 
data_CPM-734c
# start Validation Reply Form
_vrf_THETM01_CPM-734c
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
Calculated sin(theta_max)/wavelength = 0.5243
RESPONSE: The crystal poorly diffracts at higher Bragg angles. Data
refinement is carried out after several failed data collections on 
different crystals.  
; 
_vrf_PLAT213_CPM-734c
;
PROBLEM: Atom N22/C23 has ADP max/min Ratio .....        6.0 prolat
RESPONSE:  Atoms belong to flexible amide functional group that is 
very disordered.  This however, does not indicate wrong atom assignment. 
;
_vrf_PLAT214_CPM-734c
;
PROBLEM: Atom C25 (Anion/Solvent) ADP max/min Ratio       14.0 prolat
RESPONSE:  Atoms belong to a flexible functional linker that is 
very disordered.  This however, does not indicate wrong atom assignment. 
;
# end Validation Reply Form  
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C60 H15 Co2.04 N6 O16 V0.96' 
_chemical_formula_weight          1244.90

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Co'  'Co'   0.3494   0.9721
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'V'  'V'   0.3005   0.5294
 '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'
 
_space_group_crystal_system       hexagonal
_space_group_IT_number            194
_space_group_name_H-M_alt         'P 63/m m c'
_space_group_name_Hall            '-P 6c 2c'
 
_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, x, z+1/2'
 '-y, x-y, z'
 '-x, -y, z+1/2'
 '-x+y, -x, z'
 'y, -x+y, z+1/2'
 '-y, -x, -z+1/2'
 'x-y, -y, -z'
 'x, x-y, -z+1/2'
 'y, x, -z'
 '-x+y, y, -z+1/2'
 '-x, -x+y, -z'
 '-x, -y, -z'
 '-x+y, -x, -z-1/2'
 'y, -x+y, -z'
 'x, y, -z-1/2'
 'x-y, x, -z'
 '-y, x-y, -z-1/2'
 'y, x, z-1/2'
 '-x+y, y, z'
 '-x, -x+y, z-1/2'
 '-y, -x, z'
 'x-y, -y, z-1/2'
 'x, x-y, z'
 
_cell_length_a                    20.918(10)
_cell_length_b                    20.918(10)
_cell_length_c                    16.080(9)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      6093(7)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     2161
_cell_measurement_theta_min       5.076
_cell_measurement_theta_max       35.159
 
_exptl_crystal_description        Hexagonal
_exptl_crystal_colour             purple-red
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     0.679          
_exptl_crystal_F_000              1244
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_absorpt_coefficient_mu     0.382
_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   'Bruker APEX-II CCD'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             28211
_diffrn_reflns_av_unetI/netI      0.0419
_diffrn_reflns_av_R_equivalents   0.1211
_diffrn_reflns_limit_h_min        -21
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        21
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          1.693
_diffrn_reflns_theta_max          21.880
_diffrn_reflns_theta_full         21.880
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              1410
_reflns_number_gt                 1008
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          1410
_refine_ls_number_parameters      90
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1159
_refine_ls_R_factor_gt            0.0839
_refine_ls_wR_factor_ref          0.2917
_refine_ls_wR_factor_gt           0.2516
_refine_ls_goodness_of_fit_ref    1.174
_refine_ls_restrained_S_all       1.174
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Co1 Co 0.27858(4) 0.55715(7) 0.2500 0.0492(8) Uani 0.68(5) 4 d S T P . .
V1 V 0.27858(4) 0.55715(7) 0.2500 0.0492(8) Uani 0.32(5) 4 d S T P . .
O1 O 0.3333 0.6667 0.2500 0.042(3) Uani 1 12 d S T P . .
O11 O 0.2078(3) 0.5509(3) 0.1614(4) 0.110(2) Uani 1 1 d . . . . .
N21 N 0.2181(2) 0.4363(5) 0.2500 0.113(5) Uani 1 4 d S T P . .
N22 N 0.1038(4) 0.2076(7) 0.2500 0.30(2) Uani 1 4 d S T P . .
C11 C 0.1832(5) 0.5916(3) 0.1407(7) 0.090(3) Uani 1 2 d S T P . .
C12 C 0.1129(7) 0.5564(3) 0.0864(9) 0.153(7) Uani 1 2 d S T P . .
