. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   0.784
_shelx_estimated_absorpt_T_max   0.931
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           ?
_diffrn_ambient_temperature      100.0
_diffrn_ambient_environment      ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support ?
_diffrn_reflns_number            41838
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_theta_min         2.210
_diffrn_reflns_theta_max         26.082
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9004
_reflns_number_gt                7026
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       ?
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0328P)²+1.8172P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         9004
_refine_ls_number_parameters     445
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0877
_refine_ls_wR_factor_gt          0.0807
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .

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'
K K 0.2009 0.2494 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_
_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 0.20547(3) 0.17229(3) 0.80891(2) 0.01773(8) Uani 1 1 d . . . . .
K1 K 0.70260(4) 0.37664(4) 0.43564(3) 0.01636(11) Uani 1 1 d . . . . .
Si3 Si 0.04830(6) 0.29525(5) 0.91072(5) 0.02213(15) Uani 1 1 d . . . . .
Si2 Si 0.28718(6) 0.13598(6) 0.98986(5) 0.02361(15) Uani 1 1 d . . . . .
Si1 Si 0.46355(6) 0.23134(6) 0.88391(5) 0.02550(16) Uani 1 1 d . . . . .
Si4 Si -0.05745(6) 0.07536(6) 0.73452(5) 0.02486(16) Uani 1 1 d . . . . .
O4 O 0.47199(13) 0.29599(13) 0.45679(11) 0.0232(4) Uani 1 1 d . . . . .
O5 O 0.53411(13) 0.41767(13) 0.34286(11) 0.0234(4) Uani 1 1 d . . . . .
O6 O 0.70935(14) 0.16480(13) 0.36015(13) 0.0295(4) Uani 1 1 d . . . . .
O7 O 0.79732(14) 0.30833(14) 0.26866(11) 0.0257(4) Uani 1 1 d . . . . .
O2 O 0.81921(14) 0.45445(14) 0.63117(12) 0.0292(4) Uani 1 1 d . . . . .
O3 O 0.85916(15) 0.60080(14) 0.53736(14) 0.0368(5) Uani 1 1 d . . . . .
O1 O 0.25551(16) 0.14824(15) 0.61642(13) 0.0355(4) Uani 1 1 d . . . . .
N1 N 0.32656(16) 0.18148(15) 0.90158(13) 0.0201(4) Uani 1 1 d . . . . .
N2 N 0.05372(16) 0.17833(15) 0.82333(13) 0.0200(4) Uani 1 1 d . . . . .
N3 N 0.63813(18) 0.22908(17) 0.54586(16) 0.0289(5) Uani 1 1 d . . . . .
N4 N 0.76946(18) 0.52661(18) 0.33041(16) 0.0298(5) Uani 1 1 d . . . . .
C1 C 0.23706(19) 0.15636(19) 0.69327(17) 0.0211(5) Uani 1 1 d . . . . .
C23 C 0.4250(2) 0.3931(2) 0.36980(17) 0.0262(5) Uani 1 1 d . . . . .
H23A H 0.366972 0.388558 0.319933 0.031 Uiso 1 1 calc R . . . .
H23B H 0.428169 0.452648 0.432537 0.031 Uiso 1 1 calc R . . . .
C21 C 0.4403(2) 0.1973(2) 0.4737(2) 0.0334(6) Uani 1 1 d . . . . .
H21A H 0.444911 0.135363 0.416481 0.040 Uiso 1 1 calc R . . . .
H21B H 0.360208 0.176402 0.484187 0.040 Uiso 1 1 calc R . . . .
C27 C 0.7351(2) 0.1252(2) 0.4301(2) 0.0362(7) Uani 1 1 d . . . . .
H27A H 0.810511 0.176157 0.473009 0.043 Uiso 1 1 calc R . . . .
H27B H 0.738489 0.050455 0.397016 0.043 Uiso 1 1 calc R . . . .
C3 C 0.4911(2) 0.3506(2) 0.8471(2) 0.0355(6) Uani 1 1 d . . . . .
H3A H 0.445036 0.324455 0.782562 0.053 Uiso 1 1 calc GR . . . .
H3B H 0.572756 0.381250 0.845287 0.053 Uiso 1 1 calc GR . . . .
H3C H 0.470006 0.408561 0.894237 0.053 Uiso 1 1 calc GR . . . .
