# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2016

####################################################################### 
# 
# 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_1-298K
_database_code_depnum_ccdc_archive 'CCDC 1500800'
_audit_update_record             
;
2016-08-24 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Co K0.77 N6 Rb0.23, 2(C H6 N)'
_chemical_formula_sum            'C8 H12 Co K0.77 N8 Rb0.23'
_chemical_formula_weight         328.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.698(3)
_cell_length_b                   7.8637(16)
_cell_length_c                   13.681(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.65(3)
_cell_angle_gamma                90
_cell_volume                     1396.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1589
_cell_measurement_theta_min      0.491
_cell_measurement_theta_max      0.532

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_F_000             664.6
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_absorpt_coefficient_mu    2.251
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku, SCXmini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4749
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.029
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1589
_reflns_number_gt                1450
_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       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0360P)²+0.5597P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0251(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1589
_refine_ls_number_parameters     87
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0770
_refine_ls_wR_factor_gt          0.0755
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.68648(15) 0.1265(2) 0.87754(14) 0.0282(4) Uani 1 1 d . . . . .
C2 C 0.86559(15) 0.2916(2) 0.95607(14) 0.0241(4) Uani 1 1 d . . . . .
C3 C 0.81002(14) 0.0449(2) 1.06452(14) 0.0251(4) Uani 1 1 d . . . . .
C4 C 0.0978(2) 0.1297(3) 0.1424(2) 0.0517(6) Uani 1 1 d . . . . .
H4D H 0.1495 0.0953 0.2050 0.078 Uiso 1 1 calc R U . . .
H4E H 0.0884 0.0418 0.0915 0.078 Uiso 1 1 calc R U . . .
H4F H 0.0340 0.1493 0.1557 0.078 Uiso 1 1 calc R U . . .
Co1 Co 0.7500 0.2500 1.0000 0.01845(15) Uani 1 2 d S . P . .
K1 K 0.5000 -0.21453(7) 0.7500 0.03047(17) Uani 0.77 2 d S T P . .
N1 N 0.64979(17) 0.0505(3) 0.80383(14) 0.0499(6) Uani 1 1 d . . . . .
N2 N 0.93561(14) 0.3186(2) 0.93017(14) 0.0356(4) Uani 1 1 d . . . . .
N3 N 0.84323(14) -0.0813(2) 1.10225(15) 0.0394(5) Uani 1 1 d . . . . .
N4 N 0.13040(13) 0.2861(2) 0.10437(15) 0.0334(4) Uani 1 1 d . . . . .
H4A H 0.1345 0.3696 0.1494 0.050 Uiso 1 1 calc R U . . .
H4B H 0.0847 0.3138 0.0439 0.050 Uiso 1 1 calc R U . . .
H4C H 0.1918 0.2702 0.0966 0.050 Uiso 1 1 calc R U . . .
Rb1 Rb 0.5000 -0.21453(7) 0.7500 0.03047(17) Uani 0.23 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.142(3) . ?
C1 Co1 1.891(2) . ?
C2 N2 1.144(2) . ?
C2 Co1 1.893(2) . ?
C3 N3 1.144(2) . ?
C3 Co1 1.8955(19) . ?
C4 N4 1.460(3) . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?
C4 H4F 0.9600 . ?
Co1 C1 1.891(2) 7_657 ?
Co1 C2 1.893(2) 7_657 ?
Co1 C3 1.8955(19) 7_657 ?
K1 N1 2.851(2) 2_656 ?
K1 N1 2.851(2) . ?
K1 N2 2.8831(19) 3_445 ?
K1 N2 2.8831(19) 4_646 ?
K1 N3 2.915(2) 8_445 ?
K1 N3 2.9152(19) 7_647 ?
N2 Rb1 2.8830(19) 3 ?
N2 K1 2.8830(19) 3 ?
N3 Rb1 2.9152(19) 7_647 ?
N3 K1 2.9152(19) 7_647 ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?

