# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_Comp1
_database_code_depnum_ccdc_archive 'CCDC 1496000'
_audit_update_record             
;
2016-08-31 deposited with the CCDC.
2016-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Co Cr O14, C6 H13 N2, 2(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C14 H25 Co Cr N2 O18'
_chemical_formula_weight         620.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 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'

_cell_length_a                   14.6233(16)
_cell_length_b                   11.5742(13)
_cell_length_c                   14.9934(17)
_cell_angle_alpha                90
_cell_angle_beta                 97.2780(10)
_cell_angle_gamma                90
_cell_volume                     2517.2(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6219
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.47

_exptl_crystal_description       plates
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.174
_shelx_estimated_absorpt_T_min   0.720
_shelx_estimated_absorpt_T_max   0.892
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6218
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6935
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.251
_diffrn_reflns_theta_max         27.467
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3794
_reflns_number_gt                3779
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_max     0.987
_reflns_Friedel_fraction_full    0.998

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0460P)²+1.3814P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.433(16)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3794
_refine_ls_number_parameters     345
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0714
_refine_ls_wR_factor_gt          0.0714
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.113
_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
Cr1 Cr 0.48743(3) 0.73824(4) 0.22970(3) 0.01031(11) Uani 1 1 d . . . . .
Co1 Co 0.14844(2) 0.64420(3) 0.31451(3) 0.01137(10) Uani 1 1 d . . . . .
O1 O 0.36575(14) 0.68737(19) 0.16890(15) 0.0143(4) Uani 1 1 d . . . . .
O2 O 0.42463(15) 0.72166(19) 0.33938(16) 0.0129(4) Uani 1 1 d . . . . .
O3 O 0.22371(16) 0.64787(18) 0.20042(17) 0.0156(5) Uani 1 1 d . . . . .
O4 O 0.28206(15) 0.69576(19) 0.37568(16) 0.0155(4) Uani 1 1 d . . . . .
O5 O 0.45324(14) 0.90384(18) 0.22250(16) 0.0136(4) Uani 1 1 d . . . . .
O6 O 0.60314(14) 0.79756(18) 0.29579(16) 0.0146(4) Uani 1 1 d . . . . .
O7 O 0.52071(15) 1.07666(18) 0.25239(16) 0.0160(4) Uani 1 1 d . . . . .
O8 O 0.67631(14) 0.96583(19) 0.32252(17) 0.0159(4) Uani 1 1 d . . . . .
O9 O 0.53914(17) 0.74652(18) 0.11668(17) 0.0149(5) Uani 1 1 d . . . . .
O10 O 0.53835(15) 0.58084(18) 0.23313(15) 0.0139(4) Uani 1 1 d . . . . .
O11 O 0.62093(17) 0.64399(18) 0.02922(18) 0.0209(5) Uani 1 1 d . . . . .
O12 O 0.62697(17) 0.46830(19) 0.15771(16) 0.0204(5) Uani 1 1 d . . . . .
O13 O 0.10127(18) 0.64276(17) 0.43728(18) 0.0170(5) Uani 1 1 d . . . . .
O14 O 0.10064(15) 0.80607(18) 0.28833(16) 0.0165(4) Uani 1 1 d . . . . .
O15 O 0.1159(2) 0.5442(3) 0.0425(2) 0.0441(9) Uani 1 1 d D . . . .
H15A H 0.077(3) 0.599(4) 0.045(5) 0.066 Uiso 1 1 d D U . . .
H15B H 0.151(4) 0.559(5) 0.090(3) 0.066 Uiso 1 1 d D U . . .
O16 O 0.4800(3) 0.2012(3) 0.0233(2) 0.0466(9) Uani 1 1 d D . . . .
H16A H 0.456(4) 0.228(6) -0.024(2) 0.070 Uiso 1 1 d D U . . .
H16B H 0.454(5) 0.229(6) 0.065(3) 0.070 Uiso 1 1 d D U . . .
O17 O 0.42975(16) 0.3182(2) 0.32671(18) 0.0232(5) Uani 1 1 d . . . . .
H17 H 0.4863 0.3061 0.3259 0.035 Uiso 1 1 calc R U . . .
O18 O 0.3631(3) 0.2699(3) 0.1429(3) 0.0509(9) Uani 1 1 d . . . . .
H18 H 0.3778 0.2704 0.1989 0.076 Uiso 1 1 calc R U . . .
N1 N 0.22493(18) 0.0438(2) 0.49100(19) 0.0175(5) Uani 1 1 d . . . . .
H1 H 0.190(4) 0.005(5) 0.514(4) 0.038(13) Uiso 1 1 d . . . . .
N2 N 0.33935(18) 0.1599(2) 0.4156(2) 0.0169(5) Uani 1 1 d . . . . .
C1 C 0.3054(2) 0.6756(2) 0.2215(2) 0.0122(5) Uani 1 1 d . . . . .
C2 C 0.33848(19) 0.6995(2) 0.3218(2) 0.0113(5) Uani 1 1 d . . . . .
C3 C 0.52003(19) 0.9701(3) 0.2523(2) 0.0124(5) Uani 1 1 d . . . . .
C4 C 0.60829(19) 0.9068(3) 0.2941(2) 0.0127(5) Uani 1 1 d . . . . .
C5 C 0.5824(2) 0.6559(2) 0.0968(2) 0.0142(6) Uani 1 1 d . . . . .
C6 C 0.5842(2) 0.5574(2) 0.1679(2) 0.0132(5) Uani 1 1 d . . . . .
C7 C 0.1986(3) 0.1696(3) 0.4933(3) 0.0327(9) Uani 1 1 d . . . . .
H7 H 0.1894 0.1930 0.5550 0.039 Uiso 1 1 calc R U . . .
H7A H 0.1408 0.1841 0.4528 0.039 Uiso 1 1 calc R U . . .
C8 C 0.2795(3) 0.2378(3) 0.4614(3) 0.0223(7) Uani 1 1 d . . . . .
H8 H 0.2548 0.2996 0.4195 0.027 Uiso 1 1 calc R U . . .
H8A H 0.3163 0.2745 0.5137 0.027 Uiso 1 1 calc R U . . .
C9 C 0.3180(2) 0.0243(4) 0.5387(3) 0.0352(9) Uani 1 1 d . . . . .
H9 H 0.3303 -0.0596 0.5457 0.042 Uiso 1 1 calc R U . . .
H9A H 0.3236 0.0597 0.5993 0.042 Uiso 1 1 calc R U . . .
C10 C 0.3877(2) 0.0803(3) 0.4823(3) 0.0270(8) Uani 1 1 d . . . . .
H10 H 0.4350 0.1232 0.5223 0.032 Uiso 1 1 calc R U . . .
H10A H 0.4191 0.0195 0.4512 0.032 Uiso 1 1 calc R U . . .
C11 C 0.2197(3) 0.0091(4) 0.3945(3) 0.0337(9) Uani 1 1 d . . . . .
H11 H 0.1551 0.0130 0.3654 0.040 Uiso 1 1 calc R U . . .
H11A H 0.2420 -0.0712 0.3898 0.040 Uiso 1 1 calc R U . . .
C12 C 0.2804(2) 0.0926(3) 0.3479(2) 0.0198(6) Uani 1 1 d . . . . .
H12 H 0.3193 0.0482 0.3106 0.024 Uiso 1 1 calc R U . . .
H12A H 0.2408 0.1454 0.3079 0.024 Uiso 1 1 calc R U . . .
C13 C 0.4174(2) 0.4246(3) 0.3725(3) 0.0298(8) Uani 1 1 d . . . . .
H13 H 0.4532 0.4857 0.3477 0.045 Uiso 1 1 calc R U . . .
H13A H 0.4387 0.4154 0.4367 0.045 Uiso 1 1 calc R U . . .
H13B H 0.3520 0.4456 0.3643 0.045 Uiso 1 1 calc R U . . .
C14 C 0.3059(4) 0.3658(5) 0.1174(4) 0.0523(14) Uani 1 1 d . . . . .
H14 H 0.2500 0.3612 0.1469 0.078 Uiso 1 1 calc R U . . .
H14A H 0.2890 0.3655 0.0520 0.078 Uiso 1 1 calc R U . . .
H14B H 0.3391 0.4373 0.1354 0.078 Uiso 1 1 calc R U . . .


_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
Cr1 O9 1.943(3) . ?
Cr1 O10 1.966(2) . ?
Cr1 O6 1.973(2) . ?
Cr1 O5 1.980(2) . ?
Cr1 O1 1.983(2) . ?
Cr1 O2 1.992(2) . ?
Co1 O14 2.021(2) . ?
Co1 O13 2.046(3) . ?
Co1 O8 2.105(2) 3_445 ?
Co1 O7 2.128(2) 3_445 ?
Co1 O4 2.136(2) . ?
Co1 O3 2.149(3) . ?
O1 C1 1.263(4) . ?
O2 C2 1.280(4) . ?
O3 C1 1.239(4) . ?
O4 C2 1.226(4) . ?
O5 C3 1.277(4) . ?
O6 C4 1.267(4) . ?
O7 C3 1.234(4) . ?
O7 Co1 2.128(2) 3 ?
O8 C4 1.237(4) . ?
O8 Co1 2.105(2) 3 ?
O9 C5 1.280(4) . ?
O10 C6 1.282(4) . ?
O11 C5 1.228(4) . ?
O12 C6 1.226(4) . ?
O15 H15A 0.86(2) . ?
O15 H15B 0.84(2) . ?
O16 H16A 0.81(2) . ?
O16 H16B 0.84(2) . ?
O17 C13 1.432(5) . ?
O17 H17 0.8400 . ?
O18 C14 1.413(6) . ?
O18 H18 0.8400 . ?
N1 C9 1.473(5) . ?
N1 C11 1.494(5) . ?
N1 C7 1.508(5) . ?
N1 H1 0.79(6) . ?
N2 C12 1.470(4) . ?
N2 C10 1.473(4) . ?
N2 C8 1.484(4) . ?
C1 C2 1.545(4) . ?
C3 C4 1.546(4) . ?
C5 C6 1.558(4) . ?
C7 C8 1.547(5) . ?
C7 H7 0.9900 . ?
C7 H7A 0.9900 . ?
C8 H8 0.9900 . ?
C8 H8A 0.9900 . ?
C9 C10 1.547(5) . ?
C9 H9 0.9900 . ?
C9 H9A 0.9900 . ?
C10 H10 0.9900 . ?
C10 H10A 0.9900 . ?
C11 C12 1.539(5) . ?
C11 H11 0.9900 . ?
C11 H11A 0.9900 . ?
C12 H12 0.9900 . ?
C12 H12A 0.9900 . ?
C13 H13 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 H14 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 Cr1 O10 83.14(9) . . ?
O9 Cr1 O6 90.98(10) . . ?
O10 Cr1 O6 90.65(9) . . ?
O9 Cr1 O5 91.61(10) . . ?
O10 Cr1 O5 172.02(10) . . ?
O6 Cr1 O5 83.40(9) . . ?
O9 Cr1 O1 92.26(10) . . ?
O10 Cr1 O1 92.97(9) . . ?
O6 Cr1 O1 175.41(10) . . ?
O5 Cr1 O1 93.25(9) . . ?
O9 Cr1 O2 174.66(10) . . ?
O10 Cr1 O2 95.84(9) . . ?
O6 Cr1 O2 94.28(10) . . ?
O5 Cr1 O2 89.92(10) . . ?
O1 Cr1 O2 82.54(10) . . ?
O14 Co1 O13 91.98(9) . . ?
O14 Co1 O8 168.57(9) . 3_445 ?
O13 Co1 O8 91.47(9) . 3_445 ?
O14 Co1 O7 89.58(9) . 3_445 ?
O13 Co1 O7 90.77(10) . 3_445 ?
O8 Co1 O7 79.48(8) 3_445 3_445 ?
O14 Co1 O4 95.72(9) . . ?
O13 Co1 O4 90.59(10) . . ?
O8 Co1 O4 95.14(8) 3_445 . ?
O7 Co1 O4 174.48(9) 3_445 . ?
O14 Co1 O3 91.52(9) . . ?
O13 Co1 O3 168.98(9) . . ?
O8 Co1 O3 87.12(9) 3_445 . ?
O7 Co1 O3 99.70(9) 3_445 . ?
O4 Co1 O3 78.66(9) . . ?
C1 O1 Cr1 113.7(2) . . ?
C2 O2 Cr1 113.2(2) . . ?
C1 O3 Co1 112.1(2) . . ?
C2 O4 Co1 112.48(19) . . ?
C3 O5 Cr1 112.65(18) . . ?
C4 O6 Cr1 112.74(18) . . ?
C3 O7 Co1 111.99(19) . 3 ?
C4 O8 Co1 112.38(18) . 3 ?
C5 O9 Cr1 114.9(2) . . ?
C6 O10 Cr1 114.12(19) . . ?
H15A O15 H15B 99(4) . . ?
H16A O16 H16B 108(5) . . ?
C13 O17 H17 109.5 . . ?
C14 O18 H18 109.5 . . ?
C9 N1 C11 111.1(3) . . ?
C9 N1 C7 111.1(3) . . ?
C11 N1 C7 107.4(3) . . ?
C9 N1 H1 108(4) . . ?
C11 N1 H1 108(4) . . ?
C7 N1 H1 111(4) . . ?
C12 N2 C10 109.1(3) . . ?
C12 N2 C8 108.2(3) . . ?
C10 N2 C8 109.0(3) . . ?
O3 C1 O1 126.6(3) . . ?
O3 C1 C2 117.9(3) . . ?
O1 C1 C2 115.6(2) . . ?
O4 C2 O2 126.8(3) . . ?
O4 C2 C1 118.7(2) . . ?
O2 C2 C1 114.5(3) . . ?
O7 C3 O5 127.3(3) . . ?
O7 C3 C4 117.8(2) . . ?
O5 C3 C4 114.8(2) . . ?
O8 C4 O6 126.3(3) . . ?
O8 C4 C3 118.1(2) . . ?
O6 C4 C3 115.6(2) . . ?
O11 C5 O9 125.2(3) . . ?
O11 C5 C6 120.9(3) . . ?
O9 C5 C6 114.0(3) . . ?
O12 C6 O10 126.7(3) . . ?
O12 C6 C5 119.6(3) . . ?
O10 C6 C5 113.7(2) . . ?
N1 C7 C8 106.2(3) . . ?
N1 C7 H7 110.5 . . ?
C8 C7 H7 110.5 . . ?
N1 C7 H7A 110.5 . . ?
C8 C7 H7A 110.5 . . ?
H7 C7 H7A 108.7 . . ?
N2 C8 C7 110.6(3) . . ?
N2 C8 H8 109.5 . . ?
C7 C8 H8 109.5 . . ?
N2 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
H8 C8 H8A 108.1 . . ?
N1 C9 C10 107.6(3) . . ?
N1 C9 H9 110.2 . . ?
C10 C9 H9 110.2 . . ?
N1 C9 H9A 110.2 . . ?
C10 C9 H9A 110.2 . . ?
H9 C9 H9A 108.5 . . ?
N2 C10 C9 110.0(3) . . ?
N2 C10 H10 109.7 . . ?
C9 C10 H10 109.7 . . ?
N2 C10 H10A 109.7 . . ?
C9 C10 H10A 109.7 . . ?
H10 C10 H10A 108.2 . . ?
N1 C11 C12 108.0(3) . . ?
N1 C11 H11 110.1 . . ?
C12 C11 H11 110.1 . . ?
N1 C11 H11A 110.1 . . ?
C12 C11 H11A 110.1 . . ?
H11 C11 H11A 108.4 . . ?
N2 C12 C11 109.9(3) . . ?
N2 C12 H12 109.7 . . ?
C11 C12 H12 109.7 . . ?
N2 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
H12 C12 H12A 108.2 . . ?
O17 C13 H13 109.5 . . ?
O17 C13 H13A 109.5 . . ?
H13 C13 H13A 109.5 . . ?
O17 C13 H13B 109.5 . . ?
H13 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O18 C14 H14 109.5 . . ?
O18 C14 H14A 109.5 . . ?
H14 C14 H14A 109.5 . . ?
O18 C14 H14B 109.5 . . ?
H14 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?