C10 C -0.0468(2) 0.3546(2) 0.8646(2) 0.0327(6) Uani 1 1 d . . . . .
H10A H -0.031307 0.354594 0.801687 0.049 Uiso 1 1 calc GR . . . .
H10B H -0.030845 0.430990 0.911218 0.049 Uiso 1 1 calc GR . . . .
H10C H -0.127505 0.309010 0.857114 0.049 Uiso 1 1 calc GR . . . .
C24 C 0.5680(2) 0.5169(2) 0.32626(18) 0.0267(6) Uani 1 1 d . . . . .
H24A H 0.591199 0.582838 0.388975 0.032 Uiso 1 1 calc R . . . .
H24B H 0.502976 0.517184 0.286558 0.032 Uiso 1 1 calc R . . . .
C8 C 0.1941(2) 0.4075(2) 0.96126(18) 0.0305(6) Uani 1 1 d . . . . .
H8A H 0.246094 0.380049 0.986562 0.046 Uiso 1 1 calc GR . . . .
H8B H 0.189077 0.472173 1.013902 0.046 Uiso 1 1 calc GR . . . .
H8C H 0.223666 0.428945 0.909810 0.046 Uiso 1 1 calc GR . . . .
C5 C 0.3778(2) 0.0634(2) 1.02089(19) 0.0335(6) Uani 1 1 d . . . . .
H5A H 0.397488 0.018819 0.961553 0.050 Uiso 1 1 calc GR . . . .
H5B H 0.334514 0.014808 1.050343 0.050 Uiso 1 1 calc GR . . . .
H5C H 0.448310 0.119038 1.066857 0.050 Uiso 1 1 calc GR . . . .
C28 C 0.7652(2) 0.1359(2) 0.2801(2) 0.0360(7) Uani 1 1 d . . . . .
H28A H 0.734395 0.054136 0.242814 0.043 Uiso 1 1 calc R . . . .
H28B H 0.848605 0.160429 0.303833 0.043 Uiso 1 1 calc R . . . .
C25 C 0.6669(2) 0.5213(2) 0.2741(2) 0.0329(6) Uani 1 1 d . . . . .
H25A H 0.642516 0.454428 0.212016 0.039 Uiso 1 1 calc R . . . .
H25B H 0.687151 0.587290 0.258573 0.039 Uiso 1 1 calc R . . . .
C6 C 0.2959(3) 0.2511(3) 1.10842(19) 0.0450(8) Uani 1 1 d . . . . .
H6A H 0.375616 0.303311 1.133817 0.067 Uiso 1 1 calc GR . . . .
H6B H 0.269121 0.219614 1.155155 0.067 Uiso 1 1 calc GR . . . .
H6C H 0.247436 0.290289 1.098124 0.067 Uiso 1 1 calc GR . . . .
C11 C -0.0391(2) -0.0618(2) 0.6919(2) 0.0372(7) Uani 1 1 d . . . . .
H11A H 0.032143 -0.055281 0.666735 0.056 Uiso 1 1 calc GR . . . .
H11B H -0.104376 -0.118220 0.640236 0.056 Uiso 1 1 calc GR . . . .
H11C H -0.035622 -0.083614 0.746309 0.056 Uiso 1 1 calc GR . . . .
C22 C 0.3929(2) 0.2850(2) 0.37874(18) 0.0291(6) Uani 1 1 d . . . . .
H22A H 0.313979 0.262805 0.391548 0.035 Uiso 1 1 calc R . . . .
H22B H 0.394961 0.226573 0.317304 0.035 Uiso 1 1 calc R . . . .
C9 C -0.0098(3) 0.2725(2) 1.0162(2) 0.0401(7) Uani 1 1 d . . . . .
H9A H -0.090027 0.220883 0.994168 0.060 Uiso 1 1 calc GR . . . .
H9B H -0.005452 0.343654 1.066047 0.060 Uiso 1 1 calc GR . . . .
H9C H 0.035630 0.240992 1.043587 0.060 Uiso 1 1 calc GR . . . .
C29 C 0.7453(2) 0.1907(2) 0.21652(19) 0.0379(7) Uani 1 1 d . . . . .
H29A H 0.778576 0.166621 0.157906 0.045 Uiso 1 1 calc R . . . .
H29B H 0.661757 0.168959 0.195433 0.045 Uiso 1 1 calc R . . . .