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 C1 Co1 178.7(2) . . ?
N2 C2 Co1 179.14(18) . . ?
N3 C3 Co1 177.82(18) . . ?
N4 C4 H4D 109.5 . . ?
N4 C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
N4 C4 H4F 109.5 . . ?
H4D C4 H4F 109.5 . . ?
H4E C4 H4F 109.5 . . ?
C1 Co1 C1 180.00(8) . 7_657 ?
C1 Co1 C2 89.89(9) . 7_657 ?
C1 Co1 C2 90.11(9) 7_657 7_657 ?
C1 Co1 C2 90.11(9) . . ?
C1 Co1 C2 89.89(9) 7_657 . ?
C2 Co1 C2 180.0 7_657 . ?
C1 Co1 C3 90.93(8) . 7_657 ?
C1 Co1 C3 89.07(8) 7_657 7_657 ?
C2 Co1 C3 90.72(8) 7_657 7_657 ?
C2 Co1 C3 89.28(8) . 7_657 ?
C1 Co1 C3 89.07(8) . . ?
C1 Co1 C3 90.93(8) 7_657 . ?
C2 Co1 C3 89.28(8) 7_657 . ?
C2 Co1 C3 90.72(8) . . ?
C3 Co1 C3 180.00(6) 7_657 . ?
N1 K1 N1 86.07(10) 2_656 . ?
N1 K1 N2 76.30(6) 2_656 3_445 ?
N1 K1 N2 96.01(6) . 3_445 ?
N1 K1 N2 96.01(6) 2_656 4_646 ?
N1 K1 N2 76.30(6) . 4_646 ?
N2 K1 N2 169.63(8) 3_445 4_646 ?
N1 K1 N3 85.05(6) 2_656 8_445 ?
N1 K1 N3 153.04(5) . 8_445 ?
N2 K1 N3 106.48(6) 3_445 8_445 ?
N2 K1 N3 79.39(5) 4_646 8_445 ?
N1 K1 N3 153.04(6) 2_656 7_647 ?
N1 K1 N3 85.05(6) . 7_647 ?
N2 K1 N3 79.39(5) 3_445 7_647 ?
N2 K1 N3 106.48(5) 4_646 7_647 ?
N3 K1 N3 113.17(8) 8_445 7_647 ?
C1 N1 K1 133.49(16) . . ?
C2 N2 Rb1 139.84(16) . 3 ?
C2 N2 K1 139.84(16) . 3 ?
Rb1 N2 K1 0.0 3 3 ?
C3 N3 Rb1 152.78(16) . 7_647 ?
C3 N3 K1 152.78(16) . 7_647 ?
Rb1 N3 K1 0.0 7_647 7_647 ?
C4 N4 H4A 109.5 . . ?
C4 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C4 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?


_refine_diff_density_max         0.478
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.111


####################################################################### 
# 
# 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_2-298K
_database_code_depnum_ccdc_archive 'CCDC 1500801'
_audit_update_record             
;
2016-08-24 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Co K0.69 N6 Rb0.31, 2(C H6 N)'
_chemical_formula_sum            'C8 H12 Co K0.69 N8 Rb0.31'
_chemical_formula_weight         332.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.711(3)
_cell_length_b                   7.8880(16)
_cell_length_c                   13.717(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.73(3)
_cell_angle_gamma                90
_cell_volume                     1405.0(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1606
_cell_measurement_theta_min      0.455
_cell_measurement_theta_max      0.498

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_F_000             670.3
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_absorpt_coefficient_mu    2.489
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku, SCXmini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4754
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.022
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1606
_reflns_number_gt                1467
_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       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0873P)²+9.4014P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1601
_refine_ls_number_parameters     87
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0571
_refine_ls_wR_factor_ref         0.1727
_refine_ls_wR_factor_gt          0.1694
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6859(3) 0.1249(5) 0.8776(3) 0.0273(9) Uani 1 1 d . . . . .
C2 C 0.8655(3) 0.2916(5) 0.9553(3) 0.0235(8) Uani 1 1 d . . . . .
C3 C 0.8106(3) 0.0448(5) 1.0651(3) 0.0239(8) Uani 1 1 d . . . . .
C4 C 0.0980(5) 0.1310(7) 0.1425(5) 0.0506(14) Uani 1 1 d . . . . .
H4D H 0.1460 0.1038 0.2087 0.076 Uiso 1 1 calc R U . . .
H4E H 0.0968 0.0408 0.0951 0.076 Uiso 1 1 calc R U . . .
H4F H 0.0305 0.1448 0.1482 0.076 Uiso 1 1 calc R U . . .
Co1 Co 0.7500 0.2500 1.0000 0.0172(3) Uani 1 2 d S . P . .
K1 K 0.5000 -0.21527(17) 0.7500 0.0408(4) Uani 0.69 2 d S T P . .
N1 N 0.6487(4) 0.0489(6) 0.8048(3) 0.0485(12) Uani 1 1 d . . . . .
N2 N 0.9349(3) 0.3182(5) 0.9287(3) 0.0336(9) Uani 1 1 d . . . . .
N3 N 0.8437(3) -0.0808(5) 1.1033(3) 0.0383(10) Uani 1 1 d . . . . .
N4 N 0.1295(3) 0.2886(6) 0.1048(3) 0.0340(9) Uani 1 1 d . . . . .
H4A H 0.1371 0.3696 0.1519 0.051 Uiso 1 1 calc R U . . .
H4B H 0.0815 0.3197 0.0467 0.051 Uiso 1 1 calc R U . . .
H4C H 0.1890 0.2725 0.0931 0.051 Uiso 1 1 calc R U . . .
Rb1 Rb 0.5000 -0.21527(17) 0.7500 0.0408(4) Uani 0.31 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.136(6) . ?
C1 Co1 1.902(4) . ?
C2 N2 1.143(6) . ?
C2 Co1 1.901(4) . ?
C3 N3 1.144(6) . ?
C3 Co1 1.906(4) . ?
C4 N4 1.464(7) . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?
C4 H4F 0.9600 . ?
Co1 C2 1.901(4) 7_657 ?
Co1 C1 1.902(4) 7_657 ?
Co1 C3 1.906(4) 7_657 ?
K1 N1 2.842(4) 2_656 ?
K1 N1 2.842(5) . ?
K1 N2 2.877(4) 3_445 ?
K1 N2 2.877(4) 4_646 ?
K1 N3 2.909(4) 8_445 ?
K1 N3 2.909(4) 7_647 ?
N2 Rb1 2.877(4) 3 ?
N2 K1 2.877(4) 3 ?
N3 Rb1 2.909(4) 7_647 ?
N3 K1 2.909(4) 7_647 ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?