C13 C 0.0858(6) 0.4827(8) 0.0616(8) 0.224(7) Uani 1 1 d . . . . .
C15 C 0.0000 0.4699(5) 0.0000 0.142(6) Uani 1 2 d S T P . .
C16 C -0.0260(11) 0.4014(9) -0.0133(16) 0.164(11) Uani 0.5 1 d . . P . .
C21 C 0.2509(7) 0.3974(6) 0.2500 0.183(9) Uani 1 2 d S T P . .
H21 H 0.3022 0.4227 0.2500 0.220 Uiso 1 2 calc R U P . .
C22 C 0.2150(7) 0.3216(6) 0.2500 0.233(13) Uani 1 2 d S T P . .
H22 H 0.2424 0.2977 0.2500 0.279 Uiso 1 2 calc R U P . .
C23 C 0.1406(4) 0.2811(7) 0.2500 0.216(18) Uani 1 4 d S T P . .
C25 C 0.0744(10) 0.0372(5) 0.2500 0.57(5) Uani 1 4 d S T P . .
H25 H 0.1257 0.0629 0.2500 0.688 Uiso 1 4 calc R U P . .
C26 C 0.0381(12) 0.076(2) 0.2500 0.30(2) Uiso 1 4 d S . P . .
O21 O -0.0063(15) 0.1724(13) 0.2081(14) 0.132(8) Uiso 0.25 1 d . . P . .
C24 C 0.0492(16) 0.1647(16) 0.2145(16) 0.093(9) Uiso 0.25 1 d . . 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 O1 1.9839(16) . ?
Co1 O11 2.012(5) 16_556 ?
Co1 O11 2.012(5) . ?
Co1 O11 2.012(5) 11 ?
Co1 O11 2.012(5) 20 ?
Co1 N21 2.190(9) . ?
O1 V1 1.9839(16) 14_566 ?
O1 Co1 1.9839(16) 14_566 ?
O1 V1 1.9839(16) 3_665 ?
O1 Co1 1.9839(16) 3_665 ?
O11 C11 1.240(6) . ?
N21 C21 1.299(12) 20 ?
N21 C21 1.299(12) . ?
N22 C24 1.19(3) . ?
N22 C24 1.19(3) 16_556 ?
N22 C24 1.19(3) 20 ?
N22 C24 1.19(3) 11 ?
N22 C23 1.332(19) . ?
C11 O11 1.240(6) 24_565 ?
C11 C12 1.544(13) . ?
C12 C13 1.409(13) 24_565 ?
C12 C13 1.409(13) . ?
C13 C16 1.433(17) 12 ?
C15 C15 1.26(2) 13_565 ?
C15 C16 1.271(16) 12 ?
C15 C16 1.271(16) . ?
C15 C13 1.947(12) 12 ?
C16 C16 1.04(3) 12 ?
C16 C13 1.433(17) 12 ?
C21 C22 1.375(16) . ?
C21 H21 0.9300 . ?
C22 C23 1.349(14) . ?
C22 H22 0.9300 . ?
C23 C22 1.349(14) 20 ?
C25 C26 1.36(2) 14_556 ?
C25 C26 1.36(2) . ?
C25 H25 0.9300 . ?
C26 C25 1.36(2) 3 ?
C26 C24 1.84(4) . ?
C26 C24 1.84(4) 11 ?
C26 C24 1.84(4) 16_556 ?
C26 C24 1.84(4) 20 ?
O21 C24 1.25(3) . ?
O21 O21 1.35(5) 16_556 ?
O21 C24 1.76(3) 16_556 ?
C24 C24 1.14(5) 16_556 ?
C24 C24 1.39(6) 20 ?
C24 O21 1.76(3) 16_556 ?
C24 C24 1.80(6) 11 ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 Co1 O11 93.22(15) . 16_556 ?
O1 Co1 O11 93.22(15) . . ?
O11 Co1 O11 90.2(3) 16_556 . ?
O1 Co1 O11 93.22(15) . 11 ?
O11 Co1 O11 89.5(3) 16_556 11 ?
O11 Co1 O11 173.6(3) . 11 ?
O1 Co1 O11 93.22(15) . 20 ?
O11 Co1 O11 173.6(3) 16_556 20 ?
O11 Co1 O11 89.5(3) . 20 ?
O11 Co1 O11 90.2(3) 11 20 ?
