# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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 2159912'
loop_
_audit_author_name
_audit_author_address
'Lidija Andros Dubraja'
;Rudjer Boskovic Institute
Croatia
;
_audit_update_record             
;
2022-03-18 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            (H2-DABCO)[Cr(bpy)(ox)2]2
_chemical_formula_moiety         '2(C14 H8 Cr1 N2 O8), C6 H14 N2'
_chemical_formula_sum            'C34 H30 Cr2 N6 O16'
_chemical_formula_weight         882.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   16.1971(14)
_cell_length_b                   16.7689(19)
_cell_length_c                   13.7996(11)
_cell_angle_alpha                90
_cell_angle_beta                 103.514(9)
_cell_angle_gamma                90
_cell_volume                     3644.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1034
_cell_measurement_theta_min      3.8260
_cell_measurement_theta_max      71.3820

_exptl_crystal_description       stick
_exptl_crystal_colour            reddish
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_F_000             1808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    5.661
_exptl_absorpt_correction_T_min  0.14514
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.250
_oxdiff_exptl_absorpt_empirical_full_max 3.544
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Ruby
_diffrn_detector_area_resol_mean 10.4323
_diffrn_reflns_number            18998
_diffrn_reflns_av_unetI/netI     0.2325
_diffrn_reflns_av_R_equivalents  0.2831
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.851
_diffrn_reflns_theta_max         76.642
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             7401
_reflns_number_gt                2892
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SIR-2019 (Burla, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Mercury (2020)'
_computing_publication_material  'PLATON (Spek, 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0763P)²+167.9174P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7401
_refine_ls_number_parameters     320
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.3426
_refine_ls_R_factor_gt           0.2198
_refine_ls_wR_factor_ref         0.5008
_refine_ls_wR_factor_gt          0.4339
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.036
_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
N1 N 0.4174(6) 0.2098(7) 0.7006(8) 0.033(3) Uiso 1 1 d G U . . .
C1 C 0.4279(6) 0.2917(7) 0.6944(9) 0.056(6) Uiso 1 1 d G U . . .
H1 H 0.481128 0.314453 0.718088 0.067 Uiso 1 1 calc R U . . .
C2 C 0.3587(8) 0.3397(5) 0.6527(11) 0.055(6) Uiso 1 1 d G U . . .
H2 H 0.365712 0.394573 0.648533 0.066 Uiso 1 1 calc R U . . .
C3 C 0.2791(7) 0.3058(7) 0.6172(10) 0.049(5) Uiso 1 1 d G U . . .
H3 H 0.232814 0.337888 0.589362 0.059 Uiso 1 1 calc R U . . .
C4 C 0.2686(6) 0.2238(7) 0.6235(9) 0.044(5) Uiso 1 1 d G U . . .
H4 H 0.215330 0.201083 0.599741 0.053 Uiso 1 1 calc R U . . .
C5 C 0.3378(7) 0.1758(5) 0.6651(9) 0.043(5) Uiso 1 1 d G U . . .
N2 N 0.4135(7) 0.0573(8) 0.7238(9) 0.047(4) Uiso 1 1 d G U . . .
C6 C 0.3373(8) 0.0919(6) 0.6740(10) 0.040(4) Uiso 1 1 d G U . . .
C7 C 0.2682(7) 0.0440(9) 0.6322(10) 0.059(6) Uiso 1 1 d G U . . .
H7 H 0.217231 0.067070 0.598869 0.071 Uiso 1 1 calc R U . . .
C8 C 0.2751(8) -0.0385(8) 0.6401(11) 0.068(7) Uiso 1 1 d G U . . .
H8 H 0.228832 -0.070600 0.612162 0.081 Uiso 1 1 calc R U . . .
C9 C 0.3512(11) -0.0731(6) 0.6899(13) 0.082(8) Uiso 1 1 d G U . . .
H9 H 0.355891 -0.128275 0.695247 0.098 Uiso 1 1 calc R U . . .
C10 C 0.4204(8) -0.0252(8) 0.7317(11) 0.071(7) Uiso 1 1 d G U . . .
H10 H 0.471346 -0.048281 0.765042 0.085 Uiso 1 1 calc R U . . .
N3 N 0.2542(6) 0.1129(7) 0.3681(9) 0.049(4) Uiso 1 1 d G U . . .
C11 C 0.3012(8) 0.0427(6) 0.3841(10) 0.049(5) Uiso 1 1 d G U . . .
H11 H 0.274029 -0.006278 0.371213 0.059 Uiso 1 1 calc R U . . .
C12 C 0.3889(8) 0.0459(7) 0.4194(11) 0.061(6) Uiso 1 1 d G U . . .
H12 H 0.420319 -0.001024 0.430067 0.073 Uiso 1 1 calc R U . . .
C13 C 0.4295(6) 0.1192(8) 0.4386(10) 0.057(6) Uiso 1 1 d G U . . .
H13 H 0.488184 0.121267 0.462188 0.068 Uiso 1 1 calc R U . . .