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 C1 Co1 179.2(5) . . ?
N2 C2 Co1 179.4(4) . . ?
N3 C3 Co1 177.6(4) . . ?
N4 C4 H4D 109.5 . . ?
N4 C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
N4 C4 H4F 109.5 . . ?
H4D C4 H4F 109.5 . . ?
H4E C4 H4F 109.5 . . ?
C2 Co1 C2 180.0 . 7_657 ?
C2 Co1 C1 89.94(18) . 7_657 ?
C2 Co1 C1 90.06(18) 7_657 7_657 ?
C2 Co1 C1 90.06(18) . . ?
C2 Co1 C1 89.94(18) 7_657 . ?
C1 Co1 C1 180.0 7_657 . ?
C2 Co1 C3 90.85(17) . . ?
C2 Co1 C3 89.15(17) 7_657 . ?
C1 Co1 C3 91.07(17) 7_657 . ?
C1 Co1 C3 88.93(18) . . ?
C2 Co1 C3 89.15(17) . 7_657 ?
C2 Co1 C3 90.85(17) 7_657 7_657 ?
C1 Co1 C3 88.93(18) 7_657 7_657 ?
C1 Co1 C3 91.07(17) . 7_657 ?
C3 Co1 C3 180.0(2) . 7_657 ?
N1 K1 N1 85.7(2) 2_656 . ?
N1 K1 N2 76.46(12) 2_656 3_445 ?
N1 K1 N2 95.72(13) . 3_445 ?
N1 K1 N2 95.72(13) 2_656 4_646 ?
N1 K1 N2 76.46(12) . 4_646 ?
N2 K1 N2 169.49(18) 3_445 4_646 ?
N1 K1 N3 85.18(14) 2_656 8_445 ?
N1 K1 N3 153.52(13) . 8_445 ?
N2 K1 N3 106.18(12) 3_445 8_445 ?
N2 K1 N3 79.79(12) 4_646 8_445 ?
N1 K1 N3 153.52(13) 2_656 7_647 ?
N1 K1 N3 85.18(14) . 7_647 ?
N2 K1 N3 79.79(12) 3_445 7_647 ?
N2 K1 N3 106.18(12) 4_646 7_647 ?
N3 K1 N3 112.84(19) 8_445 7_647 ?
C1 N1 K1 134.6(4) . . ?
C2 N2 Rb1 140.6(3) . 3 ?
C2 N2 K1 140.6(3) . 3 ?
Rb1 N2 K1 0.0 3 3 ?
C3 N3 Rb1 153.0(4) . 7_647 ?
C3 N3 K1 153.0(4) . 7_647 ?
Rb1 N3 K1 0.0 7_647 7_647 ?
C4 N4 H4A 109.5 . . ?
C4 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C4 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?


_refine_diff_density_max         0.796
_refine_diff_density_min         -1.913
_refine_diff_density_rms         0.154


####################################################################### 
# 
# 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_3-298K
_database_code_depnum_ccdc_archive 'CCDC 1500802'
_audit_update_record             
;
2016-08-24 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Co K0.66 N6 Rb0.34, 2(C H6 N)'
_chemical_formula_sum            'C8 H12 Co K0.66 N8 Rb0.34'
_chemical_formula_weight         334.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.720(3)
_cell_length_b                   7.9003(16)
_cell_length_c                   13.729(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.62(3)
_cell_angle_gamma                90
_cell_volume                     1410.2(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1609
_cell_measurement_theta_min      0.456
_cell_measurement_theta_max      0.486