O1 Co1 N21 180.00(8) . . ?
O11 Co1 N21 86.78(15) 16_556 . ?
O11 Co1 N21 86.78(15) . . ?
O11 Co1 N21 86.78(15) 11 . ?
O11 Co1 N21 86.78(15) 20 . ?
V1 O1 Co1 0.0 14_566 14_566 ?
V1 O1 V1 120.0 14_566 3_665 ?
Co1 O1 V1 120.0 14_566 3_665 ?
V1 O1 Co1 120.0 14_566 3_665 ?
Co1 O1 Co1 120.0 14_566 3_665 ?
V1 O1 Co1 0.0 3_665 3_665 ?
V1 O1 Co1 120.0 14_566 . ?
Co1 O1 Co1 120.0 14_566 . ?
V1 O1 Co1 120.0 3_665 . ?
Co1 O1 Co1 120.0 3_665 . ?
C11 O11 Co1 133.7(5) . . ?
C21 N21 C21 114.4(12) 20 . ?
C21 N21 Co1 122.8(6) 20 . ?
C21 N21 Co1 122.8(6) . . ?
C24 N22 C24 57(2) . 16_556 ?
C24 N22 C24 72(3) . 20 ?
C24 N22 C24 98(3) 16_556 20 ?
C24 N22 C24 98(3) . 11 ?
C24 N22 C24 72(3) 16_556 11 ?
C24 N22 C24 57(2) 20 11 ?
C24 N22 C23 130.8(14) . . ?
C24 N22 C23 130.8(14) 16_556 . ?
C24 N22 C23 130.8(14) 20 . ?
C24 N22 C23 130.8(14) 11 . ?
O11 C11 O11 126.6(7) . 24_565 ?
O11 C11 C12 116.7(4) . . ?
O11 C11 C12 116.7(4) 24_565 . ?
C13 C12 C13 126.6(13) 24_565 . ?
C13 C12 C11 116.6(6) 24_565 . ?
C13 C12 C11 116.6(6) . . ?
C12 C13 C16 138.3(14) . 12 ?
C15 C15 C16 156.0(7) 13_565 12 ?
C15 C15 C16 156.0(7) 13_565 . ?
C16 C15 C16 48.1(13) 12 . ?
C15 C15 C13 108.9(5) 13_565 12 ?
C16 C15 C13 94.9(9) 12 12 ?
C16 C15 C13 47.4(8) . 12 ?
C16 C16 C15 65.9(7) 12 . ?
C16 C16 C13 156(2) 12 12 ?
C15 C16 C13 91.9(12) . 12 ?
N21 C21 C22 124.5(11) . . ?
N21 C21 H21 117.7 . . ?
C22 C21 H21 117.7 . . ?
C23 C22 C21 121.1(11) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
N22 C23 C22 122.9(7) . . ?
N22 C23 C22 122.9(7) . 20 ?
C22 C23 C22 114.2(13) . 20 ?
C26 C25 C26 122(4) 14_556 . ?
C26 C25 H25 118.8 14_556 . ?
C26 C25 H25 118.8 . . ?
C25 C26 C25 118(4) . 3 ?
C25 C26 C24 141(2) . . ?
C25 C26 C24 97.4(15) 3 . ?
C25 C26 C24 97.4(15) . 11 ?
C25 C26 C24 141(2) 3 11 ?
C24 C26 C24 59(2) . 11 ?
C25 C26 C24 141(2) . 16_556 ?
C25 C26 C24 97.4(15) 3 16_556 ?
C24 C26 C24 36.2(18) . 16_556 ?
C24 C26 C24 44(2) 11 16_556 ?
C25 C26 C24 97.4(15) . 20 ?
C25 C26 C24 141(2) 3 20 ?
C24 C26 C24 44(2) . 20 ?
C24 C26 C24 36.2(18) 11 20 ?
C24 C26 C24 59(2) 16_556 20 ?
C24 O21 O21 85.3(16) . 16_556 ?
C24 O21 C24 40(2) . 16_556 ?
O21 O21 C24 45.1(10) 16_556 16_556 ?
C24 C24 N22 61.3(12) 16_556 . ?
C24 C24 O21 94.7(16) 16_556 . ?
N22 C24 O21 123(3) . . ?
C24 C24 C24 90.002(7) 16_556 20 ?