C14 C 0.7200(2) 0.2818(3) 0.6388(2) 0.0388(7) Uani 1 1 d . . . . .
H14A H 0.789868 0.264486 0.626948 0.047 Uiso 1 1 calc R . . . .
H14B H 0.685370 0.248511 0.683094 0.047 Uiso 1 1 calc R . . . .
C15 C 0.7542(2) 0.4051(3) 0.68807(18) 0.0388(7) Uani 1 1 d . . . . .
H15A H 0.684975 0.424437 0.695305 0.047 Uiso 1 1 calc R . . . .
H15B H 0.800830 0.433346 0.753619 0.047 Uiso 1 1 calc R . . . .
C20 C 0.5199(2) 0.2172(2) 0.5618(2) 0.0355(7) Uani 1 1 d . . . . .
H20A H 0.522663 0.285585 0.616145 0.043 Uiso 1 1 calc R . . . .
H20B H 0.488751 0.154344 0.580945 0.043 Uiso 1 1 calc R . . . .
C30 C 0.7958(3) 0.3640(3) 0.20633(19) 0.0442(8) Uani 1 1 d . . . . .
H30A H 0.716039 0.340075 0.172417 0.053 Uiso 1 1 calc R . . . .
H30B H 0.842505 0.343967 0.156687 0.053 Uiso 1 1 calc R . . . .
C31 C 0.8426(3) 0.4865(3) 0.2638(2) 0.0462(8) Uani 1 1 d . . . . .
H31A H 0.919401 0.508430 0.302205 0.055 Uiso 1 1 calc R . . . .
H31B H 0.852389 0.523669 0.218504 0.055 Uiso 1 1 calc R . . . .
C7 C 0.1354(2) 0.0343(2) 0.9528(2) 0.0321(6) Uani 1 1 d . . . . .
H7A H 0.084087 0.069298 0.938882 0.048 Uiso 1 1 calc GR . . . .
H7B H 0.114261 0.011549 1.005551 0.048 Uiso 1 1 calc GR . . . .
H7C H 0.128282 -0.031160 0.894418 0.048 Uiso 1 1 calc GR . . . .
C4 C 0.4998(2) 0.1217(2) 0.7879(2) 0.0449(8) Uani 1 1 d . . . . .
H4A H 0.492270 0.060231 0.807072 0.067 Uiso 1 1 calc GR . . . .
H4B H 0.578937 0.153795 0.780280 0.067 Uiso 1 1 calc GR . . . .
H4C H 0.447227 0.093915 0.726083 0.067 Uiso 1 1 calc GR . . . .
C16 C 0.8722(2) 0.5717(2) 0.6820(2) 0.0398(7) Uani 1 1 d . . . . .
H16A H 0.924810 0.590351 0.742044 0.048 Uiso 1 1 calc R . . . .
H16B H 0.812878 0.604044 0.700618 0.048 Uiso 1 1 calc R . . . .
C13 C -0.0733(3) 0.1021(2) 0.62241(19) 0.0394(7) Uani 1 1 d . . . . .
H13A H -0.084269 0.172896 0.639386 0.059 Uiso 1 1 calc GR . . . .
H13B H -0.139954 0.041753 0.574687 0.059 Uiso 1 1 calc GR . . . .
H13C H -0.003948 0.105696 0.594655 0.059 Uiso 1 1 calc GR . . . .
C19 C 0.8326(3) 0.6412(2) 0.3997(2) 0.0444(8) Uani 1 1 d . . . . .
H19A H 0.777081 0.674090 0.429040 0.053 Uiso 1 1 calc R . . . .
H19B H 0.873440 0.684505 0.364201 0.053 Uiso 1 1 calc R . . . .
C17 C 0.9368(2) 0.6189(2) 0.6197(2) 0.0453(8) Uani 1 1 d . . . . .
H17A H 0.979673 0.699676 0.657093 0.054 Uiso 1 1 calc R . . . .
H17B H 0.992836 0.583227 0.597802 0.054 Uiso 1 1 calc R . . . .
C18 C 0.9179(2) 0.6523(2) 0.4792(3) 0.0481(8) Uani 1 1 d . . . . .
H18A H 0.971857 0.616613 0.450945 0.058 Uiso 1 1 calc R . . . .
H18B H 0.962638 0.732020 0.519807 0.058 Uiso 1 1 calc R . . . .
C26 C 0.6421(2) 0.1198(2) 0.4888(2) 0.0396(7) Uani 1 1 d . . . . .