C14 C 0.3826(7) 0.1893(6) 0.4226(9) 0.039(4) Uiso 1 1 d G U . . .
H14 H 0.409762 0.238304 0.435457 0.046 Uiso 1 1 calc R U . . .
C15 C 0.2949(7) 0.1861(6) 0.3873(9) 0.028(4) Uiso 1 1 d G U . . .
N4 N 0.1534(8) 0.2359(6) 0.3285(9) 0.045(4) Uiso 1 1 d G U . . .
C16 C 0.2393(7) 0.2514(7) 0.3652(9) 0.044(5) Uiso 1 1 d G U . . .
C17 C 0.2685(6) 0.3297(8) 0.3743(10) 0.044(5) Uiso 1 1 d G U . . .
H17 H 0.325949 0.340085 0.398881 0.053 Uiso 1 1 calc R U . . .
C18 C 0.2117(9) 0.3923(6) 0.3467(11) 0.058(6) Uiso 1 1 d G U . . .
H18 H 0.231154 0.444694 0.352839 0.069 Uiso 1 1 calc R U . . .
C19 C 0.1257(8) 0.3768(7) 0.3100(12) 0.067(7) Uiso 1 1 d G U . . .
H19 H 0.087746 0.418713 0.291547 0.080 Uiso 1 1 calc R U . . .
C20 C 0.0966(6) 0.2985(8) 0.3009(11) 0.071(7) Uiso 1 1 d G U . . .
H20 H 0.039132 0.288121 0.276297 0.086 Uiso 1 1 calc R U . . .
C21 C 0.6487(15) 0.2132(14) 0.7370(13) 0.049(6) Uani 1 1 d . . . . .
C22 C 0.6166(15) 0.1596(13) 0.6454(16) 0.052(6) Uani 1 1 d . . . . .
C23 C 0.5961(13) 0.0511(13) 0.9393(16) 0.046(5) Uiso 1 1 d . . . . .
C24 C 0.5361(16) 0.1111(16) 0.9709(19) 0.062(6) Uiso 1 1 d . . . . .
C25 C -0.0265(17) 0.1385(18) 0.3795(19) 0.072(8) Uani 1 1 d . . . . .
C26 C 0.0444(17) 0.1298(18) 0.4781(15) 0.070(8) Uani 1 1 d . . . . .
C27 C 0.1069(15) 0.0422(18) 0.1426(18) 0.067(8) Uani 1 1 d . . . . .
C28 C 0.1024(16) -0.0252(18) 0.2175(19) 0.068(7) Uani 1 1 d . . . . .
C29 C 0.9288(18) 0.1981(17) 1.046(2) 0.082(9) Uani 1 1 d . . . . .
H29A H 0.942117 0.229765 0.993119 0.099 Uiso 1 1 calc R U . . .
H29B H 0.981567 0.177393 1.086884 0.099 Uiso 1 1 calc R U . . .
C30 C 0.8850(16) 0.2509(18) 1.111(2) 0.080(9) Uani 1 1 d . . . . .
H30A H 0.913431 0.245885 1.180491 0.096 Uiso 1 1 calc R U . . .
H30B H 0.886633 0.306380 1.091367 0.096 Uiso 1 1 calc R U . . .
C31 C 0.8488(18) 0.0871(17) 1.085(2) 0.074(8) Uiso 1 1 d . . . . .
H31A H 0.898879 0.071053 1.134930 0.089 Uiso 1 1 calc R U . . .
H31B H 0.817640 0.039546 1.058475 0.089 Uiso 1 1 calc R U . . .
C32 C 0.793(2) 0.1404(16) 1.1325(19) 0.085(10) Uani 1 1 d . . . . .
H32A H 0.735198 0.121516 1.115379 0.102 Uiso 1 1 calc R U . . .
H32B H 0.813293 0.139427 1.204476 0.102 Uiso 1 1 calc R U . . .
C33 C 0.7972(18) 0.1597(17) 0.937(2) 0.076(8) Uiso 1 1 d . . . . .
H33A H 0.758271 0.115377 0.918553 0.091 Uiso 1 1 calc R U . . .
H33B H 0.810146 0.181046 0.877153 0.091 Uiso 1 1 calc R U . . .
C34 C 0.7557(17) 0.2242(16) 0.9879(19) 0.071(7) Uiso 1 1 d . . . . .
H34A H 0.762099 0.275919 0.959005 0.086 Uiso 1 1 calc R U . . .
H34B H 0.695573 0.213294 0.978948 0.086 Uiso 1 1 calc R U . . .
N5 N 0.8739(13) 0.1325(12) 1.0041(13) 0.057(5) Uani 1 1 d . . . . .
H5 H 0.904459 0.096984 0.968064 0.068 Uiso 1 1 calc R U . . .
N6 N 0.7979(11) 0.2238(11) 1.0943(13) 0.048(4) Uiso 1 1 d . . . . .
H6 H 0.767065 0.259526 1.129669 0.058 Uiso 1 1 calc R U . . .