N22 C24 C24 54.2(14) . 20 ?
O21 C24 C24 172.1(17) . 20 ?
C24 C24 O21 45.1(10) 16_556 16_556 ?
N22 C24 O21 91.2(17) . 16_556 ?
O21 C24 O21 49.6(19) . 16_556 ?
C24 C24 O21 134.7(11) 20 16_556 ?
C24 C24 C24 50.6(17) 16_556 11 ?
N22 C24 C24 40.8(14) . 11 ?
O21 C24 C24 145(3) . 11 ?
C24 C24 C24 39.4(17) 20 11 ?
O21 C24 C24 95(2) 16_556 11 ?
C24 C24 C26 71.9(9) 16_556 . ?
N22 C24 C26 102(2) . . ?
O21 C24 C26 120(2) . . ?
C24 C24 C26 67.8(11) 20 . ?
O21 C24 C26 96.6(15) 16_556 . ?
C24 C24 C26 60.7(12) 11 . ?
 
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
Co1 O11 C11 O11 15(2) . . . 24_565 ?
Co1 O11 C11 C12 -162.5(8) . . . . ?
O11 C11 C12 C13 -178.8(12) . . . 24_565 ?
O11 C11 C12 C13 3.6(19) 24_565 . . 24_565 ?
O11 C11 C12 C13 -3.6(19) . . . . ?
O11 C11 C12 C13 178.8(12) 24_565 . . . ?
C13 C12 C13 C16 -5(4) 24_565 . . 12 ?
C11 C12 C13 C16 -180(2) . . . 12 ?
C15 C15 C16 C16 180.003(6) 13_565 . . 12 ?
C13 C15 C16 C16 170(4) 12 . . 12 ?
C15 C15 C16 C13 10(4) 13_565 . . 12 ?
C16 C15 C16 C13 -170(4) 12 . . 12 ?
C21 N21 C21 C22 0.0 20 . . . ?
Co1 N21 C21 C22 180.0 . . . . ?
N21 C21 C22 C23 0.0 . . . . ?
C24 N22 C23 C22 -140.6(17) . . . . ?
C24 N22 C23 C22 140.6(17) 16_556 . . . ?
C24 N22 C23 C22 -39.4(17) 20 . . . ?
C24 N22 C23 C22 39.4(17) 11 . . . ?
C24 N22 C23 C22 39.4(17) . . . 20 ?
C24 N22 C23 C22 -39.4(17) 16_556 . . 20 ?
C24 N22 C23 C22 140.6(17) 20 . . 20 ?
C24 N22 C23 C22 -140.6(17) 11 . . 20 ?
C21 C22 C23 N22 180.0 . . . . ?
C21 C22 C23 C22 0.0 . . . 20 ?
C26 C25 C26 C25 0.0 14_556 . . 3 ?
C26 C25 C26 C24 -151(2) 14_556 . . . ?
C26 C25 C26 C24 161.8(9) 14_556 . . 11 ?
C26 C25 C26 C24 151(2) 14_556 . . 16_556 ?
C26 C25 C26 C24 -161.8(9) 14_556 . . 20 ?
C24 N22 C24 C24 113.3(15) 20 . . 16_556 ?
C24 N22 C24 C24 61.8(17) 11 . . 16_556 ?
C23 N22 C24 C24 -118.2(17) . . . 16_556 ?
C24 N22 C24 O21 76(3) 16_556 . . . ?
C24 N22 C24 O21 -171(2) 20 . . . ?
C24 N22 C24 O21 138(3) 11 . . . ?
C23 N22 C24 O21 -42(3) . . . . ?
C24 N22 C24 C24 -113.3(15) 16_556 . . 20 ?
C24 N22 C24 C24 -51.5(17) 11 . . 20 ?
C23 N22 C24 C24 128.5(17) . . . 20 ?
C24 N22 C24 O21 35.3(17) 16_556 . . 16_556 ?
C24 N22 C24 O21 148.5(9) 20 . . 16_556 ?
C24 N22 C24 O21 97.0(16) 11 . . 16_556 ?
C23 N22 C24 O21 -83.0(16) . . . 16_556 ?
C24 N22 C24 C24 -61.8(17) 16_556 . . 11 ?
C24 N22 C24 C24 51.5(17) 20 . . 11 ?