H26A H 0.567042 0.071445 0.444387 0.048 Uiso 1 1 calc R . . . .
H26B H 0.654303 0.085416 0.533298 0.048 Uiso 1 1 calc R . . . .
C12 C -0.1991(2) 0.0512(3) 0.7757(2) 0.0501(8) Uani 1 1 d . . . . .
H12A H -0.196637 0.027143 0.828802 0.075 Uiso 1 1 calc GR . . . .
H12B H -0.260527 -0.006490 0.721254 0.075 Uiso 1 1 calc GR . . . .
H12C H -0.214023 0.120451 0.798410 0.075 Uiso 1 1 calc GR . . . .
C2 C 0.5763(3) 0.2867(3) 0.9949(3) 0.0697(12) Uani 1 1 d . . . . .
H2A H 0.558807 0.341030 1.049222 0.105 Uiso 1 1 calc GR . . . .
H2B H 0.651448 0.322668 0.982268 0.105 Uiso 1 1 calc GR . . . .
H2C H 0.577692 0.225266 1.011446 0.105 Uiso 1 1 calc GR . . . .


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 N1 1.9515(18) . ?
Co1 N2 1.9529(18) . ?
Co1 C1 1.760(2) . ?
K1 O4 2.8271(16) . ?
K1 O5 2.7987(16) . ?
K1 O6 2.7735(16) . ?
K1 O7 2.8180(16) . ?
K1 O2 2.8635(17) . ?
K1 O3 2.8520(17) . ?
K1 N3 3.040(2) . ?
K1 N4 3.008(2) . ?
Si3 N2 1.6995(19) . ?
Si3 C10 1.890(3) . ?
Si3 C8 1.870(3) . ?
Si3 C9 1.874(3) . ?
Si2 N1 1.7065(19) . ?
Si2 C5 1.890(3) . ?
Si2 C6 1.879(3) . ?
Si2 C7 1.872(3) . ?
Si1 N1 1.709(2) . ?
Si1 C3 1.876(3) . ?
Si1 C4 1.876(3) . ?
Si1 C2 1.871(3) . ?
Si4 N2 1.700(2) . ?
Si4 C11 1.872(3) . ?
Si4 C13 1.878(3) . ?
Si4 C12 1.882(3) . ?
O4 C21 1.425(3) . ?
O4 C22 1.430(3) . ?
O5 C23 1.419(3) . ?
O5 C24 1.428(3) . ?
O6 C27 1.428(3) . ?
O6 C28 1.423(3) . ?
O7 C29 1.424(3) . ?
O7 C30 1.427(3) . ?
O2 C15 1.422(3) . ?
O2 C16 1.420(3) . ?
O3 C17 1.430(3) . ?
O3 C18 1.421(4) . ?
O1 C1 1.167(3) . ?
N3 C14 1.471(3) . ?
N3 C20 1.481(3) . ?
N3 C26 1.464(3) . ?
N4 C25 1.471(3) . ?
N4 C31 1.475(3) . ?
N4 C19 1.459(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C22 1.487(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C20 1.501(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C26 1.501(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.499(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.486(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.493(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.487(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.470(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C18 1.494(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Co1 N2 130.50(8) . . ?
C1 Co1 N1 115.39(9) . . ?
C1 Co1 N2 114.11(9) . . ?
O4 K1 O2 100.31(5) . . ?
O4 K1 O3 124.75(5) . . ?
O4 K1 N3 61.09(5) . . ?
O4 K1 N4 119.40(5) . . ?
O5 K1 O4 59.85(5) . . ?
O5 K1 O7 93.95(5) . . ?
O5 K1 O2 136.16(5) . . ?
O5 K1 O3 98.28(5) . . ?
O5 K1 N3 120.74(5) . . ?
O5 K1 N4 59.86(5) . . ?
O6 K1 O4 92.39(5) . . ?
O6 K1 O5 118.54(5) . . ?
O6 K1 O7 60.31(5) . . ?
O6 K1 O2 99.55(5) . . ?
O6 K1 O3 138.24(5) . . ?
O6 K1 N3 59.54(5) . . ?
O6 K1 N4 121.27(6) . . ?
O7 K1 O4 128.55(5) . . ?
O7 K1 O2 125.14(5) . . ?
O7 K1 O3 100.69(6) . . ?