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_F_000             672.5
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_absorpt_coefficient_mu    2.574
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku, SCXmini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4726
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.017
_diffrn_reflns_theta_max         27.453
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1609
_reflns_number_gt                1448
_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       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0841P)²+11.3268P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.021(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1578
_refine_ls_number_parameters     87
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0547
_refine_ls_wR_factor_ref         0.1710
_refine_ls_wR_factor_gt          0.1678
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.124
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6861(3) 0.1253(6) 0.8779(3) 0.0262(9) Uani 1 1 d . . . . .
C2 C 0.8652(3) 0.2914(5) 0.9552(3) 0.0220(8) Uani 1 1 d . . . . .
C3 C 0.8106(3) 0.0452(6) 1.0653(3) 0.0231(9) Uani 1 1 d . . . . .
C4 C 0.0979(5) 0.1310(8) 0.1426(5) 0.0489(14) Uani 1 1 d . . . . .
H4D H 0.1446 0.1055 0.2096 0.073 Uiso 1 1 calc R U . . .
H4E H 0.0985 0.0402 0.0963 0.073 Uiso 1 1 calc R U . . .
H4F H 0.0297 0.1442 0.1465 0.073 Uiso 1 1 calc R U . . .
Co1 Co 0.7500 0.2500 1.0000 0.0164(3) Uani 1 2 d S . P . .
K1 K 0.5000 -0.21523(17) 0.7500 0.0421(4) Uani 0.66 2 d S T P . .
N1 N 0.6486(4) 0.0492(6) 0.8049(3) 0.0479(13) Uani 1 1 d . . . . .
N2 N 0.9351(3) 0.3186(6) 0.9287(3) 0.0325(9) Uani 1 1 d . . . . .
N3 N 0.8439(3) -0.0811(6) 1.1031(3) 0.0368(10) Uani 1 1 d . . . . .
N4 N 0.1298(3) 0.2884(6) 0.1049(3) 0.0331(9) Uani 1 1 d . . . . .
H4A H 0.1333 0.3711 0.1499 0.050 Uiso 1 1 calc R U . . .
H4B H 0.0841 0.3158 0.0446 0.050 Uiso 1 1 calc R U . . .
H4C H 0.1913 0.2739 0.0972 0.050 Uiso 1 1 calc R U . . .
Rb1 Rb 0.5000 -0.21523(17) 0.7500 0.0421(4) Uani 0.34 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.141(6) . ?
C1 Co1 1.900(4) . ?
C2 N2 1.148(6) . ?
C2 Co1 1.899(4) . ?
C3 N3 1.150(6) . ?
C3 Co1 1.907(4) . ?
C4 N4 1.467(7) . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?
C4 H4F 0.9600 . ?
Co1 C2 1.899(4) 7_657 ?
Co1 C1 1.900(4) 7_657 ?
Co1 C3 1.907(4) 7_657 ?
K1 N1 2.847(5) . ?
K1 N1 2.847(5) 2_656 ?
K1 N2 2.878(4) 3_445 ?
K1 N2 2.878(4) 4_646 ?
K1 N3 2.913(4) 8_445 ?
K1 N3 2.913(4) 7_647 ?
N2 Rb1 2.878(4) 3 ?
N2 K1 2.878(4) 3 ?
N3 Rb1 2.913(4) 7_647 ?
N3 K1 2.913(4) 7_647 ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?

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 C1 Co1 179.3(5) . . ?
N2 C2 Co1 179.0(4) . . ?
N3 C3 Co1 177.6(4) . . ?
N4 C4 H4D 109.5 . . ?
N4 C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
N4 C4 H4F 109.5 . . ?
H4D C4 H4F 109.5 . . ?
H4E C4 H4F 109.5 . . ?
C2 Co1 C2 180.0(2) 7_657 . ?
C2 Co1 C1 89.97(19) 7_657 . ?
C2 Co1 C1 90.03(19) . . ?
C2 Co1 C1 90.03(19) 7_657 7_657 ?
C2 Co1 C1 89.97(19) . 7_657 ?
C1 Co1 C1 180.0 . 7_657 ?
C2 Co1 C3 89.12(18) 7_657 . ?
C2 Co1 C3 90.88(17) . . ?
C1 Co1 C3 89.08(18) . . ?
C1 Co1 C3 90.92(18) 7_657 . ?
C2 Co1 C3 90.88(17) 7_657 7_657 ?
C2 Co1 C3 89.12(18) . 7_657 ?
C1 Co1 C3 90.92(18) . 7_657 ?
C1 Co1 C3 89.08(18) 7_657 7_657 ?
C3 Co1 C3 180.0 . 7_657 ?
N1 K1 N1 85.6(2) . 2_656 ?
N1 K1 N2 95.56(14) . 3_445 ?
N1 K1 N2 76.53(13) 2_656 3_445 ?
N1 K1 N2 76.53(13) . 4_646 ?
N1 K1 N2 95.56(14) 2_656 4_646 ?
N2 K1 N2 169.35(19) 3_445 4_646 ?
N1 K1 N3 153.43(13) . 8_445 ?
N1 K1 N3 85.18(14) 2_656 8_445 ?
N2 K1 N3 106.41(13) 3_445 8_445 ?
N2 K1 N3 79.63(13) 4_646 8_445 ?
N1 K1 N3 85.18(14) . 7_647 ?
N1 K1 N3 153.43(13) 2_656 7_647 ?
N2 K1 N3 79.63(12) 3_445 7_647 ?
N2 K1 N3 106.41(13) 4_646 7_647 ?
N3 K1 N3 112.95(19) 8_445 7_647 ?
C1 N1 K1 134.6(4) . . ?
C2 N2 Rb1 140.3(4) . 3 ?
C2 N2 K1 140.3(4) . 3 ?
Rb1 N2 K1 0.0 3 3 ?
C3 N3 Rb1 152.9(4) . 7_647 ?
C3 N3 K1 152.9(4) . 7_647 ?
Rb1 N3 K1 0.0 7_647 7_647 ?
C4 N4 H4A 109.5 . . ?
C4 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C4 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?