C23 N22 C24 C24 180.001(6) . . . 11 ?
C24 N22 C24 C26 -61.8(17) 16_556 . . . ?
C24 N22 C24 C26 51.5(17) 20 . . . ?
C24 N22 C24 C26 -0.001(4) 11 . . . ?
C23 N22 C24 C26 180.000(1) . . . . ?
O21 O21 C24 C24 0.000(5) 16_556 . . 16_556 ?
O21 O21 C24 N22 -59(2) 16_556 . . . ?
C24 O21 C24 N22 -59(2) 16_556 . . . ?
C24 O21 C24 O21 0.000(13) 16_556 . . 16_556 ?
O21 O21 C24 C24 -9(3) 16_556 . . 11 ?
C24 O21 C24 C24 -9(3) 16_556 . . 11 ?
O21 O21 C24 C26 71.8(18) 16_556 . . . ?
C24 O21 C24 C26 71.8(18) 16_556 . . . ?
C25 C26 C24 C24 -114(3) . . . 16_556 ?
C25 C26 C24 C24 92.4(6) 3 . . 16_556 ?
C24 C26 C24 C24 -54.4(17) 11 . . 16_556 ?
C24 C26 C24 C24 -97.7(6) 20 . . 16_556 ?
C25 C26 C24 N22 -59(3) . . . . ?
C25 C26 C24 N22 146.8(16) 3 . . . ?
C24 C26 C24 N22 0.001(4) 11 . . . ?
C24 C26 C24 N22 54.4(17) 16_556 . . . ?
C24 C26 C24 N22 -43.3(17) 20 . . . ?
C25 C26 C24 O21 161(3) . . . . ?
C25 C26 C24 O21 7(3) 3 . . . ?
C24 C26 C24 O21 -139(3) 11 . . . ?
C24 C26 C24 O21 -85(2) 16_556 . . . ?
C24 C26 C24 O21 177(2) 20 . . . ?
C25 C26 C24 C24 -16(2) . . . 20 ?
C25 C26 C24 C24 -169.9(9) 3 . . 20 ?
C24 C26 C24 C24 43.3(17) 11 . . 20 ?
C24 C26 C24 C24 97.7(6) 16_556 . . 20 ?
C25 C26 C24 O21 -152(2) . . . 16_556 ?
C25 C26 C24 O21 54.2(15) 3 . . 16_556 ?
C24 C26 C24 O21 -92.6(19) 11 . . 16_556 ?
C24 C26 C24 O21 -38.2(15) 16_556 . . 16_556 ?
C24 C26 C24 O21 -135.9(11) 20 . . 16_556 ?
C25 C26 C24 C24 -59(3) . . . 11 ?
C25 C26 C24 C24 146.8(16) 3 . . 11 ?
C24 C26 C24 C24 54.4(17) 16_556 . . 11 ?
C24 C26 C24 C24 -43.3(17) 20 . . 11 ?
 
_refine_diff_density_max    0.681
_refine_diff_density_min   -0.534
_refine_diff_density_rms    0.080



_platon_squeeze_details
;
The 793 electrons scattering per cell found by SQUEEZE/PLATON belongs to 
DMF and H2O molecules in the channel.