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 O3 C1 O1 -178.5(2) . . . . ?
Co1 O3 C1 C2 1.1(3) . . . . ?
Cr1 O1 C1 O3 178.0(2) . . . . ?
Cr1 O1 C1 C2 -1.6(3) . . . . ?
Co1 O4 C2 O2 -176.2(2) . . . . ?
Co1 O4 C2 C1 3.8(3) . . . . ?
Cr1 O2 C2 O4 -172.7(2) . . . . ?
Cr1 O2 C2 C1 7.3(3) . . . . ?
O3 C1 C2 O4 -3.6(4) . . . . ?
O1 C1 C2 O4 176.1(3) . . . . ?
O3 C1 C2 O2 176.4(3) . . . . ?
O1 C1 C2 O2 -3.9(3) . . . . ?
Co1 O7 C3 O5 177.9(3) 3 . . . ?
Co1 O7 C3 C4 -0.8(3) 3 . . . ?
Cr1 O5 C3 O7 176.2(3) . . . . ?
Cr1 O5 C3 C4 -5.0(3) . . . . ?
Co1 O8 C4 O6 -175.4(3) 3 . . . ?
Co1 O8 C4 C3 4.5(3) 3 . . . ?
Cr1 O6 C4 O8 -172.7(3) . . . . ?
Cr1 O6 C4 C3 7.4(3) . . . . ?
O7 C3 C4 O8 -2.7(4) . . . . ?
O5 C3 C4 O8 178.5(3) . . . . ?
O7 C3 C4 O6 177.2(3) . . . . ?
O5 C3 C4 O6 -1.6(4) . . . . ?
Cr1 O9 C5 O11 -179.1(3) . . . . ?
Cr1 O9 C5 C6 0.1(3) . . . . ?
Cr1 O10 C6 O12 175.5(2) . . . . ?
Cr1 O10 C6 C5 -4.6(3) . . . . ?
O11 C5 C6 O12 2.2(4) . . . . ?
O9 C5 C6 O12 -177.0(3) . . . . ?
O11 C5 C6 O10 -177.7(3) . . . . ?
O9 C5 C6 O10 3.1(4) . . . . ?
C9 N1 C7 C8 50.7(4) . . . . ?
C11 N1 C7 C8 -71.0(4) . . . . ?
C12 N2 C8 C7 50.0(4) . . . . ?
C10 N2 C8 C7 -68.5(4) . . . . ?
N1 C7 C8 N2 16.4(4) . . . . ?
C11 N1 C9 C10 50.2(4) . . . . ?
C7 N1 C9 C10 -69.3(4) . . . . ?
C12 N2 C10 C9 -68.5(4) . . . . ?
C8 N2 C10 C9 49.5(4) . . . . ?
N1 C9 C10 N2 15.5(5) . . . . ?
C9 N1 C11 C12 -67.1(4) . . . . ?
C7 N1 C11 C12 54.6(4) . . . . ?
C10 N2 C12 C11 51.1(4) . . . . ?
C8 N2 C12 C11 -67.4(4) . . . . ?
N1 C11 C12 N2 13.1(4) . . . . ?

_refine_diff_density_max         0.664
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.102

####################################################################### 
# 
# 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_Comp2
_database_code_depnum_ccdc_archive 'CCDC 1496001'
_audit_update_record             
;
2016-08-31 deposited with the CCDC.
2016-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Cr O14 Zn, C6 H13 N2, 2(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C14 H29 Cr N2 O18 Zn'
_chemical_formula_weight         630.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 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'

_cell_length_a                   14.632(5)
_cell_length_b                   11.548(5)
_cell_length_c                   15.017(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.246(5)
_cell_angle_gamma                90
_cell_volume                     2517.2(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3202
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      28.96

_exptl_crystal_description       plates
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_F_000             1300
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_exptl_absorpt_coefficient_mu    1.469
_shelx_estimated_absorpt_T_min   0.591
_shelx_estimated_absorpt_T_max   0.591
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5911
_exptl_absorpt_correction_T_max  0.5911
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6673
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.254
_diffrn_reflns_theta_max         27.442
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4954
_reflns_number_gt                4854
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_max     0.987
_reflns_Friedel_fraction_full    0.998

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0543P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.050(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4954
_refine_ls_number_parameters     342
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0989
_refine_ls_wR_factor_gt          0.0986
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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
Cr1 Cr 0.21720(4) 0.73824(5) 0.37688(4) 0.01327(16) Uani 1 1 d . . . . .
Zn1 Zn 0.55670(3) 0.64518(4) 0.29047(3) 0.01503(14) Uani 1 1 d . . . . .
O1 O 0.3393(2) 0.6880(3) 0.4371(2) 0.0178(6) Uani 1 1 d . . . . .
O2 O 0.2799(2) 0.7216(3) 0.2674(2) 0.0170(6) Uani 1 1 d . . . . .
O3 O 0.4816(3) 0.6500(2) 0.4058(2) 0.0196(8) Uani 1 1 d . . . . .
O4 O 0.4215(2) 0.6929(3) 0.2300(2) 0.0190(6) Uani 1 1 d . . . . .
O5 O 0.2510(2) 0.9044(3) 0.3852(2) 0.0166(6) Uani 1 1 d . . . . .
O6 O 0.1015(2) 0.7980(3) 0.3109(2) 0.0178(6) Uani 1 1 d . . . . .
O7 O 0.1831(2) 1.0775(3) 0.3574(2) 0.0202(6) Uani 1 1 d . . . . .
O8 O 0.0288(2) 0.9658(3) 0.2821(2) 0.0197(6) Uani 1 1 d . . . . .
O9 O 0.1656(2) 0.7461(3) 0.4903(2) 0.0180(7) Uani 1 1 d . . . . .
O10 O 0.1670(2) 0.5804(2) 0.3735(2) 0.0177(6) Uani 1 1 d . . . . .
O11 O 0.0840(3) 0.6429(3) 0.5771(2) 0.0249(7) Uani 1 1 d . . . . .
O12 O 0.0799(2) 0.4666(2) 0.4497(2) 0.0234(7) Uani 1 1 d . . . . .
O13 O 0.6021(3) 0.6446(2) 0.1684(3) 0.0208(8) Uani 1 1 d . . . . .
O14 O 0.6035(2) 0.8071(3) 0.3157(2) 0.0184(6) Uani 1 1 d . . . . .
N1 N 0.4799(3) 0.0444(3) 0.1150(3) 0.0216(8) Uani 1 1 d . . . . .
H1 H 0.5249 -0.0022 0.0851 0.026 Uiso 1 1 calc R U . . .
N2 N 0.3652(3) 0.1604(3) 0.1914(3) 0.0206(8) Uani 1 1 d . . . . .
C1 C 0.3992(3) 0.6762(3) 0.3845(3) 0.0155(7) Uani 1 1 d . . . . .
C2 C 0.3656(3) 0.6990(3) 0.2841(3) 0.0161(8) Uani 1 1 d . . . . .
C3 C 0.1844(3) 0.9709(3) 0.3560(3) 0.0143(7) Uani 1 1 d . . . . .
C4 C 0.0967(3) 0.9072(4) 0.3121(3) 0.0161(8) Uani 1 1 d . . . . .
C5 C 0.1232(3) 0.6556(3) 0.5093(3) 0.0184(9) Uani 1 1 d . . . . .
C6 C 0.1215(3) 0.5562(3) 0.4393(3) 0.0165(8) Uani 1 1 d . . . . .
C7 C 0.5061(5) 0.1712(5) 0.1132(5) 0.0392(13) Uani 1 1 d . . . . .
H7 H 0.5154 0.1949 0.0517 0.047 Uiso 1 1 calc R U . . .
H7A H 0.5638 0.1856 0.1537 0.047 Uiso 1 1 calc R U . . .
C8 C 0.4254(4) 0.2393(4) 0.1451(4) 0.0284(10) Uani 1 1 d . . . . .
H8 H 0.4500 0.3013 0.1869 0.034 Uiso 1 1 calc R U . . .
H8A H 0.3885 0.2760 0.0929 0.034 Uiso 1 1 calc R U . . .
C9 C 0.3873(4) 0.0261(6) 0.0680(4) 0.0417(14) Uani 1 1 d . . . . .
H9 H 0.3749 -0.0579 0.0604 0.050 Uiso 1 1 calc R U . . .
H9A H 0.3819 0.0622 0.0078 0.050 Uiso 1 1 calc R U . . .
C10 C 0.3172(3) 0.0812(5) 0.1239(4) 0.0333(11) Uani 1 1 d . . . . .
H10 H 0.2702 0.1245 0.0840 0.040 Uiso 1 1 calc R U . . .
H10A H 0.2856 0.0198 0.1544 0.040 Uiso 1 1 calc R U . . .
C11 C 0.4860(4) 0.0100(5) 0.2111(4) 0.0399(13) Uani 1 1 d . . . . .
H11 H 0.5507 0.0146 0.2398 0.048 Uiso 1 1 calc R U . . .
H11A H 0.4643 -0.0706 0.2162 0.048 Uiso 1 1 calc R U . . .
C12 C 0.4249(3) 0.0938(4) 0.2580(3) 0.0242(9) Uani 1 1 d . . . . .
H12 H 0.3868 0.0492 0.2958 0.029 Uiso 1 1 calc R U . . .
H12A H 0.4645 0.1473 0.2974 0.029 Uiso 1 1 calc R U . . .
O15 O 0.0862(3) 0.9561(4) 0.0640(3) 0.0449(11) Uani 1 1 d D . . . .
H15A H 0.066(6) 0.906(5) 0.025(4) 0.067 Uiso 1 1 d D U . . .
H15B H 0.090(7) 1.011(5) 0.026(4) 0.067 Uiso 1 1 d D U . . .
O16 O 0.7251(4) 0.3030(5) 0.0849(3) 0.0500(12) Uani 1 1 d D . . . .
H16A H 0.756(6) 0.264(7) 0.051(6) 0.075 Uiso 1 1 d D U . . .
H16B H 0.688(6) 0.253(6) 0.099(6) 0.075 Uiso 1 1 d D U . . .
O17 O 0.2746(2) 0.3178(3) 0.2796(3) 0.0293(8) Uani 1 1 d . . . . .
H17 H 0.2957 0.2632 0.2514 0.044 Uiso 1 1 calc R U . . .
O18 O 0.3391(4) 0.2703(5) 0.4645(4) 0.0580(14) Uani 1 1 d . . . . .
H18 H 0.3174 0.2755 0.4101 0.087 Uiso 1 1 calc R U . . .
C13 C 0.2878(4) 0.4250(4) 0.2349(5) 0.0376(13) Uani 1 1 d . . . . .
H13 H 0.2547 0.4869 0.2619 0.056 Uiso 1 1 calc R U . . .
H13A H 0.2641 0.4179 0.1711 0.056 Uiso 1 1 calc R U . . .
H13B H 0.3537 0.4435 0.2411 0.056 Uiso 1 1 calc R U . . .
C14 C 0.3975(7) 0.3648(8) 0.4881(6) 0.061(2) Uani 1 1 d . . . . .
H14 H 0.3635 0.4371 0.4745 0.092 Uiso 1 1 calc R U . . .
H14A H 0.4501 0.3617 0.4538 0.092 Uiso 1 1 calc R U . . .
H14B H 0.4196 0.3616 0.5524 0.092 Uiso 1 1 calc R U . . .