_refine_diff_density_max         0.717
_refine_diff_density_min         -2.035
_refine_diff_density_rms         0.163


####################################################################### 
# 
# 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_4-298K
_database_code_depnum_ccdc_archive 'CCDC 1500803'
_audit_update_record             
;
2016-08-24 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Co K0.56 N6 Rb0.44, 2(C H6 N)'
_chemical_formula_sum            'C8 H12 Co K0.56 N8 Rb0.44'
_chemical_formula_weight         338.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.754(3)
_cell_length_b                   7.8831(16)
_cell_length_c                   13.749(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.47(3)
_cell_angle_gamma                90
_cell_volume                     1413.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1616
_cell_measurement_theta_min      0.414
_cell_measurement_theta_max      0.447

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_F_000             679.7
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_absorpt_coefficient_mu    2.879
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku, SCXmini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4808
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.019
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1616
_reflns_number_gt                1472
_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       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0980P)²+2.0840P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.020(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1611
_refine_ls_number_parameters     87
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1573
_refine_ls_wR_factor_gt          0.1545
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_restrained_S_all      1.187
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6869(3) 0.1275(4) 0.8772(3) 0.0290(7) Uani 1 1 d . . . . .
C2 C 0.8656(3) 0.2932(4) 0.9569(2) 0.0247(7) Uani 1 1 d . . . . .
C3 C 0.8098(2) 0.0439(4) 1.0640(2) 0.0255(7) Uani 1 1 d . . . . .
C4 C 0.0974(4) 0.1289(6) 0.1420(4) 0.0513(11) Uani 1 1 d . . . . .
H4D H 0.1499 0.0920 0.2027 0.077 Uiso 1 1 calc R U . . .
H4E H 0.0853 0.0422 0.0904 0.077 Uiso 1 1 calc R U . . .
H4F H 0.0354 0.1503 0.1578 0.077 Uiso 1 1 calc R U . . .
Co1 Co 0.7500 0.2500 1.0000 0.0185(3) Uani 1 2 d S . P . .
K1 K 0.5000 -0.21422(11) 0.7500 0.0352(3) Uani 0.56 2 d S T P . .
N1 N 0.6503(3) 0.0527(5) 0.8047(3) 0.0510(10) Uani 1 1 d . . . . .
N2 N 0.9356(2) 0.3201(4) 0.9309(2) 0.0354(7) Uani 1 1 d . . . . .
N3 N 0.8426(3) -0.0821(4) 1.1017(3) 0.0410(8) Uani 1 1 d . . . . .
N4 N 0.1306(2) 0.2855(4) 0.1035(3) 0.0322(7) Uani 1 1 d . . . . .
H4A H 0.1323 0.3701 0.1469 0.048 Uiso 1 1 calc R U . . .
H4B H 0.0868 0.3107 0.0422 0.048 Uiso 1 1 calc R U . . .
H4C H 0.1929 0.2704 0.0983 0.048 Uiso 1 1 calc R U . . .
Rb1 Rb 0.5000 -0.21422(11) 0.7500 0.0352(3) Uani 0.44 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.130(5) . ?
C1 Co1 1.900(3) . ?
C2 N2 1.148(4) . ?
C2 Co1 1.895(3) . ?
C3 N3 1.145(5) . ?
C3 Co1 1.906(3) . ?
C4 N4 1.471(5) . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?
C4 H4F 0.9600 . ?
Co1 C2 1.895(3) 7_657 ?
Co1 C1 1.900(3) 7_657 ?
Co1 C3 1.906(3) 7_657 ?
K1 N1 2.877(4) 2_656 ?
K1 N1 2.877(4) . ?
K1 N2 2.905(3) 4_646 ?
K1 N2 2.905(3) 3_445 ?
K1 N3 2.936(3) 8_445 ?
K1 N3 2.936(3) 7_647 ?
N2 Rb1 2.905(3) 3 ?
N2 K1 2.905(3) 3 ?
N3 Rb1 2.936(3) 7_647 ?
N3 K1 2.936(3) 7_647 ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?

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 C1 Co1 179.0(4) . . ?
N2 C2 Co1 179.7(3) . . ?
N3 C3 Co1 177.7(3) . . ?
N4 C4 H4D 109.5 . . ?
N4 C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
N4 C4 H4F 109.5 . . ?
H4D C4 H4F 109.5 . . ?
H4E C4 H4F 109.5 . . ?
C2 Co1 C2 180.0 . 7_657 ?
C2 Co1 C1 90.30(15) . . ?
C2 Co1 C1 89.70(15) 7_657 . ?
C2 Co1 C1 89.70(15) . 7_657 ?
C2 Co1 C1 90.30(15) 7_657 7_657 ?
C1 Co1 C1 180.0 . 7_657 ?
C2 Co1 C3 90.86(14) . . ?
C2 Co1 C3 89.14(14) 7_657 . ?
C1 Co1 C3 89.19(15) . . ?
C1 Co1 C3 90.81(15) 7_657 . ?
C2 Co1 C3 89.13(14) . 7_657 ?
C2 Co1 C3 90.87(14) 7_657 7_657 ?
C1 Co1 C3 90.80(15) . 7_657 ?
C1 Co1 C3 89.20(15) 7_657 7_657 ?
C3 Co1 C3 180.0 . 7_657 ?
N1 K1 N1 86.03(18) 2_656 . ?
N1 K1 N2 95.57(10) 2_656 4_646 ?
N1 K1 N2 76.52(10) . 4_646 ?
N1 K1 N2 76.52(10) 2_656 3_445 ?
N1 K1 N2 95.58(10) . 3_445 ?
N2 K1 N2 169.32(14) 4_646 3_445 ?
N1 K1 N3 84.71(11) 2_656 8_445 ?
N1 K1 N3 153.08(10) . 8_445 ?
N2 K1 N3 79.30(10) 4_646 8_445 ?
N2 K1 N3 106.70(10) 3_445 8_445 ?
N1 K1 N3 153.08(10) 2_656 7_647 ?
N1 K1 N3 84.71(11) . 7_647 ?
N2 K1 N3 106.70(10) 4_646 7_647 ?
N2 K1 N3 79.30(9) 3_445 7_647 ?
N3 K1 N3 113.72(15) 8_445 7_647 ?
C1 N1 K1 134.0(3) . . ?
C2 N2 Rb1 139.7(3) . 3 ?
C2 N2 K1 139.7(3) . 3 ?
Rb1 N2 K1 0.0 3 3 ?
C3 N3 Rb1 152.5(3) . 7_647 ?
C3 N3 K1 152.5(3) . 7_647 ?
Rb1 N3 K1 0.0 7_647 7_647 ?
C4 N4 H4A 109.5 . . ?
C4 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C4 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?