O7 K1 N3 119.36(5) . . ?
O7 K1 N4 61.33(5) . . ?
O2 K1 N3 60.10(6) . . ?
O2 K1 N4 118.72(6) . . ?
O3 K1 O2 59.15(5) . . ?
O3 K1 N3 118.82(6) . . ?
O3 K1 N4 59.99(6) . . ?
N4 K1 N3 178.81(6) . . ?
N2 Si3 C10 112.90(11) . . ?
N2 Si3 C8 111.27(11) . . ?
N2 Si3 C9 113.38(12) . . ?
C8 Si3 C10 106.93(12) . . ?
C8 Si3 C9 106.74(13) . . ?
C9 Si3 C10 105.14(13) . . ?
N1 Si2 C5 114.10(11) . . ?
N1 Si2 C6 113.22(12) . . ?
N1 Si2 C7 111.23(11) . . ?
C6 Si2 C5 105.11(13) . . ?
C7 Si2 C5 106.18(12) . . ?
C7 Si2 C6 106.41(14) . . ?
N1 Si1 C3 113.03(11) . . ?
N1 Si1 C4 112.24(11) . . ?
N1 Si1 C2 113.79(14) . . ?
C3 Si1 C4 107.00(13) . . ?
C2 Si1 C3 104.38(14) . . ?
C2 Si1 C4 105.73(18) . . ?
N2 Si4 C11 112.27(11) . . ?
N2 Si4 C13 112.90(11) . . ?
N2 Si4 C12 112.73(12) . . ?
C11 Si4 C13 105.03(13) . . ?
C11 Si4 C12 105.63(14) . . ?
C13 Si4 C12 107.71(15) . . ?
C21 O4 K1 114.29(13) . . ?
C21 O4 C22 111.70(18) . . ?
C22 O4 K1 112.28(13) . . ?
C23 O5 K1 117.46(13) . . ?
C23 O5 C24 112.14(17) . . ?
C24 O5 K1 118.06(13) . . ?
C27 O6 K1 115.57(14) . . ?
C28 O6 K1 118.18(14) . . ?
C28 O6 C27 112.23(19) . . ?
C29 O7 K1 109.73(14) . . ?
C29 O7 C30 111.3(2) . . ?
C30 O7 K1 115.89(14) . . ?
C15 O2 K1 114.32(14) . . ?
C16 O2 K1 115.52(15) . . ?
C16 O2 C15 111.7(2) . . ?
C17 O3 K1 114.41(15) . . ?
C18 O3 K1 115.95(16) . . ?
C18 O3 C17 111.1(2) . . ?
Si2 N1 Co1 117.99(10) . . ?
Si2 N1 Si1 125.91(11) . . ?
Si1 N1 Co1 116.07(10) . . ?
Si3 N2 Co1 117.20(10) . . ?
Si3 N2 Si4 126.24(11) . . ?
Si4 N2 Co1 115.70(10) . . ?
C14 N3 K1 109.03(15) . . ?
C14 N3 C20 111.2(2) . . ?
C20 N3 K1 107.19(14) . . ?
C26 N3 K1 110.08(15) . . ?
C26 N3 C14 109.4(2) . . ?
C26 N3 C20 110.0(2) . . ?
C25 N4 K1 110.50(14) . . ?
C25 N4 C31 109.5(2) . . ?
C31 N4 K1 107.04(14) . . ?
C19 N4 K1 110.18(16) . . ?
C19 N4 C25 109.3(2) . . ?
C19 N4 C31 110.2(2) . . ?
O1 C1 Co1 177.4(2) . . ?
O5 C23 H23A 110.0 . . ?
O5 C23 H23B 110.0 . . ?
O5 C23 C22 108.51(19) . . ?
H23A C23 H23B 108.4 . . ?
C22 C23 H23A 110.0 . . ?
C22 C23 H23B 110.0 . . ?
O4 C21 H21A 109.8 . . ?
O4 C21 H21B 109.8 . . ?
O4 C21 C20 109.3(2) . . ?
H21A C21 H21B 108.3 . . ?
C20 C21 H21A 109.8 . . ?
C20 C21 H21B 109.8 . . ?
O6 C27 H27A 110.1 . . ?
O6 C27 H27B 110.1 . . ?
O6 C27 C26 107.9(2) . . ?
H27A C27 H27B 108.4 . . ?
C26 C27 H27A 110.1 . . ?