_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
Cr1 O9 1.950(3) . ?
Cr1 O10 1.963(3) . ?
Cr1 O6 1.975(3) . ?
Cr1 O5 1.982(3) . ?
Cr1 O1 1.984(3) . ?
Cr1 O2 1.990(3) . ?
Zn1 O14 2.011(3) . ?
Zn1 O13 2.027(4) . ?
Zn1 O8 2.112(3) 3_545 ?
Zn1 O7 2.139(3) 3_545 ?
Zn1 O4 2.143(3) . ?
Zn1 O3 2.166(4) . ?
O1 C1 1.259(5) . ?
O2 C2 1.275(5) . ?
O3 C1 1.245(6) . ?
O4 C2 1.226(5) . ?
O5 C3 1.275(5) . ?
O6 C4 1.264(6) . ?
O7 C3 1.231(5) . ?
O7 Zn1 2.139(3) 3_455 ?
O8 C4 1.238(5) . ?
O8 Zn1 2.112(3) 3_455 ?
O9 C5 1.266(6) . ?
O10 C6 1.289(6) . ?
O11 C5 1.238(6) . ?
O12 C6 1.221(5) . ?
N1 C9 1.462(7) . ?
N1 C11 1.489(7) . ?
N1 C7 1.515(7) . ?
N1 H1 1.0000 . ?
N2 C12 1.461(6) . ?
N2 C10 1.474(6) . ?
N2 C8 1.498(7) . ?
C1 C2 1.548(5) . ?
C3 C4 1.552(5) . ?
C5 C6 1.555(6) . ?
C7 C8 1.544(7) . ?
C7 H7 0.9900 . ?
C7 H7A 0.9900 . ?
C8 H8 0.9900 . ?
C8 H8A 0.9900 . ?
C9 C10 1.543(7) . ?
C9 H9 0.9900 . ?
C9 H9A 0.9900 . ?
C10 H10 0.9900 . ?
C10 H10A 0.9900 . ?
C11 C12 1.546(7) . ?
C11 H11 0.9900 . ?
C11 H11A 0.9900 . ?
C12 H12 0.9900 . ?
C12 H12A 0.9900 . ?
O15 H15A 0.85(3) . ?
O15 H15B 0.86(3) . ?
O16 H16A 0.85(3) . ?
O16 H16B 0.83(3) . ?
O17 C13 1.433(7) . ?
O17 H17 0.8400 . ?
O18 C14 1.404(9) . ?
O18 H18 0.8400 . ?
C13 H13 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 H14 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 Cr1 O10 83.14(13) . . ?
O9 Cr1 O6 91.15(15) . . ?
O10 Cr1 O6 91.00(13) . . ?
O9 Cr1 O5 91.20(13) . . ?
O10 Cr1 O5 171.97(14) . . ?
O6 Cr1 O5 83.39(13) . . ?
O9 Cr1 O1 92.35(14) . . ?
O10 Cr1 O1 93.00(13) . . ?
O6 Cr1 O1 174.98(13) . . ?
O5 Cr1 O1 92.93(13) . . ?
O9 Cr1 O2 174.47(15) . . ?
O10 Cr1 O2 95.67(13) . . ?
O6 Cr1 O2 94.28(13) . . ?
O5 Cr1 O2 90.49(13) . . ?
O1 Cr1 O2 82.30(13) . . ?
O14 Zn1 O13 91.76(13) . . ?
O14 Zn1 O8 169.12(12) . 3_545 ?
O13 Zn1 O8 91.49(12) . 3_545 ?
O14 Zn1 O7 89.87(12) . 3_545 ?
O13 Zn1 O7 93.53(14) . 3_545 ?
O8 Zn1 O7 79.56(12) 3_545 3_545 ?
O14 Zn1 O4 96.58(13) . . ?
O13 Zn1 O4 90.45(14) . . ?
O8 Zn1 O4 93.78(12) 3_545 . ?
O7 Zn1 O4 172.31(12) 3_545 . ?
O14 Zn1 O3 91.19(12) . . ?
O13 Zn1 O3 168.68(14) . . ?
O8 Zn1 O3 87.64(12) 3_545 . ?
O7 Zn1 O3 97.41(13) 3_545 . ?
O4 Zn1 O3 78.35(13) . . ?
C1 O1 Cr1 113.8(3) . . ?
C2 O2 Cr1 113.7(3) . . ?
C1 O3 Zn1 111.9(3) . . ?
C2 O4 Zn1 113.0(3) . . ?
C3 O5 Cr1 112.8(3) . . ?
C4 O6 Cr1 112.8(3) . . ?
C3 O7 Zn1 111.8(3) . 3_455 ?
C4 O8 Zn1 111.9(3) . 3_455 ?
C5 O9 Cr1 114.5(3) . . ?
C6 O10 Cr1 114.2(3) . . ?
C9 N1 C11 111.6(5) . . ?
C9 N1 C7 110.7(5) . . ?
C11 N1 C7 106.9(4) . . ?
C9 N1 H1 109.2 . . ?
C11 N1 H1 109.2 . . ?
C7 N1 H1 109.2 . . ?
C12 N2 C10 109.6(4) . . ?
C12 N2 C8 107.5(4) . . ?
C10 N2 C8 108.4(4) . . ?
O3 C1 O1 126.4(4) . . ?
O3 C1 C2 118.0(4) . . ?
O1 C1 C2 115.6(3) . . ?
O4 C2 O2 127.1(4) . . ?
O4 C2 C1 118.7(3) . . ?
O2 C2 C1 114.2(4) . . ?
O7 C3 O5 127.5(4) . . ?
O7 C3 C4 117.9(4) . . ?
O5 C3 C4 114.6(3) . . ?
O8 C4 O6 125.7(4) . . ?
O8 C4 C3 118.6(3) . . ?
O6 C4 C3 115.7(3) . . ?
O11 C5 O9 125.1(4) . . ?
O11 C5 C6 119.9(4) . . ?
O9 C5 C6 115.0(4) . . ?
O12 C6 O10 126.6(4) . . ?
O12 C6 C5 120.3(4) . . ?
O10 C6 C5 113.1(4) . . ?
N1 C7 C8 106.3(4) . . ?
N1 C7 H7 110.5 . . ?
C8 C7 H7 110.5 . . ?
N1 C7 H7A 110.5 . . ?
C8 C7 H7A 110.5 . . ?
H7 C7 H7A 108.7 . . ?
N2 C8 C7 110.6(4) . . ?
N2 C8 H8 109.5 . . ?
C7 C8 H8 109.5 . . ?
N2 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
H8 C8 H8A 108.1 . . ?
N1 C9 C10 108.4(4) . . ?
N1 C9 H9 110.0 . . ?
C10 C9 H9 110.0 . . ?
N1 C9 H9A 110.0 . . ?
C10 C9 H9A 110.0 . . ?
H9 C9 H9A 108.4 . . ?
N2 C10 C9 109.8(4) . . ?
N2 C10 H10 109.7 . . ?
C9 C10 H10 109.7 . . ?
N2 C10 H10A 109.7 . . ?
C9 C10 H10A 109.7 . . ?
H10 C10 H10A 108.2 . . ?
N1 C11 C12 107.8(4) . . ?
N1 C11 H11 110.1 . . ?
C12 C11 H11 110.1 . . ?
N1 C11 H11A 110.1 . . ?
C12 C11 H11A 110.1 . . ?
H11 C11 H11A 108.5 . . ?
N2 C12 C11 110.4(4) . . ?
N2 C12 H12 109.6 . . ?
C11 C12 H12 109.6 . . ?
N2 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
H12 C12 H12A 108.1 . . ?
H15A O15 H15B 96(5) . . ?
H16A O16 H16B 101(6) . . ?
C13 O17 H17 109.5 . . ?
C14 O18 H18 109.5 . . ?
O17 C13 H13 109.5 . . ?
O17 C13 H13A 109.5 . . ?
H13 C13 H13A 109.5 . . ?
O17 C13 H13B 109.5 . . ?
H13 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O18 C14 H14 109.5 . . ?
O18 C14 H14A 109.5 . . ?
H14 C14 H14A 109.5 . . ?
O18 C14 H14B 109.5 . . ?
H14 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?

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
Zn1 O3 C1 O1 -178.5(3) . . . . ?
Zn1 O3 C1 C2 0.5(4) . . . . ?
Cr1 O1 C1 O3 177.1(3) . . . . ?
Cr1 O1 C1 C2 -1.9(4) . . . . ?
Zn1 O4 C2 O2 -177.5(3) . . . . ?
Zn1 O4 C2 C1 1.8(4) . . . . ?
Cr1 O2 C2 O4 -174.2(3) . . . . ?
Cr1 O2 C2 C1 6.5(4) . . . . ?
O3 C1 C2 O4 -1.6(5) . . . . ?
O1 C1 C2 O4 177.5(4) . . . . ?
O3 C1 C2 O2 177.8(4) . . . . ?
O1 C1 C2 O2 -3.1(5) . . . . ?
Zn1 O7 C3 O5 175.7(4) 3_455 . . . ?
Zn1 O7 C3 C4 -2.7(5) 3_455 . . . ?
Cr1 O5 C3 O7 175.5(4) . . . . ?
Cr1 O5 C3 C4 -6.1(4) . . . . ?
Zn1 O8 C4 O6 -175.7(3) 3_455 . . . ?
Zn1 O8 C4 C3 4.8(5) 3_455 . . . ?
Cr1 O6 C4 O8 -173.9(4) . . . . ?
Cr1 O6 C4 C3 5.6(4) . . . . ?
O7 C3 C4 O8 -1.5(6) . . . . ?
O5 C3 C4 O8 179.9(4) . . . . ?
O7 C3 C4 O6 179.0(4) . . . . ?
O5 C3 C4 O6 0.4(5) . . . . ?
Cr1 O9 C5 O11 -178.8(4) . . . . ?
Cr1 O9 C5 C6 0.6(5) . . . . ?
Cr1 O10 C6 O12 176.0(4) . . . . ?
Cr1 O10 C6 C5 -4.1(4) . . . . ?
O11 C5 C6 O12 1.7(7) . . . . ?
O9 C5 C6 O12 -177.7(4) . . . . ?
O11 C5 C6 O10 -178.2(4) . . . . ?
O9 C5 C6 O10 2.4(6) . . . . ?
C9 N1 C7 C8 50.3(6) . . . . ?
C11 N1 C7 C8 -71.5(5) . . . . ?
C12 N2 C8 C7 49.8(6) . . . . ?
C10 N2 C8 C7 -68.6(5) . . . . ?
N1 C7 C8 N2 16.7(6) . . . . ?
C11 N1 C9 C10 49.6(6) . . . . ?
C7 N1 C9 C10 -69.3(6) . . . . ?
C12 N2 C10 C9 -67.5(6) . . . . ?
C8 N2 C10 C9 49.6(6) . . . . ?
N1 C9 C10 N2 15.5(7) . . . . ?
C9 N1 C11 C12 -66.3(6) . . . . ?
C7 N1 C11 C12 54.9(6) . . . . ?
C10 N2 C12 C11 50.2(6) . . . . ?
C8 N2 C12 C11 -67.5(5) . . . . ?
N1 C11 C12 N2 13.3(6) . . . . ?