_refine_diff_density_max         1.213
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.193


####################################################################### 
# 
# 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_5-298K
_database_code_depnum_ccdc_archive 'CCDC 1500804'
_audit_update_record             
;
2016-08-24 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Co K0.38 N6 Rb0.62, 2(C H6 N)'
_chemical_formula_sum            'C8 H12 Co K0.38 N8 Rb0.62'
_chemical_formula_weight         347.04

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.781(3)
_cell_length_b                   7.8981(16)
_cell_length_c                   13.776(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.34(3)
_cell_angle_gamma                90
_cell_volume                     1423.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1630
_cell_measurement_theta_min      0.348
_cell_measurement_theta_max      0.384

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_F_000             692.6
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_absorpt_coefficient_mu    3.419
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku, SCXmini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4832
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.013
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1630
_reflns_number_gt                1485
_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       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0724P)²+4.6075P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0038(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1628
_refine_ls_number_parameters     87
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1418
_refine_ls_wR_factor_gt          0.1385
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3660(3) 0.2067(4) 0.9576(3) 0.0241(7) Uani 1 1 d . . . . .
C2 C 0.1910(2) 0.0431(5) 0.9370(3) 0.0259(7) Uani 1 1 d . . . . .
C3 C 0.3122(3) 0.1287(5) 1.1234(3) 0.0292(8) Uani 1 1 d . . . . .
C4 C 0.5967(4) 0.3729(7) 0.1416(4) 0.0529(12) Uani 1 1 d . . . . .
H4A H 0.6476 0.4073 0.2037 0.079 Uiso 1 1 calc R U . . .
H4B H 0.5334 0.3515 0.1548 0.079 Uiso 1 1 calc R U . . .
H4C H 0.5869 0.4611 0.0915 0.079 Uiso 1 1 calc R U . . .
Co1 Co 0.2500 0.2500 1.0000 0.0186(3) Uani 1 2 d S . P . .
K1 K 0.5000 0.21321(10) 0.7500 0.0353(3) Uani 0.38 2 d S T P . .
N1 N 0.4360(2) 0.1796(5) 0.9327(3) 0.0358(8) Uani 1 1 d . . . . .
N2 N 0.1586(3) -0.0832(5) 0.9001(3) 0.0412(9) Uani 1 1 d . . . . .
N3 N 0.3481(3) 0.0552(5) 1.1973(3) 0.0495(10) Uani 1 1 d . . . . .
N4 N 0.6308(2) 0.2168(4) 0.1026(3) 0.0310(7) Uani 1 1 d . . . . .
H4D H 0.6923 0.2336 0.0963 0.047 Uiso 1 1 calc R U . . .
H4E H 0.5866 0.1906 0.0420 0.047 Uiso 1 1 calc R U . . .
H4F H 0.6339 0.1323 0.1463 0.047 Uiso 1 1 calc R U . . .
Rb1 Rb 0.5000 0.21321(10) 0.7500 0.0353(3) Uani 0.62 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.140(5) . ?
C1 Co1 1.899(4) . ?
C2 N2 1.145(5) . ?
C2 Co1 1.908(4) . ?
C3 N3 1.141(5) . ?
C3 Co1 1.904(4) . ?
C4 N4 1.479(6) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
Co1 C1 1.899(4) 7_557 ?
Co1 C3 1.904(4) 7_557 ?
Co1 C2 1.908(4) 7_557 ?
K1 N3 2.906(4) 6 ?
K1 N3 2.906(4) 5_657 ?
K1 N1 2.929(3) 2_656 ?
K1 N1 2.929(3) . ?
K1 N2 2.965(4) 3 ?
K1 N2 2.965(3) 4_556 ?
N2 Rb1 2.965(3) 3_445 ?
N2 K1 2.965(3) 3_445 ?
N3 Rb1 2.906(4) 5_657 ?
N3 K1 2.906(4) 5_657 ?
N4 H4D 0.8900 . ?
N4 H4E 0.8900 . ?
N4 H4F 0.8900 . ?