TITL CPM-734c.res in P-31c      New: P63/mmc
CELL   20.9180   20.9180   16.0800     90.00     90.00    120.00
SPGR P63/mmc
# Solvent Accessible Volume =      3900
# Electrons Found in S.A.V. =       793
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.683 0.318 0.004 !       1.30 eA-3
C102 0.634 0.313 0.437 !       0.90 eA-3
C103 0.645 0.362 0.449 !       0.86 eA-3
C104 0.637 0.268 0.483 !       0.85 eA-3
C105 0.513 0.094 0.250 !       0.83 eA-3
C106 0.715 0.418 0.028 !       0.80 eA-3
C107 0.520 0.265 0.448 !       0.77 eA-3
C108 0.507 0.142 0.281 !       0.72 eA-3
C109 0.752 0.373 0.157 !       0.72 eA-3
C110 0.846 0.156 0.404 !       0.68 eA-3
C111 0.543 0.016 0.260 !       0.68 eA-3
C112 0.687 0.125 0.252 !       0.67 eA-3
C113 0.991 0.020 0.446 !       0.66 eA-3
C114 0.625 0.438 0.248 !       0.66 eA-3
C115 0.292 0.123 0.046 !       0.65 eA-3
C116 0.535 0.469 0.246 !       0.65 eA-3
C117 0.619 0.236 0.097 !       0.64 eA-3
C118 0.778 0.555 0.452 !       0.64 eA-3
C119 0.706 0.345 0.144 !       0.64 eA-3
C120 0.032 0.061 0.029 !       0.64 eA-3
C121 0.705 0.344 0.207 !       0.64 eA-3
C122 0.620 0.375 0.286 !       0.64 eA-3
C123 0.613 0.391 0.244 !       0.62 eA-3
C124 0.268 0.583 0.893 !       0.62 eA-3
C125 0.938 0.344 0.235 !       0.61 eA-3
C126 0.593 0.189 0.201 !       0.60 eA-3
C127 0.472 0.231 0.467 !       0.60 eA-3
C128 0.689 0.372 0.161 !       0.60 eA-3
C129 0.098 0.641 0.742 !       0.60 eA-3
C130 0.596 0.130 0.205 !       0.60 eA-3
C131 0.406 0.237 0.014 !       0.59 eA-3
C132 0.233 0.715 0.004 !       0.59 eA-3
C133 0.439 0.747 0.928 !       0.58 eA-3
C134 0.447 0.562 0.740 !       0.57 eA-3
C135 0.774 0.503 0.076 !       0.56 eA-3
Q136 0.198 0.386 0.367 !       0.56 eA-3
C137 0.871 0.106 0.506 !       0.56 eA-3
C138 0.410 0.306 0.295 !       0.55 eA-3
C139 0.257 0.514 0.628 !       0.55 eA-3
C140 0.198 0.345 0.467 !       0.55 eA-3
C141 0.202 0.798 0.470 !       0.54 eA-3
C142 0.886 0.532 0.211 !       0.54 eA-3
C143 0.701 0.839 0.019 !       0.54 eA-3
Q144 0.668 0.842 0.353 !       0.53 eA-3
C145 0.606 0.047 0.250 !       0.53 eA-3
C146 0.875 0.940 0.032 !       0.53 eA-3
C147 0.578 0.267 0.326 !       0.53 eA-3
Q148 0.785 0.391 0.032 !       0.52 eA-3
C149 0.730 0.825 0.062 !       0.52 eA-3
C150 0.217 0.663 0.799 !       0.52 eA-3
Q151 0.832 0.828 0.106 !       0.52 eA-3
C152 0.953 0.042 0.062 !       0.51 eA-3
C153 0.830 0.182 0.451 !       0.51 eA-3
C154 0.567 0.349 0.121 !       0.50 eA-3
Q155 0.800 0.767 0.096 !       0.50 eA-3
)
;



 
data_CPM-734t
# start Validation Reply Form
_vrf_THETM01_CPM-734t
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
Calculated sin(theta_max)/wavelength = 0.5272
RESPONSE: The crystal poorly diffracts at higher Bragg angles. Data
refinement is carried out after several failed data collections on 
different crystals.  
; 
_vrf_PLAT602_CPM-734t
;
PROBLEM: Solvent Accessible VOID(S) in Structure ........! Check
RESPONSE:  Toplogy of crystal structure results in very large accessible
voids.  The largest peak in the final difference map is just 0.92 e/A3,
and no model of solvent could be found.