_refine_diff_density_max         0.867
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.105

####################################################################### 
# 
# 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_Comp3
_database_code_depnum_ccdc_archive 'CCDC 1496002'
_audit_update_record             
;
2016-08-31 deposited with the CCDC.
2016-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H6 Co Cr O14, C10 H21 N2'
_chemical_formula_sum            'C17 H27 Co Cr N2 O14'
_chemical_formula_weight         594.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   9.085(2)
_cell_length_b                   13.921(4)
_cell_length_c                   10.159(3)
_cell_angle_alpha                90
_cell_angle_beta                 115.178(5)
_cell_angle_gamma                90
_cell_volume                     1162.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1056
_cell_measurement_theta_min      2.477
_cell_measurement_theta_max      22.2275

_exptl_crystal_description       plates
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_F_000             612
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.255
_shelx_estimated_absorpt_T_min   0.787
_shelx_estimated_absorpt_T_max   0.940
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7874
_exptl_absorpt_correction_T_max  0.9399
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7313
_diffrn_reflns_av_unetI/netI     0.1099
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.215
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_point_group_measured_fraction_full 0.918
_reflns_number_total             4694
_reflns_number_gt                4079
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.721
_reflns_Friedel_fraction_max     0.767
_reflns_Friedel_fraction_full    0.830

_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0608P)²+0.2840P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1099 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4694
_refine_ls_number_parameters     324
_refine_ls_number_restraints     124
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0812
_refine_ls_wR_factor_ref         0.1578
_refine_ls_wR_factor_gt          0.1510
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.076
_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
Cr1 Cr 0.07854(18) 0.29428(11) 0.72375(17) 0.0134(4) Uani 1 1 d . . . . .
Co1 Co 0.54765(15) 0.09805(9) 0.66253(14) 0.0133(3) Uani 1 1 d . . . . .
O1 O 0.2017(8) 0.3010(5) 0.6045(7) 0.0170(15) Uani 1 1 d . U . . .
O2 O 0.2254(8) 0.1849(5) 0.8168(7) 0.0121(15) Uani 1 1 d . U . . .
O3 O 0.3898(9) 0.2158(6) 0.5662(8) 0.0223(18) Uani 1 1 d . U . . .
O4 O 0.4129(8) 0.0962(6) 0.7857(7) 0.0198(16) Uani 1 1 d . U . . .
O5 O -0.0775(8) 0.2029(5) 0.5845(8) 0.0158(16) Uani 1 1 d . U . . .
O6 O -0.0585(8) 0.2739(6) 0.8308(7) 0.0182(18) Uani 1 1 d . U . . .
O7 O -0.2955(8) 0.1163(5) 0.5615(7) 0.0169(17) Uani 1 1 d . U . . .
O8 O -0.2892(9) 0.2021(5) 0.8024(8) 0.0154(17) Uani 1 1 d . U . . .
O9 O -0.0517(9) 0.4059(5) 0.6292(8) 0.0206(18) Uani 1 1 d . . . . .
O10 O 0.2126(9) 0.3882(5) 0.8678(8) 0.0155(16) Uani 1 1 d . . . . .
O11 O -0.0832(8) 0.5595(5) 0.6705(8) 0.0208(17) Uani 1 1 d . . . . .
O12 O 0.2022(9) 0.5407(5) 0.9301(8) 0.0228(17) Uani 1 1 d . . . . .
O13 O 0.6855(9) -0.0127(6) 0.7859(8) 0.0222(19) Uani 1 1 d D . . . .
H13C H 0.716(11) 0.000(9) 0.874(4) 0.033 Uiso 1 1 d D U . . .
H13D H 0.771(7) -0.014(9) 0.775(10) 0.033 Uiso 1 1 d D U . . .
O14 O 0.3950(9) 0.0128(6) 0.5017(8) 0.0272(19) Uani 1 1 d . . . . .
H14C H 0.2847 0.0327 0.4535 0.033 Uiso 1 1 calc R U . . .
N1 N 0.7660(10) 0.3250(6) 0.1580(9) 0.0150(19) Uani 1 1 d . U . . .
N2 N 1.0139(10) 0.4317(6) 0.2032(9) 0.0173(19) Uani 1 1 d . U . . .
C1 C 0.3032(12) 0.2321(8) 0.6306(11) 0.015(2) Uani 1 1 d . U . . .
C2 C 0.3177(12) 0.1648(8) 0.7564(11) 0.015(2) Uani 1 1 d . U . . .
C3 C -0.1830(11) 0.1743(7) 0.6244(10) 0.010(2) Uani 1 1 d . U . . .
C4 C -0.1788(12) 0.2211(7) 0.7649(11) 0.014(2) Uani 1 1 d . U . . .
C5 C -0.0083(12) 0.4835(7) 0.7016(11) 0.018(2) Uani 1 1 d . . . . .
C6 C 0.1494(11) 0.4734(7) 0.8445(10) 0.014(2) Uani 1 1 d . . . . .
C7 C 0.4389(13) -0.0755(8) 0.4539(12) 0.030(3) Uani 1 1 d . . . . .
H7 H 0.5574 -0.0787 0.4894 0.044 Uiso 1 1 calc R U . . .
H7A H 0.3880 -0.0778 0.3474 0.044 Uiso 1 1 calc R U . . .
H7B H 0.4012 -0.1300 0.4923 0.044 Uiso 1 1 calc R U . . .
C8 C 0.3388(14) 0.1736(10) 0.1828(13) 0.034(3) Uani 1 1 d . . . . .
H8 H 0.3626 0.2027 0.2775 0.051 Uiso 1 1 calc R U . . .
H8A H 0.2497 0.1273 0.1584 0.051 Uiso 1 1 calc R U . . .
H8B H 0.3069 0.2239 0.1082 0.051 Uiso 1 1 calc R U . . .
C9 C 0.4873(14) 0.1230(9) 0.1891(12) 0.031(3) Uani 1 1 d . . . . .
H9 H 0.4657 0.0978 0.0915 0.038 Uiso 1 1 calc R U . . .
H9A H 0.5125 0.0678 0.2568 0.038 Uiso 1 1 calc R U . . .
C10 C 0.6345(13) 0.1914(8) 0.2406(12) 0.027(3) Uani 1 1 d . . . . .
H10 H 0.6414 0.2276 0.3270 0.033 Uiso 1 1 calc R U . . .
H10A H 0.7356 0.1535 0.2692 0.033 Uiso 1 1 calc R U . . .
C11 C 0.6194(12) 0.2616(8) 0.1206(11) 0.022(2) Uani 1 1 d . . . . .
H11 H 0.6010 0.2248 0.0316 0.026 Uiso 1 1 calc R U . . .
H11A H 0.5229 0.3027 0.0985 0.026 Uiso 1 1 calc R U . . .
C12 C 0.9134(12) 0.2652(8) 0.1751(12) 0.026(3) Uani 1 1 d . U . . .
H12 H 0.9438 0.2217 0.2598 0.031 Uiso 1 1 calc R U . . .
H12A H 0.8874 0.2255 0.0871 0.031 Uiso 1 1 calc R U . . .
C13 C 1.0531(12) 0.3323(8) 0.1974(11) 0.021(2) Uani 1 1 d . U . . .
H13 H 1.1472 0.3151 0.2892 0.025 Uiso 1 1 calc R U . . .
H13A H 1.0858 0.3231 0.1168 0.025 Uiso 1 1 calc R U . . .
C14 C 0.7317(12) 0.3922(8) 0.0324(11) 0.022(2) Uani 1 1 d . U . . .
H14 H 0.6350 0.4318 0.0162 0.026 Uiso 1 1 calc R U . . .
H14A H 0.7082 0.3546 -0.0570 0.026 Uiso 1 1 calc R U . . .
C15 C 0.8800(12) 0.4583(8) 0.0643(12) 0.023(2) Uani 1 1 d . U . . .
H15 H 0.9156 0.4523 -0.0149 0.028 Uiso 1 1 calc R U . . .
H15A H 0.8488 0.5260 0.0682 0.028 Uiso 1 1 calc R U . . .
C16 C 0.8097(14) 0.3830(9) 0.2911(13) 0.028(3) Uani 1 1 d . U . . .
H16 H 0.8331 0.3400 0.3752 0.033 Uiso 1 1 calc R U . . .
H16A H 0.7169 0.4247 0.2803 0.033 Uiso 1 1 calc R U . . .
C17 C 0.9594(12) 0.4454(8) 0.3191(10) 0.016(2) Uani 1 1 d . U . . .
H17 H 0.9321 0.5138 0.3233 0.020 Uiso 1 1 calc R U . . .
H17A H 1.0484 0.4279 0.4141 0.020 Uiso 1 1 calc R U . . .