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 C1 Co1 179.4(4) . . ?
N2 C2 Co1 177.8(3) . . ?
N3 C3 Co1 179.0(4) . . ?
N4 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 Co1 C1 180.00(18) 7_557 . ?
C1 Co1 C3 89.89(15) 7_557 7_557 ?
C1 Co1 C3 90.11(15) . 7_557 ?
C1 Co1 C3 90.11(15) 7_557 . ?
C1 Co1 C3 89.89(15) . . ?
C3 Co1 C3 180.0 7_557 . ?
C1 Co1 C2 89.17(15) 7_557 7_557 ?
C1 Co1 C2 90.83(15) . 7_557 ?
C3 Co1 C2 89.03(16) 7_557 7_557 ?
C3 Co1 C2 90.98(16) . 7_557 ?
C1 Co1 C2 90.83(15) 7_557 . ?
C1 Co1 C2 89.17(15) . . ?
C3 Co1 C2 90.97(16) 7_557 . ?
C3 Co1 C2 89.03(16) . . ?
C2 Co1 C2 180.0 7_557 . ?
N3 K1 N3 86.34(18) 6 5_657 ?
N3 K1 N1 96.18(11) 6 2_656 ?
N3 K1 N1 76.13(11) 5_657 2_656 ?
N3 K1 N1 76.13(11) 6 . ?
N3 K1 N1 96.18(11) 5_657 . ?
N1 K1 N1 169.61(15) 2_656 . ?
N3 K1 N2 152.19(11) 6 3 ?
N3 K1 N2 84.63(12) 5_657 3 ?
N1 K1 N2 107.04(10) 2_656 3 ?
N1 K1 N2 78.77(10) . 3 ?
N3 K1 N2 84.63(12) 6 4_556 ?
N3 K1 N2 152.19(11) 5_657 4_556 ?
N1 K1 N2 78.77(10) 2_656 4_556 ?
N1 K1 N2 107.04(10) . 4_556 ?
N2 K1 N2 114.32(16) 3 4_556 ?
C1 N1 K1 138.8(3) . . ?
C2 N2 Rb1 151.8(3) . 3_445 ?
C2 N2 K1 151.8(3) . 3_445 ?
Rb1 N2 K1 0.0 3_445 3_445 ?
C3 N3 Rb1 132.0(3) . 5_657 ?
C3 N3 K1 132.0(3) . 5_657 ?
Rb1 N3 K1 0.0 5_657 5_657 ?
C4 N4 H4D 109.5 . . ?
C4 N4 H4E 109.5 . . ?
H4D N4 H4E 109.5 . . ?
C4 N4 H4F 109.5 . . ?
H4D N4 H4F 109.5 . . ?
H4E N4 H4F 109.5 . . ?


_refine_diff_density_max         0.665
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.206


####################################################################### 
# 
# 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_1-460K
_database_code_depnum_ccdc_archive 'CCDC 1500805'
_audit_update_record             
;
2016-08-24 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 Co2 N12, C4 N4, 0.46(Rb), 1.54(K)'
_chemical_formula_sum            'C16 Co2 K1.54 N16 Rb0.46'
_chemical_formula_weight         633.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'

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

_cell_length_a                   11.466(5)
_cell_length_b                   11.466(5)
_cell_length_c                   11.466(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1507(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    460(2)
_cell_measurement_reflns_used    121
_cell_measurement_theta_min      0.519
_cell_measurement_theta_max      0.558

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_F_000             616.5
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_absorpt_coefficient_mu    2.083
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.519
_exptl_absorpt_correction_T_max  0.558
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      460(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku, SCXmini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4020
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_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         3.077
_diffrn_reflns_theta_max         27.301
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.969
_reflns_number_total             121
_reflns_number_gt                117
_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       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1831P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.32(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         121
_refine_ls_number_parameters     15
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0929
_refine_ls_wR_factor_ref         0.2396
_refine_ls_wR_factor_gt          0.2398
_refine_ls_goodness_of_fit_ref   1.279
_refine_ls_restrained_S_all      1.229
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0000 0.0000 0.1637(14) 0.153(6) Uani 1 8 d S TU P . .
C2 C 0.7500 0.867(4) 0.2500 0.19(3) Uani 0.1667 4 d DS TU P . .
Co1 Co 0.0000 0.0000 0.0000 0.059(2) Uani 1 48 d S TU P . .
K1 K 0.0000 0.0000 0.5000 0.080(2) Uani 0.7699 48 d S TU P . .
N1 N 0.0000 0.0000 0.2567(10) 0.168(14) Uani 1 8 d S TU P . .
N2 N 0.7500 0.7500 0.2500 0.19(3) Uani 1 24 d DS TU P . .
Rb1 Rb 0.0000 0.0000 0.5000 0.080(2) Uani 0.2299 48 d S TU 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
C1 N1 1.067(18) . ?
C1 Co1 1.876(16) . ?
C2 N2 1.34(5) . ?
C2 C2 1.90(7) 82_656 ?
C2 C2 1.90(7) 78_566 ?
C2 C2 1.90(7) 53_554 ?
C2 C2 1.90(7) 33_554 ?
Co1 C1 1.876(16) 105 ?
Co1 C1 1.876(16) 9 ?
Co1 C1 1.876(16) 97 ?
Co1 C1 1.876(16) 5 ?
Co1 C1 1.876(16) 101 ?
K1 N1 2.790(11) . ?
K1 N1 2.790(11) 129 ?
K1 N1 2.790(11) 97_556 ?
K1 N1 2.790(11) 53_455 ?
K1 N1 2.790(11) 149 ?
K1 N1 2.790(11) 33_545 ?
N2 C2 1.34(5) 82_656 ?
N2 C2 1.34(5) 33_554 ?
N2 C2 1.34(5) 74_665 ?
N2 C2 1.34(5) 53_554 ?
N2 C2 1.34(5) 78_566 ?