;
# end Validation Reply Form 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C54 H30 Co1.98 N6 O13 V1.02' 
_chemical_formula_weight          1139.48

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Co'  'Co'   0.3494   0.9721
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'V'  'V'   0.3005   0.5294
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       hexagonal
_space_group_IT_number            194
_space_group_name_H-M_alt         'P 63/m m c'
_space_group_name_Hall            '-P 6c 2c'
 
_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'
 '-y, x-y, z'
 '-x+y, -x, z'
 '-x, -y, z+1/2'
 'y, -x+y, z+1/2'
 'x-y, x, z+1/2'
 'y, x, -z'
 'x-y, -y, -z'
 '-x, -x+y, -z'
 '-y, -x, -z+1/2'
 '-x+y, y, -z+1/2'
 'x, x-y, -z+1/2'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 'x, y, -z-1/2'
 '-y, x-y, -z-1/2'
 '-x+y, -x, -z-1/2'
 '-y, -x, z'
 '-x+y, y, z'
 'x, x-y, z'
 'y, x, z-1/2'
 'x-y, -y, z-1/2'
 '-x, -x+y, z-1/2'
 
_cell_length_a                    16.799(5)
_cell_length_b                    16.799(5)
_cell_length_c                    20.706(7)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      5060(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used     1427
_cell_measurement_theta_min       4.818
_cell_measurement_theta_max       34.706
 
_exptl_crystal_description        Hexagonal
_exptl_crystal_colour             deep-red
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     0.748          
_exptl_crystal_F_000              1154
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_absorpt_coefficient_mu     0.449
_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       296(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             21932
_diffrn_reflns_av_unetI/netI      0.0367
_diffrn_reflns_av_R_equivalents   0.1146
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          1.400
_diffrn_reflns_theta_max          22.007
_diffrn_reflns_theta_full         22.007
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              1212
_reflns_number_gt                 931
_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)+(0.1072P)²+27.8844P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          1212
_refine_ls_number_parameters      61
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1133
_refine_ls_R_factor_gt            0.0905
_refine_ls_wR_factor_ref          0.2513
_refine_ls_wR_factor_gt           0.2327
_refine_ls_goodness_of_fit_ref    1.096
_refine_ls_restrained_S_all       1.096
_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
Co01 Co 0.73397(6) 0.46793(12) 0.2500 0.0342(8) Uani 0.66(6) 4 d S T P . .
V01 V 0.73397(6) 0.46793(12) 0.2500 0.0342(8) Uani 0.34(6) 4 d S T P . .
O1 O 0.6667 0.3333 0.2500 0.034(4) Uani 1 12 d S T P . .
O11 O 0.8223(3) 0.4771(3) 0.3193(3) 0.0629(18) Uani 1 1 d . . . . .
N21 N 0.8092(4) 0.6185(7) 0.2500 0.074(5) Uani 1 4 d S T P . .
N22 N 1.0469(4) 0.9531(4) 0.2500 0.118(8) Uani 1 4 d S T P . .
C11 C 0.8442(7) 0.4221(3) 0.3413(5) 0.049(3) Uiso 1 2 d S . P . .
C12 C 0.9051(11) 0.4525(5) 0.4012(7) 0.098(5) Uiso 1 2 d S . P . .
C13 C 0.9305(10) 0.5337(10) 0.4269(7) 0.156(6) Uiso 1 1 d . . . . .
H13 H 0.8957 0.5557 0.4070 0.188 Uiso 1 1 calc R U . . .
C14 C 1.0000 0.5382(8) 0.5000 0.100(5) Uiso 1 2 d S . P . .
C15 C 1.0120(15) 0.6130(14) 0.5282(8) 0.094(6) Uiso 0.5 1 d . . P . .
H15 H 0.9915 0.6545 0.5216 0.113 Uiso 0.5 1 calc R U P . .
C21 C 0.7662(7) 0.6656(7) 0.2500 0.102(6) Uani 1 2 d S T P . .
H21 H 0.7023 0.6334 0.2500 0.123 Uiso 1 2 calc R U P . .
C22 C 0.8107(7) 0.7596(7) 0.2500 0.115(7) Uani 1 2 d S T P . .
H22 H 0.7769 0.7897 0.2500 0.138 Uiso 1 2 calc R U P . .
C23 C 0.9047(5) 0.8094(10) 0.2500 0.099(8) Uani 1 4 d S T P . .
C24 C 0.9551(5) 0.9102(10) 0.2500 0.101(9) Uani 1 4 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
Co01 O1 1.9582(18) . ?
Co01 O11 2.013(5) 11_655 ?
Co01 O11 2.013(5) 20_655 ?
Co01 O11 2.013(5) 16_556 ?
Co01 O11 2.013(5) . ?
Co01 N21 2.190(11) . ?
O1 V01 1.9582(18) 3_665 ?
O1 Co01 1.9582(18) 3_665 ?
O1 V01 1.9582(18) 2_655 ?
O1 Co01 1.9582(18) 2_655 ?
O11 C11 1.241(6) . ?
N21 C21 1.311(12) 20_655 ?
N21 C21 1.311(12) . ?
N22 C24 1.336(9) 2_765 ?
N22 C24 1.336(9) . ?
C11 O11 1.241(6) 21 ?