_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
Cr1 O9 1.942(7) . ?
Cr1 O10 1.954(7) . ?
Cr1 O1 1.970(7) . ?
Cr1 O2 1.979(7) . ?
Cr1 O5 1.980(7) . ?
Cr1 O6 1.991(7) . ?
Co1 O14 2.018(8) . ?
Co1 O13 2.044(8) . ?
Co1 O4 2.090(7) . ?
Co1 O7 2.096(7) 1_655 ?
Co1 O3 2.123(8) . ?
Co1 O8 2.127(8) 1_655 ?
O1 C1 1.278(12) . ?
O2 C2 1.264(12) . ?
O3 C1 1.239(11) . ?
O4 C2 1.237(13) . ?
O5 C3 1.254(11) . ?
O6 C4 1.249(12) . ?
O7 C3 1.245(11) . ?
O7 Co1 2.096(7) 1_455 ?
O8 C4 1.244(12) . ?
O8 Co1 2.127(8) 1_455 ?
O9 C5 1.271(12) . ?
O10 C6 1.294(12) . ?
O11 C5 1.225(12) . ?
O12 C6 1.229(12) . ?
O13 H13C 0.84(3) . ?
O13 H13D 0.83(3) . ?
O14 C7 1.439(13) . ?
O14 H14C 0.9500 . ?
N1 C16 1.477(14) . ?
N1 C11 1.505(12) . ?
N1 C14 1.504(13) . ?
N1 C12 1.523(13) . ?
N2 C13 1.437(13) . ?
N2 C15 1.466(13) . ?
N2 C17 1.472(12) . ?
C1 C2 1.543(13) . ?
C3 C4 1.555(12) . ?
C5 C6 1.552(13) . ?
C7 H7 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 C9 1.499(16) . ?
C8 H8 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 C10 1.541(14) . ?
C9 H9 0.9900 . ?
C9 H9A 0.9900 . ?
C10 C11 1.522(14) . ?
C10 H10 0.9900 . ?
C10 H10A 0.9900 . ?
C11 H11 0.9900 . ?
C11 H11A 0.9900 . ?
C12 C13 1.514(14) . ?
C12 H12 0.9900 . ?
C12 H12A 0.9900 . ?
C13 H13 0.9900 . ?
C13 H13A 0.9900 . ?
C14 C15 1.548(14) . ?
C14 H14 0.9900 . ?
C14 H14A 0.9900 . ?
C15 H15 0.9900 . ?
C15 H15A 0.9900 . ?
C16 C17 1.535(14) . ?
C16 H16 0.9900 . ?
C16 H16A 0.9900 . ?
C17 H17 0.9900 . ?
C17 H17A 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 Cr1 O10 83.6(3) . . ?
O9 Cr1 O1 92.5(3) . . ?
O10 Cr1 O1 95.3(3) . . ?
O9 Cr1 O2 175.4(3) . . ?
O10 Cr1 O2 94.5(3) . . ?
O1 Cr1 O2 83.5(3) . . ?
O9 Cr1 O5 93.4(3) . . ?
O10 Cr1 O5 173.4(3) . . ?
O1 Cr1 O5 90.7(3) . . ?
O2 Cr1 O5 88.8(3) . . ?
O9 Cr1 O6 89.6(3) . . ?
O10 Cr1 O6 91.2(3) . . ?
O1 Cr1 O6 173.3(3) . . ?
O2 Cr1 O6 94.6(3) . . ?
O5 Cr1 O6 82.8(3) . . ?
O14 Co1 O13 94.8(3) . . ?
O14 Co1 O4 95.8(3) . . ?
O13 Co1 O4 89.2(3) . . ?
O14 Co1 O7 92.9(3) . 1_655 ?
O13 Co1 O7 91.4(3) . 1_655 ?
O4 Co1 O7 171.1(3) . 1_655 ?
O14 Co1 O3 89.1(3) . . ?
O13 Co1 O3 169.2(3) . . ?
O4 Co1 O3 80.4(3) . . ?
O7 Co1 O3 98.5(3) 1_655 . ?
O14 Co1 O8 170.1(3) . 1_655 ?
O13 Co1 O8 91.9(3) . 1_655 ?
O4 Co1 O8 91.6(3) . 1_655 ?
O7 Co1 O8 79.6(3) 1_655 1_655 ?
O3 Co1 O8 85.6(3) . 1_655 ?
C1 O1 Cr1 112.7(7) . . ?
C2 O2 Cr1 113.0(6) . . ?
C1 O3 Co1 110.7(7) . . ?
C2 O4 Co1 112.0(7) . . ?
C3 O5 Cr1 112.7(6) . . ?
C4 O6 Cr1 113.5(7) . . ?
C3 O7 Co1 114.1(6) . 1_455 ?
C4 O8 Co1 111.3(7) . 1_455 ?
C5 O9 Cr1 114.8(6) . . ?
C6 O10 Cr1 112.9(6) . . ?
Co1 O13 H13C 109(8) . . ?
Co1 O13 H13D 108(8) . . ?
H13C O13 H13D 104(6) . . ?
C7 O14 Co1 125.6(7) . . ?
C7 O14 H14C 117.2 . . ?
Co1 O14 H14C 117.2 . . ?
C16 N1 C11 114.6(8) . . ?
C16 N1 C14 108.4(8) . . ?
C11 N1 C14 108.0(7) . . ?
C16 N1 C12 108.3(8) . . ?
C11 N1 C12 110.4(8) . . ?
C14 N1 C12 106.9(8) . . ?
C13 N2 C15 108.8(8) . . ?
C13 N2 C17 109.3(8) . . ?
C15 N2 C17 108.3(8) . . ?
O3 C1 O1 126.3(10) . . ?
O3 C1 C2 118.4(9) . . ?
O1 C1 C2 115.3(8) . . ?
O4 C2 O2 126.5(10) . . ?
O4 C2 C1 118.2(9) . . ?
O2 C2 C1 115.3(8) . . ?
O7 C3 O5 127.9(9) . . ?
O7 C3 C4 115.9(8) . . ?
O5 C3 C4 116.1(8) . . ?
O8 C4 O6 126.6(10) . . ?
O8 C4 C3 119.0(8) . . ?
O6 C4 C3 114.4(8) . . ?
O11 C5 O9 125.7(9) . . ?
O11 C5 C6 120.7(9) . . ?
O9 C5 C6 113.6(9) . . ?
O12 C6 O10 124.0(9) . . ?
O12 C6 C5 121.3(9) . . ?
O10 C6 C5 114.5(9) . . ?
O14 C7 H7 109.5 . . ?
O14 C7 H7A 109.5 . . ?
H7 C7 H7A 109.5 . . ?
O14 C7 H7B 109.5 . . ?
H7 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C9 C8 H8 109.5 . . ?
C9 C8 H8A 109.5 . . ?
H8 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C8 C9 C10 111.1(11) . . ?
C8 C9 H9 109.4 . . ?
C10 C9 H9 109.4 . . ?
C8 C9 H9A 109.4 . . ?
C10 C9 H9A 109.4 . . ?
H9 C9 H9A 108.0 . . ?
C11 C10 C9 110.8(8) . . ?
C11 C10 H10 109.5 . . ?
C9 C10 H10 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10A 109.5 . . ?
H10 C10 H10A 108.1 . . ?
N1 C11 C10 113.9(8) . . ?
N1 C11 H11 108.8 . . ?
C10 C11 H11 108.8 . . ?
N1 C11 H11A 108.8 . . ?
C10 C11 H11A 108.8 . . ?
H11 C11 H11A 107.7 . . ?
C13 C12 N1 108.7(9) . . ?
C13 C12 H12 110.0 . . ?
N1 C12 H12 110.0 . . ?
C13 C12 H12A 110.0 . . ?
N1 C12 H12A 110.0 . . ?
H12 C12 H12A 108.3 . . ?
N2 C13 C12 113.2(8) . . ?
N2 C13 H13 108.9 . . ?
C12 C13 H13 108.9 . . ?
N2 C13 H13A 108.9 . . ?
C12 C13 H13A 108.9 . . ?
H13 C13 H13A 107.8 . . ?
N1 C14 C15 110.2(8) . . ?
N1 C14 H14 109.6 . . ?
C15 C14 H14 109.6 . . ?
N1 C14 H14A 109.6 . . ?
C15 C14 H14A 109.6 . . ?
H14 C14 H14A 108.1 . . ?
N2 C15 C14 110.1(9) . . ?
N2 C15 H15 109.6 . . ?
C14 C15 H15 109.6 . . ?
N2 C15 H15A 109.6 . . ?
C14 C15 H15A 109.6 . . ?
H15 C15 H15A 108.2 . . ?
N1 C16 C17 110.5(9) . . ?
N1 C16 H16 109.5 . . ?
C17 C16 H16 109.5 . . ?
N1 C16 H16A 109.5 . . ?
C17 C16 H16A 109.5 . . ?
H16 C16 H16A 108.1 . . ?
N2 C17 C16 110.6(8) . . ?
N2 C17 H17 109.5 . . ?
C16 C17 H17 109.5 . . ?
N2 C17 H17A 109.5 . . ?
C16 C17 H17A 109.5 . . ?
H17 C17 H17A 108.1 . . ?

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 O3 C1 O1 176.1(8) . . . . ?
Co1 O3 C1 C2 -3.1(10) . . . . ?
Cr1 O1 C1 O3 175.9(9) . . . . ?
Cr1 O1 C1 C2 -4.9(10) . . . . ?
Co1 O4 C2 O2 -177.0(8) . . . . ?
Co1 O4 C2 C1 5.1(10) . . . . ?
Cr1 O2 C2 O4 -174.7(8) . . . . ?
Cr1 O2 C2 C1 3.2(9) . . . . ?
O3 C1 C2 O4 -1.4(13) . . . . ?
O1 C1 C2 O4 179.3(10) . . . . ?
O3 C1 C2 O2 -179.5(10) . . . . ?
O1 C1 C2 O2 1.2(11) . . . . ?
Co1 O7 C3 O5 -175.8(8) 1_455 . . . ?
Co1 O7 C3 C4 0.6(9) 1_455 . . . ?
Cr1 O5 C3 O7 -179.1(8) . . . . ?
Cr1 O5 C3 C4 4.5(9) . . . . ?
Co1 O8 C4 O6 -174.6(9) 1_455 . . . ?
Co1 O8 C4 C3 4.0(10) 1_455 . . . ?
Cr1 O6 C4 O8 -174.8(8) . . . . ?
Cr1 O6 C4 C3 6.6(10) . . . . ?
O7 C3 C4 O8 -3.3(12) . . . . ?
O5 C3 C4 O8 173.5(10) . . . . ?
O7 C3 C4 O6 175.4(10) . . . . ?
O5 C3 C4 O6 -7.8(11) . . . . ?
Cr1 O9 C5 O11 -171.5(8) . . . . ?
Cr1 O9 C5 C6 5.0(11) . . . . ?
Cr1 O10 C6 O12 170.9(8) . . . . ?
Cr1 O10 C6 C5 -5.3(10) . . . . ?
O11 C5 C6 O12 0.6(15) . . . . ?
O9 C5 C6 O12 -176.1(9) . . . . ?
O11 C5 C6 O10 176.9(9) . . . . ?
O9 C5 C6 O10 0.2(12) . . . . ?
C8 C9 C10 C11 -74.3(12) . . . . ?
C16 N1 C11 C10 -57.3(12) . . . . ?
C14 N1 C11 C10 -178.2(9) . . . . ?
C12 N1 C11 C10 65.2(12) . . . . ?
C9 C10 C11 N1 -174.8(9) . . . . ?
C16 N1 C12 C13 -59.5(11) . . . . ?
C11 N1 C12 C13 174.3(8) . . . . ?
C14 N1 C12 C13 57.1(11) . . . . ?
C15 N2 C13 C12 -61.5(11) . . . . ?
C17 N2 C13 C12 56.6(11) . . . . ?
N1 C12 C13 N2 2.7(12) . . . . ?
C16 N1 C14 C15 56.1(11) . . . . ?
C11 N1 C14 C15 -179.2(9) . . . . ?
C12 N1 C14 C15 -60.4(11) . . . . ?
C13 N2 C15 C14 57.1(11) . . . . ?
C17 N2 C15 C14 -61.7(11) . . . . ?
N1 C14 C15 N2 3.7(13) . . . . ?
C11 N1 C16 C17 -179.7(8) . . . . ?
C14 N1 C16 C17 -59.0(11) . . . . ?
C12 N1 C16 C17 56.7(11) . . . . ?
C13 N2 C17 C16 -59.1(11) . . . . ?
C15 N2 C17 C16 59.3(11) . . . . ?
N1 C16 C17 N2 1.6(13) . . . . ?

_refine_diff_density_max         0.967
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.123

####################################################################### 
# 
# 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_Comp4_100K
_database_code_depnum_ccdc_archive 'CCDC 1496003'
_audit_update_record             
;
2016-08-31 deposited with the CCDC.
2016-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H6 Cr O14 Zn, C10 H21 N2'
_chemical_formula_sum            'C17 H27 Cr N2 O14 Zn'
_chemical_formula_weight         600.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   8.750(5)
_cell_length_b                   13.866(5)
_cell_length_c                   10.267(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 113.271(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     1144.3(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    738
_cell_measurement_theta_min      2.638
_cell_measurement_theta_max      23.425

_exptl_crystal_description       plates
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_F_000             618
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.599
_shelx_estimated_absorpt_T_min   0.646
_shelx_estimated_absorpt_T_max   0.924
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6456
_exptl_absorpt_correction_T_max  0.9243
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6408
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.159
_diffrn_reflns_theta_max         27.393
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.636
_diffrn_reflns_point_group_measured_fraction_full 0.669
_reflns_number_total             3316
_reflns_number_gt                2839
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.253
_reflns_Friedel_fraction_max     0.268
_reflns_Friedel_fraction_full    0.312