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 C1 Co1 180.0 . . ?
N2 C2 C2 44.999(3) . 82_656 ?
N2 C2 C2 44.999(1) . 78_566 ?
C2 C2 C2 59.999(3) 82_656 78_566 ?
N2 C2 C2 44.999(1) . 53_554 ?
C2 C2 C2 59.999(5) 82_656 53_554 ?
C2 C2 C2 89.999(1) 78_566 53_554 ?
N2 C2 C2 44.999(3) . 33_554 ?
C2 C2 C2 89.999(3) 82_656 33_554 ?
C2 C2 C2 59.999(4) 78_566 33_554 ?
C2 C2 C2 59.999(5) 53_554 33_554 ?
C1 Co1 C1 180.0 105 9 ?
C1 Co1 C1 90.0 105 97 ?
C1 Co1 C1 90.0 9 97 ?
C1 Co1 C1 90.0 105 5 ?
C1 Co1 C1 90.0 9 5 ?
C1 Co1 C1 90.0 97 5 ?
C1 Co1 C1 90.0 105 101 ?
C1 Co1 C1 90.0 9 101 ?
C1 Co1 C1 90.0 97 101 ?
C1 Co1 C1 180.0 5 101 ?
C1 Co1 C1 90.0 105 . ?
C1 Co1 C1 90.0 9 . ?
C1 Co1 C1 180.0 97 . ?
C1 Co1 C1 90.0 5 . ?
C1 Co1 C1 90.0 101 . ?
N1 K1 N1 90.0 . 129 ?
N1 K1 N1 180.0 . 97_556 ?
N1 K1 N1 90.0 129 97_556 ?
N1 K1 N1 90.000(1) . 53_455 ?
N1 K1 N1 90.0 129 53_455 ?
N1 K1 N1 90.0 97_556 53_455 ?
N1 K1 N1 90.0 . 149 ?
N1 K1 N1 90.000(1) 129 149 ?
N1 K1 N1 90.000(1) 97_556 149 ?
N1 K1 N1 180.0 53_455 149 ?
N1 K1 N1 90.000(1) . 33_545 ?
N1 K1 N1 180.0 129 33_545 ?
N1 K1 N1 90.0 97_556 33_545 ?
N1 K1 N1 90.000(1) 53_455 33_545 ?
N1 K1 N1 90.0 149 33_545 ?
C1 N1 K1 180.0 . . ?
C2 N2 C2 180.0 82_656 33_554 ?
C2 N2 C2 90.000(12) 82_656 74_665 ?
C2 N2 C2 90.000(6) 33_554 74_665 ?
C2 N2 C2 90.000(8) 82_656 53_554 ?
C2 N2 C2 90.000(6) 33_554 53_554 ?
C2 N2 C2 90.000(3) 74_665 53_554 ?
C2 N2 C2 90.000(7) 82_656 78_566 ?
C2 N2 C2 90.000(6) 33_554 78_566 ?
C2 N2 C2 90.000(3) 74_665 78_566 ?
C2 N2 C2 180.0 53_554 78_566 ?
C2 N2 C2 90.000(8) 82_656 . ?
C2 N2 C2 90.000(10) 33_554 . ?
C2 N2 C2 180.0 74_665 . ?
C2 N2 C2 90.000(4) 53_554 . ?
C2 N2 C2 90.0 78_566 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C2 N2 C2 -90.000(7) 78_566 . . 82_656 ?
C2 C2 N2 C2 90.000(7) 53_554 . . 82_656 ?
C2 C2 N2 C2 180.0 33_554 . . 82_656 ?
C2 C2 N2 C2 180.0 82_656 . . 33_554 ?
C2 C2 N2 C2 90.000(6) 78_566 . . 33_554 ?
C2 C2 N2 C2 -90.000(10) 53_554 . . 33_554 ?
C2 C2 N2 C2 -90.000(7) 82_656 . . 53_554 ?
C2 C2 N2 C2 180.000(2) 78_566 . . 53_554 ?
C2 C2 N2 C2 90.000(7) 33_554 . . 53_554 ?
C2 C2 N2 C2 90.000(7) 82_656 . . 78_566 ?
C2 C2 N2 C2 180.000(14) 53_554 . . 78_566 ?
C2 C2 N2 C2 -90.000(7) 33_554 . . 78_566 ?

_refine_diff_density_max         0.709
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.134




# END OF CIF