C11 C12 1.523(18) . ?
C12 C13 1.321(15) . ?
C12 C13 1.321(15) 21 ?
C13 C15 1.41(2) 9_766 ?
C13 H13 0.9300 . ?
C14 C14 1.28(3) 13_766 ?
C14 C15 1.306(19) . ?
C14 C15 1.306(19) 9_766 ?
C14 C13 1.889(16) 9_766 ?
C15 C13 1.41(2) 9_766 ?
C15 H15 0.9300 . ?
C21 C22 1.368(15) . ?
C21 H21 0.9300 . ?
C22 C23 1.369(13) . ?
C22 H22 0.9300 . ?
C23 C22 1.369(13) 20_655 ?
C23 C24 1.47(2) . ?
C24 N22 1.336(9) 3_675 ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 Co01 O11 93.82(14) . 11_655 ?
O1 Co01 O11 93.82(14) . 20_655 ?
O11 Co01 O11 90.9(3) 11_655 20_655 ?
O1 Co01 O11 93.82(14) . 16_556 ?
O11 Co01 O11 88.6(3) 11_655 16_556 ?
O11 Co01 O11 172.4(3) 20_655 16_556 ?
O1 Co01 O11 93.82(14) . . ?
O11 Co01 O11 172.4(3) 11_655 . ?
O11 Co01 O11 88.6(3) 20_655 . ?
O11 Co01 O11 90.9(3) 16_556 . ?
O1 Co01 N21 180.0 . . ?
O11 Co01 N21 86.18(14) 11_655 . ?
O11 Co01 N21 86.18(14) 20_655 . ?
O11 Co01 N21 86.18(14) 16_556 . ?
O11 Co01 N21 86.18(14) . . ?
V01 O1 Co01 0.0 3_665 3_665 ?
V01 O1 V01 120.000(1) 3_665 2_655 ?
Co01 O1 V01 120.000(1) 3_665 2_655 ?
V01 O1 Co01 120.0 3_665 2_655 ?
Co01 O1 Co01 120.000(1) 3_665 2_655 ?
V01 O1 Co01 0.0 2_655 2_655 ?
V01 O1 Co01 120.0 3_665 . ?
Co01 O1 Co01 120.0 3_665 . ?
V01 O1 Co01 120.0 2_655 . ?
Co01 O1 Co01 120.0 2_655 . ?
C11 O11 Co01 133.4(5) . . ?
C21 N21 C21 117.0(12) 20_655 . ?
C21 N21 Co01 121.5(6) 20_655 . ?
C21 N21 Co01 121.5(6) . . ?
C24 N22 C24 115.7(15) 2_765 . ?
O11 C11 O11 126.6(9) . 21 ?
O11 C11 C12 116.7(5) . . ?
O11 C11 C12 116.7(5) 21 . ?
C13 C12 C13 121.1(19) . 21 ?
C13 C12 C11 119.4(10) . . ?
C13 C12 C11 119.4(10) 21 . ?
C12 C13 C15 146.4(18) . 9_766 ?
C12 C13 H13 106.8 . . ?
C15 C13 H13 106.8 9_766 . ?
C14 C14 C15 152.2(8) 13_766 . ?
C14 C14 C15 152.2(8) 13_766 9_766 ?
C15 C14 C15 55.6(16) . 9_766 ?
C14 C14 C13 105.6(6) 13_766 9_766 ?
C15 C14 C13 48.1(9) . 9_766 ?
C15 C14 C13 101.0(12) 9_766 9_766 ?
C14 C15 C13 88.1(13) . 9_766 ?
C14 C15 H15 135.9 . . ?
C13 C15 H15 135.9 9_766 . ?
N21 C21 C22 123.3(10) . . ?
N21 C21 H21 118.4 . . ?
C22 C21 H21 118.4 . . ?
C21 C22 C23 120.2(10) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C22 C23 C22 116.0(13) . 20_655 ?
C22 C23 C24 122.0(7) . . ?
C22 C23 C24 122.0(7) 20_655 . ?
N22 C24 N22 124.3(15) 3_675 . ?
N22 C24 C23 117.9(8) 3_675 . ?
N22 C24 C23 117.9(8) . . ?
 
_refine_diff_density_max    0.894
_refine_diff_density_min   -0.918
_refine_diff_density_rms    0.092