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0267P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 578 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.027(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3316
_refine_ls_number_parameters     324
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.0854
_refine_ls_wR_factor_gt          0.0794
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.004
_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
Cr1 Cr 0.03183(9) 0.26682(7) 0.20044(11) 0.0141(2) Uani 1 1 d . . . . .
Zn1 Zn 0.51394(6) 0.48502(5) 0.16482(7) 0.01484(18) Uani 1 1 d . . . . .
O1 O 0.1564(4) 0.3860(3) 0.2880(4) 0.0150(11) Uani 1 1 d . . . . .
O2 O 0.1701(4) 0.2715(4) 0.0888(4) 0.0157(9) Uani 1 1 d . . . . .
O3 O 0.3531(4) 0.4814(4) 0.2693(4) 0.0162(9) Uani 1 1 d . . . . .
O4 O 0.3582(4) 0.3672(3) 0.0567(5) 0.0167(11) Uani 1 1 d . . . . .
O5 O -0.1388(4) 0.3505(3) 0.0611(4) 0.0138(10) Uani 1 1 d . . . . .
O6 O -0.1143(4) 0.2817(3) 0.3055(4) 0.0163(10) Uani 1 1 d . . . . .
O7 O -0.3300(4) 0.4578(3) 0.0606(4) 0.0165(11) Uani 1 1 d . . . . .
O8 O -0.3289(4) 0.3711(3) 0.2990(5) 0.0160(11) Uani 1 1 d . . . . .
O9 O -0.0681(4) 0.1442(3) 0.1156(4) 0.0160(10) Uani 1 1 d . . . . .
O10 O 0.1867(4) 0.1846(3) 0.3472(5) 0.0160(11) Uani 1 1 d . . . . .
O11 O -0.0156(4) -0.0139(4) 0.1399(4) 0.0274(10) Uani 1 1 d . . . . .
O12 O 0.2320(4) 0.0300(3) 0.4099(4) 0.0222(11) Uani 1 1 d . . . . .
O13 O 0.6534(5) 0.5860(4) 0.3059(5) 0.0195(12) Uani 1 1 d D . . . .
H13C H 0.739(5) 0.602(5) 0.293(6) 0.029 Uiso 1 1 d D U . . .
H13D H 0.683(6) 0.569(6) 0.390(3) 0.029 Uiso 1 1 d D U . . .
O14 O 0.3936(4) 0.5905(3) 0.0211(5) 0.0212(12) Uani 1 1 d . . . . .
H14C H 0.2757 0.5882 -0.0244 0.025 Uiso 1 1 calc R U . . .
N1 N 0.7741(5) 0.2351(4) 0.6411(5) 0.0129(11) Uani 1 1 d . . . . .
N2 N 1.0568(5) 0.1513(4) 0.7028(5) 0.0175(12) Uani 1 1 d . . . . .
C1 C 0.2587(6) 0.4104(5) 0.2339(6) 0.0144(15) Uani 1 1 d . . . . .
C2 C 0.2651(6) 0.3449(5) 0.1159(6) 0.0133(14) Uani 1 1 d . . . . .
C3 C -0.2336(6) 0.3888(5) 0.1123(6) 0.0149(15) Uani 1 1 d . . . . .
C4 C -0.2273(6) 0.3441(5) 0.2508(6) 0.0134(14) Uani 1 1 d . . . . .
C5 C 0.0160(6) 0.0682(5) 0.1813(6) 0.0161(14) Uani 1 1 d . . . . .
C6 C 0.1593(6) 0.0924(5) 0.3270(7) 0.0160(14) Uani 1 1 d . . . . .
C7 C 0.4795(7) 0.6673(5) -0.0135(7) 0.0226(16) Uani 1 1 d . . . . .
H7 H 0.4805 0.7242 0.0436 0.034 Uiso 1 1 calc R U . . .
H7A H 0.4228 0.6831 -0.1143 0.034 Uiso 1 1 calc R U . . .
H7B H 0.5940 0.6474 0.0066 0.034 Uiso 1 1 calc R U . . .
C8 C 0.3779(7) 0.4681(5) 0.7319(7) 0.0295(19) Uani 1 1 d . . . . .
H8 H 0.3690 0.4277 0.8069 0.044 Uiso 1 1 calc R U . . .
H8A H 0.2711 0.5001 0.6797 0.044 Uiso 1 1 calc R U . . .
H8B H 0.4645 0.5169 0.7742 0.044 Uiso 1 1 calc R U . . .
C9 C 0.4225(6) 0.4060(5) 0.6318(7) 0.0243(17) Uani 1 1 d . . . . .
H9 H 0.4322 0.4475 0.5569 0.029 Uiso 1 1 calc R U . . .
H9A H 0.3311 0.3596 0.5853 0.029 Uiso 1 1 calc R U . . .
C10 C 0.5849(6) 0.3501(5) 0.7040(6) 0.0189(15) Uani 1 1 d . . . . .
H10 H 0.6799 0.3955 0.7398 0.023 Uiso 1 1 calc R U . . .
H10A H 0.5817 0.3132 0.7854 0.023 Uiso 1 1 calc R U . . .
C11 C 0.6061(6) 0.2819(5) 0.5970(6) 0.0187(15) Uani 1 1 d . . . . .
H11 H 0.5213 0.2304 0.5757 0.022 Uiso 1 1 calc R U . . .
H11A H 0.5831 0.3180 0.5081 0.022 Uiso 1 1 calc R U . . .
C12 C 0.9020(6) 0.3080(5) 0.6401(7) 0.0171(15) Uani 1 1 d . . . . .
H12 H 0.9049 0.3632 0.7022 0.021 Uiso 1 1 calc R U . . .
H12A H 0.8735 0.3325 0.5428 0.021 Uiso 1 1 calc R U . . .
C13 C 1.0734(6) 0.2571(5) 0.6947(7) 0.0197(15) Uani 1 1 d . . . . .
H13 H 1.1298 0.2720 0.6304 0.024 Uiso 1 1 calc R U . . .
H13A H 1.1434 0.2822 0.7900 0.024 Uiso 1 1 calc R U . . .
C14 C 0.7600(6) 0.1561(5) 0.5374(6) 0.0184(15) Uani 1 1 d . . . . .
H14 H 0.7081 0.1815 0.4394 0.022 Uiso 1 1 calc R U . . .
H14A H 0.6886 0.1038 0.5477 0.022 Uiso 1 1 calc R U . . .
C15 C 0.9341(6) 0.1165(5) 0.5651(6) 0.0202(15) Uani 1 1 d . . . . .
H15 H 0.9313 0.0451 0.5653 0.024 Uiso 1 1 calc R U . . .
H15A H 0.9679 0.1374 0.4882 0.024 Uiso 1 1 calc R U . . .
C16 C 0.8350(6) 0.1911(5) 0.7871(6) 0.0173(14) Uani 1 1 d . . . . .
H16 H 0.7468 0.1500 0.7957 0.021 Uiso 1 1 calc R U . . .
H16A H 0.8623 0.2426 0.8594 0.021 Uiso 1 1 calc R U . . .
C17 C 0.9909(6) 0.1298(5) 0.8117(6) 0.0169(15) Uani 1 1 d . . . . .
H17 H 1.0772 0.1437 0.9069 0.020 Uiso 1 1 calc R U . . .
H17A H 0.9623 0.0605 0.8078 0.020 Uiso 1 1 calc R U . . .


_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
Cr1 O10 1.948(4) . ?
Cr1 O9 1.953(4) . ?
Cr1 O2 1.969(4) . ?
Cr1 O6 1.982(4) . ?
Cr1 O5 1.984(4) . ?
Cr1 O1 1.988(4) . ?
Zn1 O13 2.037(5) . ?
Zn1 O14 2.049(4) . ?
Zn1 O7 2.075(4) 1_655 ?
Zn1 O3 2.080(4) . ?
Zn1 O4 2.136(4) . ?
Zn1 O8 2.188(4) 1_655 ?
O1 C1 1.271(7) . ?
O2 C2 1.274(8) . ?
O3 C1 1.244(8) . ?
O4 C2 1.232(7) . ?
O5 C3 1.261(7) . ?
O6 C4 1.266(7) . ?
O7 C3 1.247(7) . ?
O7 Zn1 2.075(4) 1_455 ?
O8 C4 1.234(7) . ?
O8 Zn1 2.188(4) 1_455 ?
O9 C5 1.309(7) . ?
O10 C6 1.302(8) . ?
O11 C5 1.208(8) . ?
O12 C6 1.204(7) . ?
O13 H13C 0.84(2) . ?
O13 H13D 0.83(2) . ?
O14 C7 1.426(7) . ?
O14 H14C 0.9500 . ?
N1 C14 1.497(8) . ?
N1 C11 1.503(6) . ?
N1 C16 1.508(8) . ?
N1 C12 1.511(7) . ?
N2 C17 1.477(8) . ?
N2 C15 1.478(7) . ?
N2 C13 1.479(8) . ?
C1 C2 1.533(8) . ?
C3 C4 1.532(8) . ?
C5 C6 1.563(7) . ?
C7 H7 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 C9 1.506(9) . ?
C8 H8 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 C10 1.529(8) . ?
C9 H9 0.9900 . ?
C9 H9A 0.9900 . ?
C10 C11 1.516(9) . ?
C10 H10 0.9900 . ?
C10 H10A 0.9900 . ?
C11 H11 0.9900 . ?
C11 H11A 0.9900 . ?
C12 C13 1.548(7) . ?
C12 H12 0.9900 . ?
C12 H12A 0.9900 . ?
C13 H13 0.9900 . ?
C13 H13A 0.9900 . ?
C14 C15 1.537(7) . ?
C14 H14 0.9900 . ?
C14 H14A 0.9900 . ?
C15 H15 0.9900 . ?
C15 H15A 0.9900 . ?
C16 C17 1.541(8) . ?
C16 H16 0.9900 . ?
C16 H16A 0.9900 . ?
C17 H17 0.9900 . ?
C17 H17A 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Cr1 O9 83.53(17) . . ?
O10 Cr1 O2 94.01(18) . . ?
O9 Cr1 O2 92.20(19) . . ?
O10 Cr1 O6 92.36(18) . . ?
O9 Cr1 O6 93.55(18) . . ?
O2 Cr1 O6 171.9(2) . . ?
O10 Cr1 O5 174.77(19) . . ?
O9 Cr1 O5 96.39(17) . . ?
O2 Cr1 O5 91.23(18) . . ?
O6 Cr1 O5 82.42(17) . . ?
O10 Cr1 O1 92.70(18) . . ?
O9 Cr1 O1 173.90(16) . . ?
O2 Cr1 O1 83.26(18) . . ?
O6 Cr1 O1 91.39(18) . . ?
O5 Cr1 O1 87.81(17) . . ?
O13 Zn1 O14 90.8(2) . . ?
O13 Zn1 O7 99.20(18) . 1_655 ?
O14 Zn1 O7 90.82(17) . 1_655 ?
O13 Zn1 O3 89.3(2) . . ?
O14 Zn1 O3 97.39(18) . . ?
O7 Zn1 O3 168.1(2) 1_655 . ?
O13 Zn1 O4 167.17(19) . . ?
O14 Zn1 O4 97.52(16) . . ?
O7 Zn1 O4 90.46(17) 1_655 . ?
O3 Zn1 O4 80.02(18) . . ?
O13 Zn1 O8 89.87(16) . 1_655 ?
O14 Zn1 O8 170.15(18) . 1_655 ?
O7 Zn1 O8 79.37(17) 1_655 1_655 ?
O3 Zn1 O8 92.44(17) . 1_655 ?
O4 Zn1 O8 83.59(17) . 1_655 ?
C1 O1 Cr1 112.3(4) . . ?
C2 O2 Cr1 113.4(4) . . ?
C1 O3 Zn1 112.0(4) . . ?
C2 O4 Zn1 110.3(4) . . ?
C3 O5 Cr1 112.2(4) . . ?
C4 O6 Cr1 112.9(4) . . ?
C3 O7 Zn1 113.1(4) . 1_455 ?
C4 O8 Zn1 109.8(4) . 1_455 ?
C5 O9 Cr1 114.2(3) . . ?
C6 O10 Cr1 115.0(4) . . ?
Zn1 O13 H13C 113(5) . . ?
Zn1 O13 H13D 113(5) . . ?
H13C O13 H13D 108(4) . . ?
C7 O14 Zn1 122.7(3) . . ?
C7 O14 H14C 118.6 . . ?
Zn1 O14 H14C 118.6 . . ?
C14 N1 C11 107.8(4) . . ?
C14 N1 C16 108.0(5) . . ?
C11 N1 C16 113.2(5) . . ?
C14 N1 C12 109.7(5) . . ?
C11 N1 C12 110.3(5) . . ?
C16 N1 C12 107.8(4) . . ?
C17 N2 C15 107.7(5) . . ?
C17 N2 C13 108.6(5) . . ?
C15 N2 C13 108.7(5) . . ?
O3 C1 O1 125.8(6) . . ?
O3 C1 C2 118.2(5) . . ?
O1 C1 C2 116.1(5) . . ?
O4 C2 O2 126.5(6) . . ?
O4 C2 C1 118.6(5) . . ?
O2 C2 C1 114.9(5) . . ?
O7 C3 O5 126.3(6) . . ?
O7 C3 C4 118.4(5) . . ?
O5 C3 C4 115.3(5) . . ?
O8 C4 O6 126.1(6) . . ?
O8 C4 C3 118.8(5) . . ?
O6 C4 C3 115.1(5) . . ?
O11 C5 O9 125.0(5) . . ?
O11 C5 C6 121.7(6) . . ?
O9 C5 C6 113.3(5) . . ?
O12 C6 O10 125.4(5) . . ?
O12 C6 C5 121.5(6) . . ?
O10 C6 C5 113.1(5) . . ?
O14 C7 H7 109.5 . . ?
O14 C7 H7A 109.5 . . ?
H7 C7 H7A 109.5 . . ?
O14 C7 H7B 109.5 . . ?
H7 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C9 C8 H8 109.5 . . ?
C9 C8 H8A 109.5 . . ?
H8 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C8 C9 C10 113.6(5) . . ?
C8 C9 H9 108.8 . . ?
C10 C9 H9 108.8 . . ?
C8 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
H9 C9 H9A 107.7 . . ?
C11 C10 C9 108.8(5) . . ?
C11 C10 H10 109.9 . . ?
C9 C10 H10 109.9 . . ?
C11 C10 H10A 109.9 . . ?
C9 C10 H10A 109.9 . . ?
H10 C10 H10A 108.3 . . ?
N1 C11 C10 115.9(4) . . ?
N1 C11 H11 108.3 . . ?
C10 C11 H11 108.3 . . ?
N1 C11 H11A 108.3 . . ?
C10 C11 H11A 108.3 . . ?
H11 C11 H11A 107.4 . . ?
N1 C12 C13 107.8(5) . . ?
N1 C12 H12 110.1 . . ?
C13 C12 H12 110.1 . . ?
N1 C12 H12A 110.1 . . ?
C13 C12 H12A 110.1 . . ?
H12 C12 H12A 108.5 . . ?
N2 C13 C12 111.7(4) . . ?
N2 C13 H13 109.3 . . ?
C12 C13 H13 109.3 . . ?
N2 C13 H13A 109.3 . . ?
C12 C13 H13A 109.3 . . ?
H13 C13 H13A 107.9 . . ?
N1 C14 C15 109.4(4) . . ?
N1 C14 H14 109.8 . . ?
C15 C14 H14 109.8 . . ?
N1 C14 H14A 109.8 . . ?
C15 C14 H14A 109.8 . . ?
H14 C14 H14A 108.2 . . ?
N2 C15 C14 110.7(5) . . ?
N2 C15 H15 109.5 . . ?
C14 C15 H15 109.5 . . ?
N2 C15 H15A 109.5 . . ?
C14 C15 H15A 109.5 . . ?
H15 C15 H15A 108.1 . . ?
N1 C16 C17 109.2(5) . . ?
N1 C16 H16 109.8 . . ?
C17 C16 H16 109.8 . . ?
N1 C16 H16A 109.8 . . ?
C17 C16 H16A 109.8 . . ?
H16 C16 H16A 108.3 . . ?
N2 C17 C16 110.5(5) . . ?
N2 C17 H17 109.6 . . ?
C16 C17 H17 109.6 . . ?
N2 C17 H17A 109.6 . . ?
C16 C17 H17A 109.6 . . ?
H17 C17 H17A 108.1 . . ?