C26 C27 H27B 110.1 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C24 H24A 109.9 . . ?
O5 C24 H24B 109.9 . . ?
O5 C24 C25 108.71(19) . . ?
H24A C24 H24B 108.3 . . ?
C25 C24 H24A 109.9 . . ?
C25 C24 H24B 109.9 . . ?
Si3 C8 H8A 109.5 . . ?
Si3 C8 H8B 109.5 . . ?
Si3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O6 C28 H28A 109.9 . . ?
O6 C28 H28B 109.9 . . ?
O6 C28 C29 109.0(2) . . ?
H28A C28 H28B 108.3 . . ?
C29 C28 H28A 109.9 . . ?
C29 C28 H28B 109.9 . . ?
N4 C25 C24 113.5(2) . . ?
N4 C25 H25A 108.9 . . ?
N4 C25 H25B 108.9 . . ?
C24 C25 H25A 108.9 . . ?
C24 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si4 C11 H11A 109.5 . . ?
Si4 C11 H11B 109.5 . . ?
Si4 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O4 C22 C23 109.19(19) . . ?
O4 C22 H22A 109.8 . . ?
O4 C22 H22B 109.8 . . ?
C23 C22 H22A 109.8 . . ?
C23 C22 H22B 109.8 . . ?
H22A C22 H22B 108.3 . . ?
Si3 C9 H9A 109.5 . . ?
Si3 C9 H9B 109.5 . . ?
Si3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O7 C29 C28 109.4(2) . . ?
O7 C29 H29A 109.8 . . ?
O7 C29 H29B 109.8 . . ?
C28 C29 H29A 109.8 . . ?
C28 C29 H29B 109.8 . . ?
H29A C29 H29B 108.2 . . ?
N3 C14 H14A 108.6 . . ?
N3 C14 H14B 108.6 . . ?
N3 C14 C15 114.5(2) . . ?
H14A C14 H14B 107.6 . . ?
C15 C14 H14A 108.6 . . ?
C15 C14 H14B 108.6 . . ?
O2 C15 C14 108.9(2) . . ?
O2 C15 H15A 109.9 . . ?
O2 C15 H15B 109.9 . . ?
C14 C15 H15A 109.9 . . ?
C14 C15 H15B 109.9 . . ?
H15A C15 H15B 108.3 . . ?
N3 C20 C21 113.2(2) . . ?
N3 C20 H20A 108.9 . . ?
N3 C20 H20B 108.9 . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
O7 C30 H30A 109.6 . . ?
O7 C30 H30B 109.6 . . ?
O7 C30 C31 110.2(2) . . ?
H30A C30 H30B 108.1 . . ?
C31 C30 H30A 109.6 . . ?
C31 C30 H30B 109.6 . . ?
N4 C31 C30 113.8(2) . . ?
N4 C31 H31A 108.8 . . ?
N4 C31 H31B 108.8 . . ?
C30 C31 H31A 108.8 . . ?
C30 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O2 C16 H16A 109.7 . . ?
O2 C16 H16B 109.7 . . ?
O2 C16 C17 109.6(2) . . ?
H16A C16 H16B 108.2 . . ?
C17 C16 H16A 109.7 . . ?
C17 C16 H16B 109.7 . . ?
Si4 C13 H13A 109.5 . . ?
Si4 C13 H13B 109.5 . . ?
Si4 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N4 C19 H19A 108.8 . . ?
N4 C19 H19B 108.8 . . ?
N4 C19 C18 113.9(2) . . ?
H19A C19 H19B 107.7 . . ?
C18 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
O3 C17 C16 109.7(2) . . ?
O3 C17 H17A 109.7 . . ?
O3 C17 H17B 109.7 . . ?
C16 C17 H17A 109.7 . . ?
C16 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
O3 C18 C19 109.4(2) . . ?
O3 C18 H18A 109.8 . . ?
O3 C18 H18B 109.8 . . ?
C19 C18 H18A 109.8 . . ?
C19 C18 H18B 109.8 . . ?
H18A C18 H18B 108.2 . . ?
N3 C26 C27 113.1(2) . . ?
N3 C26 H26A 109.0 . . ?
N3 C26 H26B 109.0 . . ?
C27 C26 H26A 109.0 . . ?
C27 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?
Si4 C12 H12A 109.5 . . ?
Si4 C12 H12B 109.5 . . ?
Si4 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