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
Zn1 O3 C1 O1 174.5(4) . . . . ?
Zn1 O3 C1 C2 -4.9(6) . . . . ?
Cr1 O1 C1 O3 -179.5(5) . . . . ?
Cr1 O1 C1 C2 0.0(5) . . . . ?
Zn1 O4 C2 O2 -171.7(5) . . . . ?
Zn1 O4 C2 C1 8.7(6) . . . . ?
Cr1 O2 C2 O4 -176.5(5) . . . . ?
Cr1 O2 C2 C1 3.1(6) . . . . ?
O3 C1 C2 O4 -3.0(7) . . . . ?
O1 C1 C2 O4 177.6(5) . . . . ?
O3 C1 C2 O2 177.4(5) . . . . ?
O1 C1 C2 O2 -2.1(7) . . . . ?
Zn1 O7 C3 O5 172.0(5) 1_455 . . . ?
Zn1 O7 C3 C4 -7.6(6) 1_455 . . . ?
Cr1 O5 C3 O7 165.4(5) . . . . ?
Cr1 O5 C3 C4 -15.0(6) . . . . ?
Zn1 O8 C4 O6 177.3(5) 1_455 . . . ?
Zn1 O8 C4 C3 -2.4(6) 1_455 . . . ?
Cr1 O6 C4 O8 -175.8(5) . . . . ?
Cr1 O6 C4 C3 3.9(6) . . . . ?
O7 C3 C4 O8 7.1(8) . . . . ?
O5 C3 C4 O8 -172.5(5) . . . . ?
O7 C3 C4 O6 -172.6(5) . . . . ?
O5 C3 C4 O6 7.8(7) . . . . ?
Cr1 O9 C5 O11 -173.3(5) . . . . ?
Cr1 O9 C5 C6 10.2(6) . . . . ?
Cr1 O10 C6 O12 -173.9(5) . . . . ?
Cr1 O10 C6 C5 5.1(6) . . . . ?
O11 C5 C6 O12 -7.9(9) . . . . ?
O9 C5 C6 O12 168.8(5) . . . . ?
O11 C5 C6 O10 173.1(6) . . . . ?
O9 C5 C6 O10 -10.2(7) . . . . ?
C8 C9 C10 C11 173.4(6) . . . . ?
C14 N1 C11 C10 168.3(5) . . . . ?
C16 N1 C11 C10 49.0(7) . . . . ?
C12 N1 C11 C10 -71.9(7) . . . . ?
C9 C10 C11 N1 168.6(5) . . . . ?
C14 N1 C12 C13 -64.7(6) . . . . ?
C11 N1 C12 C13 176.7(5) . . . . ?
C16 N1 C12 C13 52.7(7) . . . . ?
C17 N2 C13 C12 -65.6(6) . . . . ?
C15 N2 C13 C12 51.3(7) . . . . ?
N1 C12 C13 N2 11.6(7) . . . . ?
C11 N1 C14 C15 171.6(5) . . . . ?
C16 N1 C14 C15 -65.9(6) . . . . ?
C12 N1 C14 C15 51.4(6) . . . . ?
C17 N2 C15 C14 51.9(7) . . . . ?
C13 N2 C15 C14 -65.6(7) . . . . ?
N1 C14 C15 N2 12.8(7) . . . . ?
C14 N1 C16 C17 50.7(5) . . . . ?
C11 N1 C16 C17 169.9(5) . . . . ?
C12 N1 C16 C17 -67.8(6) . . . . ?
C15 N2 C17 C16 -67.3(6) . . . . ?
C13 N2 C17 C16 50.3(6) . . . . ?
N1 C16 C17 N2 13.9(7) . . . . ?

_refine_diff_density_max         0.913
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.104

####################################################################### 
# 
# 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_Comp4_130K
_database_code_depnum_ccdc_archive 'CCDC 1496004'
_audit_update_record             
;
2016-08-31 deposited with the CCDC.
2016-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H6 Cr O14 Zn, C10 H21 N2'
_chemical_formula_sum            'C17 H27 Cr N2 O14 Zn'
_chemical_formula_weight         600.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   9.039(5)
_cell_length_b                   13.961(7)
_cell_length_c                   10.216(6)
_cell_angle_alpha                90
_cell_angle_beta                 114.888(9)
_cell_angle_gamma                90
_cell_volume                     1169.5(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    738
_cell_measurement_theta_min      2.638
_cell_measurement_theta_max      23.425

_exptl_crystal_description       plates
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_F_000             618
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.564
_shelx_estimated_absorpt_T_min   0.651
_shelx_estimated_absorpt_T_max   0.926
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6512
_exptl_absorpt_correction_T_max  0.9259
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6406
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.198
_diffrn_reflns_theta_max         25.564
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.683
_diffrn_reflns_point_group_measured_fraction_full 0.687
_reflns_number_total             2984
_reflns_number_gt                2580
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.313
_reflns_Friedel_fraction_max     0.340
_reflns_Friedel_fraction_full    0.347

_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0366P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.03(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2984
_refine_ls_number_parameters     324
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_ref         0.0917
_refine_ls_wR_factor_gt          0.0884
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_restrained_S_all      0.990
_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
Cr1 Cr 0.08064(15) 0.05175(9) 0.22452(13) 0.0210(3) Uani 1 1 d . . . . .
Zn1 Zn 0.54863(10) 0.25185(6) 0.16200(9) 0.0225(2) Uani 1 1 d . . . . .
O1 O 0.2261(6) 0.1606(4) 0.3174(6) 0.0226(14) Uani 1 1 d . . . . .
O2 O 0.2063(6) 0.0467(4) 0.1054(5) 0.0227(12) Uani 1 1 d . . . . .
O3 O 0.4132(6) 0.2514(6) 0.2858(5) 0.0265(13) Uani 1 1 d . . . . .
O4 O 0.3922(7) 0.1338(4) 0.0668(6) 0.0245(14) Uani 1 1 d . . . . .
O5 O -0.0767(7) 0.1423(4) 0.0868(5) 0.0226(13) Uani 1 1 d . . . . .
O6 O -0.0553(6) 0.0717(5) 0.3330(5) 0.0244(16) Uani 1 1 d . . . . .
O7 O -0.2951(6) 0.2294(4) 0.0630(5) 0.0228(14) Uani 1 1 d . . . . .
O8 O -0.2845(7) 0.1464(5) 0.3075(7) 0.0242(15) Uani 1 1 d . . . . .
O9 O -0.0495(6) -0.0594(4) 0.1302(6) 0.0246(14) Uani 1 1 d . . . . .
O10 O 0.2154(7) -0.0427(4) 0.3668(6) 0.0225(14) Uani 1 1 d . . . . .
O11 O -0.0825(6) -0.2115(4) 0.1746(6) 0.0345(15) Uani 1 1 d . . . . .
O12 O 0.2047(7) -0.1934(4) 0.4313(5) 0.0327(15) Uani 1 1 d . . . . .
O13 O 0.6810(7) 0.3601(5) 0.2863(6) 0.0273(16) Uani 1 1 d D . . . .
H13C H 0.767(6) 0.374(6) 0.279(8) 0.041 Uiso 1 1 d D U . . .
H13D H 0.699(8) 0.340(6) 0.367(4) 0.041 Uiso 1 1 d D U . . .
O14 O 0.3980(7) 0.3376(4) 0.0013(6) 0.0342(16) Uani 1 1 d . . . . .
H14C H 0.2881 0.3172 -0.0487 0.041 Uiso 1 1 calc R U . . .
N1 N 0.7674(8) 0.0220(5) 0.6588(6) 0.0248(17) Uani 1 1 d . . . . .
N2 N 1.0206(8) -0.0822(5) 0.7053(7) 0.0305(18) Uani 1 1 d . . . . .
C1 C 0.3183(9) 0.1839(6) 0.2561(8) 0.0201(19) Uani 1 1 d . . . . .
C2 C 0.3063(9) 0.1158(6) 0.1311(8) 0.0219(19) Uani 1 1 d . . . . .
C3 C -0.1849(9) 0.1708(6) 0.1261(8) 0.0210(19) Uani 1 1 d . . . . .
C4 C -0.1743(9) 0.1271(6) 0.2690(8) 0.0199(18) Uani 1 1 d . . . . .
C5 C -0.0078(9) -0.1373(6) 0.2026(8) 0.0218(18) Uani 1 1 d . . . . .
C6 C 0.1517(9) -0.1259(6) 0.3469(8) 0.0237(19) Uani 1 1 d . . . . .
C7 C 0.4414(11) 0.4250(6) -0.0433(9) 0.038(2) Uani 1 1 d . . . . .
H7 H 0.4037 0.4787 -0.0034 0.057 Uiso 1 1 calc R U . . .
H7A H 0.3903 0.4286 -0.1489 0.057 Uiso 1 1 calc R U . . .
H7B H 0.5602 0.4283 -0.0085 0.057 Uiso 1 1 calc R U . . .
C8 C 0.3458(13) 0.1760(8) 0.6859(10) 0.059(3) Uani 1 1 d . . . . .
H8 H 0.3115 0.1281 0.6086 0.088 Uiso 1 1 calc R U . . .
H8A H 0.2566 0.2213 0.6680 0.088 Uiso 1 1 calc R U . . .
H8B H 0.3740 0.1439 0.7787 0.088 Uiso 1 1 calc R U . . .
C9 C 0.4886(10) 0.2277(8) 0.6896(9) 0.046(3) Uani 1 1 d . . . . .
H9 H 0.5142 0.2826 0.7570 0.055 Uiso 1 1 calc R U . . .
H9A H 0.4667 0.2525 0.5924 0.055 Uiso 1 1 calc R U . . .
C10 C 0.6364(12) 0.1552(8) 0.7415(9) 0.055(3) Uani 1 1 d . . . . .
H10 H 0.7394 0.1913 0.7690 0.066 Uiso 1 1 calc R U . . .
H10A H 0.6418 0.1204 0.8278 0.066 Uiso 1 1 calc R U . . .
C11 C 0.6191(10) 0.0829(7) 0.6230(9) 0.039(2) Uani 1 1 d . . . . .
H11 H 0.5246 0.0408 0.6060 0.047 Uiso 1 1 calc R U . . .
H11A H 0.5961 0.1181 0.5324 0.047 Uiso 1 1 calc R U . . .
C12 C 0.9126(10) 0.0826(6) 0.6761(10) 0.041(2) Uani 1 1 d . . . . .
H12 H 0.9395 0.1266 0.7590 0.049 Uiso 1 1 calc R U . . .
H12A H 0.8862 0.1217 0.5883 0.049 Uiso 1 1 calc R U . . .
C13 C 1.0585(10) 0.0185(6) 0.7011(9) 0.036(2) Uani 1 1 d . . . . .
H13 H 1.0940 0.0291 0.6229 0.043 Uiso 1 1 calc R U . . .
H13A H 1.1500 0.0364 0.7935 0.043 Uiso 1 1 calc R U . . .
C14 C 0.8129(11) -0.0356(7) 0.7923(9) 0.037(2) Uani 1 1 d . . . . .
H14 H 0.7211 -0.0779 0.7826 0.045 Uiso 1 1 calc R U . . .
H14A H 0.8354 0.0077 0.8753 0.045 Uiso 1 1 calc R U . . .
C15 C 0.9631(10) -0.0957(6) 0.8195(8) 0.029(2) Uani 1 1 d . . . . .
H15 H 1.0513 -0.0778 0.9138 0.035 Uiso 1 1 calc R U . . .
H15A H 0.9370 -0.1642 0.8240 0.035 Uiso 1 1 calc R U . . .
C16 C 0.7359(10) -0.0456(6) 0.5360(9) 0.034(2) Uani 1 1 d . . . . .
H16 H 0.7085 -0.0087 0.4461 0.041 Uiso 1 1 calc R U . . .
H16A H 0.6417 -0.0871 0.5225 0.041 Uiso 1 1 calc R U . . .
C17 C 0.8844(10) -0.1073(7) 0.5654(8) 0.037(2) Uani 1 1 d . . . . .
H17 H 0.8554 -0.1756 0.5667 0.044 Uiso 1 1 calc R U . . .
H17A H 0.9199 -0.0986 0.4868 0.044 Uiso 1 1 calc R U . . .


_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
Cr1 O9 1.941(6) . ?
Cr1 O10 1.960(6) . ?
Cr1 O1 1.971(5) . ?
Cr1 O5 1.978(5) . ?
Cr1 O2 1.985(5) . ?
Cr1 O6 1.991(5) . ?
Zn1 O13 2.012(6) . ?
Zn1 O14 2.025(6) . ?
Zn1 O7 2.078(5) 1_655 ?
Zn1 O3 2.098(5) . ?
Zn1 O4 2.123(6) . ?
Zn1 O8 2.183(6) 1_655 ?
O1 C1 1.277(9) . ?
O2 C2 1.272(10) . ?
O3 C1 1.224(10) . ?
O4 C2 1.235(9) . ?
O5 C3 1.268(9) . ?
O6 C4 1.262(9) . ?
O7 C3 1.240(8) . ?
O7 Zn1 2.078(5) 1_455 ?
O8 C4 1.245(9) . ?
O8 Zn1 2.183(6) 1_455 ?
O9 C5 1.279(9) . ?
O10 C6 1.274(9) . ?
O11 C5 1.204(9) . ?
O12 C6 1.231(9) . ?
O13 H13C 0.83(2) . ?
O13 H13D 0.82(2) . ?
O14 C7 1.415(10) . ?
O14 H14C 0.9500 . ?
N1 C14 1.485(10) . ?
N1 C11 1.498(10) . ?
N1 C16 1.498(10) . ?
N1 C12 1.508(10) . ?
N2 C13 1.452(11) . ?
N2 C15 1.476(9) . ?
N2 C17 1.483(10) . ?
C1 C2 1.559(10) . ?
C3 C4 1.547(9) . ?
C5 C6 1.577(10) . ?
C7 H7 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 C9 1.465(12) . ?
C8 H8 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 C10 1.579(12) . ?
C9 H9 0.9900 . ?
C9 H9A 0.9900 . ?
C10 C11 1.533(12) . ?
C10 H10 0.9900 . ?
C10 H10A 0.9900 . ?
C11 H11 0.9900 . ?
C11 H11A 0.9900 . ?
C12 C13 1.524(12) . ?
C12 H12 0.9900 . ?
C12 H12A 0.9900 . ?
C13 H13 0.9900 . ?
C13 H13A 0.9900 . ?
C14 C15 1.519(11) . ?
C14 H14 0.9900 . ?
C14 H14A 0.9900 . ?
C15 H15 0.9900 . ?
C15 H15A 0.9900 . ?
C16 C17 1.515(11) . ?
C16 H16 0.9900 . ?
C16 H16A 0.9900 . ?
C17 H17 0.9900 . ?
C17 H17A 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 Cr1 O10 83.6(2) . . ?
O9 Cr1 O1 175.7(2) . . ?
O10 Cr1 O1 94.6(2) . . ?
O9 Cr1 O5 93.1(2) . . ?
O10 Cr1 O5 173.2(3) . . ?
O1 Cr1 O5 89.1(2) . . ?
O9 Cr1 O2 92.9(2) . . ?
O10 Cr1 O2 95.4(2) . . ?
O1 Cr1 O2 83.4(2) . . ?
O5 Cr1 O2 90.7(2) . . ?
O9 Cr1 O6 90.1(2) . . ?
O10 Cr1 O6 91.0(2) . . ?
O1 Cr1 O6 93.9(2) . . ?
O5 Cr1 O6 83.1(2) . . ?
O2 Cr1 O6 173.2(3) . . ?
O13 Zn1 O14 94.9(3) . . ?
O13 Zn1 O7 94.3(2) . 1_655 ?
O14 Zn1 O7 93.3(2) . 1_655 ?
O13 Zn1 O3 88.0(3) . . ?
O14 Zn1 O3 97.3(2) . . ?
O7 Zn1 O3 169.0(2) 1_655 . ?
O13 Zn1 O4 167.7(2) . . ?
O14 Zn1 O4 89.8(2) . . ?
O7 Zn1 O4 96.8(2) 1_655 . ?
O3 Zn1 O4 80.1(2) . . ?
O13 Zn1 O8 91.1(2) . 1_655 ?
O14 Zn1 O8 170.7(3) . 1_655 ?
O7 Zn1 O8 79.3(2) 1_655 1_655 ?
O3 Zn1 O8 89.9(2) . 1_655 ?
O4 Zn1 O8 85.7(2) . 1_655 ?
C1 O1 Cr1 113.7(5) . . ?
C2 O2 Cr1 112.8(5) . . ?
C1 O3 Zn1 112.3(5) . . ?
C2 O4 Zn1 111.1(5) . . ?
C3 O5 Cr1 113.2(5) . . ?
C4 O6 Cr1 112.8(5) . . ?
C3 O7 Zn1 114.1(5) . 1_455 ?
C4 O8 Zn1 110.2(5) . 1_455 ?
C5 O9 Cr1 115.0(5) . . ?
C6 O10 Cr1 113.4(5) . . ?
Zn1 O13 H13C 116(6) . . ?
Zn1 O13 H13D 101(6) . . ?
H13C O13 H13D 112(5) . . ?
C7 O14 Zn1 126.0(5) . . ?
C7 O14 H14C 117.0 . . ?
Zn1 O14 H14C 117.0 . . ?
C14 N1 C11 113.9(7) . . ?
C14 N1 C16 108.0(7) . . ?
C11 N1 C16 108.6(6) . . ?
C14 N1 C12 107.8(6) . . ?
C11 N1 C12 110.8(7) . . ?
C16 N1 C12 107.6(7) . . ?
C13 N2 C15 108.3(7) . . ?
C13 N2 C17 108.1(7) . . ?
C15 N2 C17 107.8(7) . . ?
O3 C1 O1 127.5(7) . . ?
O3 C1 C2 118.2(7) . . ?
O1 C1 C2 114.3(6) . . ?
O4 C2 O2 126.5(8) . . ?
O4 C2 C1 118.0(7) . . ?
O2 C2 C1 115.5(6) . . ?
O7 C3 O5 126.9(8) . . ?
O7 C3 C4 117.9(7) . . ?
O5 C3 C4 115.2(6) . . ?
O8 C4 O6 126.1(8) . . ?
O8 C4 C3 118.3(7) . . ?
O6 C4 C3 115.6(6) . . ?
O11 C5 O9 126.5(7) . . ?
O11 C5 C6 120.7(7) . . ?
O9 C5 C6 112.7(7) . . ?
O12 C6 O10 124.8(7) . . ?
O12 C6 C5 120.7(7) . . ?
O10 C6 C5 114.5(7) . . ?
O14 C7 H7 109.5 . . ?
O14 C7 H7A 109.5 . . ?
H7 C7 H7A 109.5 . . ?
O14 C7 H7B 109.5 . . ?
H7 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C9 C8 H8 109.5 . . ?
C9 C8 H8A 109.5 . . ?
H8 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C8 C9 C10 107.7(9) . . ?
C8 C9 H9 110.2 . . ?
C10 C9 H9 110.2 . . ?
C8 C9 H9A 110.2 . . ?
C10 C9 H9A 110.2 . . ?
H9 C9 H9A 108.5 . . ?
C11 C10 C9 111.5(7) . . ?
C11 C10 H10 109.3 . . ?
C9 C10 H10 109.3 . . ?
C11 C10 H10A 109.3 . . ?
C9 C10 H10A 109.3 . . ?
H10 C10 H10A 108.0 . . ?
N1 C11 C10 113.5(7) . . ?
N1 C11 H11 108.9 . . ?
C10 C11 H11 108.9 . . ?
N1 C11 H11A 108.9 . . ?
C10 C11 H11A 108.9 . . ?
H11 C11 H11A 107.7 . . ?
N1 C12 C13 109.8(7) . . ?
N1 C12 H12 109.7 . . ?
C13 C12 H12 109.7 . . ?
N1 C12 H12A 109.7 . . ?
C13 C12 H12A 109.7 . . ?
H12 C12 H12A 108.2 . . ?
N2 C13 C12 112.0(7) . . ?
N2 C13 H13 109.2 . . ?
C12 C13 H13 109.2 . . ?
N2 C13 H13A 109.2 . . ?
C12 C13 H13A 109.2 . . ?
H13 C13 H13A 107.9 . . ?
N1 C14 C15 110.4(7) . . ?
N1 C14 H14 109.6 . . ?
C15 C14 H14 109.6 . . ?
N1 C14 H14A 109.6 . . ?
C15 C14 H14A 109.6 . . ?
H14 C14 H14A 108.1 . . ?
N2 C15 C14 111.7(7) . . ?
N2 C15 H15 109.3 . . ?
C14 C15 H15 109.3 . . ?
N2 C15 H15A 109.3 . . ?
C14 C15 H15A 109.3 . . ?
H15 C15 H15A 107.9 . . ?
N1 C16 C17 110.6(6) . . ?
N1 C16 H16 109.5 . . ?
C17 C16 H16 109.5 . . ?
N1 C16 H16A 109.5 . . ?
C17 C16 H16A 109.5 . . ?
H16 C16 H16A 108.1 . . ?
N2 C17 C16 111.3(7) . . ?
N2 C17 H17 109.4 . . ?
C16 C17 H17 109.4 . . ?
N2 C17 H17A 109.4 . . ?
C16 C17 H17A 109.4 . . ?
H17 C17 H17A 108.0 . . ?

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
Zn1 O3 C1 O1 175.7(6) . . . . ?
Zn1 O3 C1 C2 -3.4(8) . . . . ?
Cr1 O1 C1 O3 175.7(7) . . . . ?
Cr1 O1 C1 C2 -5.2(7) . . . . ?
Zn1 O4 C2 O2 -176.2(6) . . . . ?
Zn1 O4 C2 C1 4.2(7) . . . . ?
Cr1 O2 C2 O4 -175.2(6) . . . . ?
Cr1 O2 C2 C1 4.4(7) . . . . ?
O3 C1 C2 O4 -0.7(9) . . . . ?
O1 C1 C2 O4 -179.9(7) . . . . ?
O3 C1 C2 O2 179.7(8) . . . . ?
O1 C1 C2 O2 0.5(8) . . . . ?
Zn1 O7 C3 O5 177.9(6) 1_455 . . . ?
Zn1 O7 C3 C4 -2.6(7) 1_455 . . . ?
Cr1 O5 C3 O7 177.8(6) . . . . ?
Cr1 O5 C3 C4 -1.7(7) . . . . ?
Zn1 O8 C4 O6 177.2(7) 1_455 . . . ?
Zn1 O8 C4 C3 -5.7(8) 1_455 . . . ?
Cr1 O6 C4 O8 174.6(7) . . . . ?
Cr1 O6 C4 C3 -2.7(8) . . . . ?
O7 C3 C4 O8 6.1(10) . . . . ?
O5 C3 C4 O8 -174.4(8) . . . . ?
O7 C3 C4 O6 -176.5(8) . . . . ?
O5 C3 C4 O6 3.0(9) . . . . ?
Cr1 O9 C5 O11 169.9(7) . . . . ?
Cr1 O9 C5 C6 -5.4(8) . . . . ?
Cr1 O10 C6 O12 -171.4(6) . . . . ?
Cr1 O10 C6 C5 7.6(8) . . . . ?
O11 C5 C6 O12 1.9(11) . . . . ?
O9 C5 C6 O12 177.4(7) . . . . ?
O11 C5 C6 O10 -177.1(7) . . . . ?
O9 C5 C6 O10 -1.6(9) . . . . ?
C8 C9 C10 C11 73.5(10) . . . . ?
C14 N1 C11 C10 59.4(10) . . . . ?
C16 N1 C11 C10 179.8(8) . . . . ?
C12 N1 C11 C10 -62.3(10) . . . . ?
C9 C10 C11 N1 171.5(8) . . . . ?
C14 N1 C12 C13 59.1(9) . . . . ?
C11 N1 C12 C13 -175.7(7) . . . . ?
C16 N1 C12 C13 -57.2(9) . . . . ?
C15 N2 C13 C12 -57.1(9) . . . . ?
C17 N2 C13 C12 59.4(9) . . . . ?
N1 C12 C13 N2 -1.5(10) . . . . ?
C11 N1 C14 C15 179.4(7) . . . . ?
C16 N1 C14 C15 58.7(9) . . . . ?
C12 N1 C14 C15 -57.2(9) . . . . ?
C13 N2 C15 C14 59.1(9) . . . . ?
C17 N2 C15 C14 -57.6(9) . . . . ?
N1 C14 C15 N2 -1.1(10) . . . . ?
C14 N1 C16 C17 -57.5(9) . . . . ?
C11 N1 C16 C17 178.6(8) . . . . ?
C12 N1 C16 C17 58.6(9) . . . . ?
C13 N2 C17 C16 -58.0(9) . . . . ?
C15 N2 C17 C16 58.8(10) . . . . ?
N1 C16 C17 N2 -1.3(11) . . . . ?

_refine_diff_density_max         0.622
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.085