O1 O 0.6004(9) 0.2151(9) 0.7997(9) 0.049(4) Uani 1 1 d . . . . .
O2 O 0.7156(9) 0.2527(10) 0.7476(11) 0.056(4) Uani 1 1 d . . . . .
O3 O 0.6609(12) 0.1554(10) 0.5845(12) 0.073(5) Uani 1 1 d . . . . .
O4 O 0.5504(10) 0.1190(9) 0.6489(9) 0.051(4) Uani 1 1 d . . . . .
O5 O 0.5912(8) 0.0540(9) 0.8451(8) 0.049(4) Uani 1 1 d . . . . .
O6 O 0.6488(12) 0.0157(11) 0.9995(11) 0.081(6) Uani 1 1 d . . . . .
O7 O 0.5386(14) 0.1223(14) 1.0621(13) 0.105(8) Uani 1 1 d . . . . .
O8 O 0.4847(9) 0.1483(9) 0.9005(9) 0.051(4) Uani 1 1 d . . . . .
O9 O 0.0051(9) 0.1319(9) 0.3014(10) 0.052(4) Uiso 1 1 d . . . . .
O10 O -0.1008(11) 0.1514(14) 0.3803(13) 0.089(6) Uani 1 1 d . . . . .
O11 O 0.0276(12) 0.1417(14) 0.5568(13) 0.092(6) Uani 1 1 d . . . . .
O12 O 0.1182(9) 0.1177(10) 0.4654(10) 0.054(4) Uani 1 1 d . . . . .
O13 O 0.1197(9) 0.1112(10) 0.1811(9) 0.054(4) Uani 1 1 d . . . . .
O14 O 0.1008(14) 0.0234(12) 0.0572(13) 0.091(6) Uani 1 1 d . . . . .
O15 O 0.0905(13) -0.0955(11) 0.1929(14) 0.082(6) Uani 1 1 d . . . . .
O16 O 0.1130(9) -0.0004(10) 0.3090(10) 0.059(4) Uani 1 1 d . . . . .
Cr1 Cr 0.5109(2) 0.1335(2) 0.7728(2) 0.0410(8) Uani 1 1 d . . . . .
Cr3 Cr 0.1250(2) 0.1153(2) 0.3253(2) 0.0486(10) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.3900 . ?
N1 C5 1.3900 . ?
N1 Cr1 2.054(9) . ?
C1 C2 1.3900 . ?
C1 H1 0.9300 . ?
C2 C3 1.3900 . ?
C2 H2 0.9300 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.413(13) . ?
N2 C6 1.3900 . ?
N2 C10 1.3900 . ?
N2 Cr1 2.021(11) . ?
C6 C7 1.3900 . ?
C7 C8 1.3900 . ?
C7 H7 0.9300 . ?
C8 C9 1.3900 . ?
C8 H8 0.9300 . ?
C9 C10 1.3900 . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
N3 C11 1.3900 . ?
N3 C15 1.3900 . ?
N3 Cr3 2.039(9) . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 H12 0.9300 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 C15 1.3900 . ?
C14 H14 0.9300 . ?
C15 C16 1.405(13) . ?
N4 C16 1.3900 . ?
N4 C20 1.3900 . ?
N4 Cr3 2.072(11) . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C17 H17 0.9300 . ?
C18 C19 1.3900 . ?
C18 H18 0.9300 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 O2 1.25(3) . ?
C21 O1 1.30(2) . ?
C21 C22 1.54(3) . ?
C22 O3 1.23(3) . ?
C22 O4 1.28(3) . ?
C23 O6 1.20(2) . ?
C23 O5 1.28(2) . ?
C23 C24 1.53(3) . ?
C24 O7 1.26(3) . ?
C24 O8 1.28(3) . ?
C25 O10 1.22(3) . ?
C25 O9 1.30(3) . ?
C25 C26 1.57(3) . ?
C26 O11 1.20(2) . ?
C26 O12 1.26(3) . ?
C27 O14 1.20(3) . ?
C27 O13 1.27(3) . ?
C27 C28 1.54(4) . ?
C28 O15 1.23(3) . ?
C28 O16 1.30(3) . ?
C29 N5 1.45(3) . ?
C29 C30 1.54(3) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 N6 1.45(3) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 N5 1.49(3) . ?
C31 C32 1.52(3) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 N6 1.50(3) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 N5 1.44(3) . ?
C33 C34 1.53(3) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 N6 1.47(3) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
N5 H5 0.9800 . ?
N6 H6 0.9800 . ?
O1 Cr1 1.964(16) . ?
O4 Cr1 1.974(13) . ?
O5 Cr1 1.964(13) . ?
O8 Cr1 1.924(13) . ?
O9 Cr3 1.912(14) . ?
O12 Cr3 1.961(14) . ?
O13 Cr3 1.973(13) . ?
O16 Cr3 1.958(18) . ?

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
C1 N1 C5 120.0 . . ?
C1 N1 Cr1 124.0(6) . . ?
C5 N1 Cr1 115.7(6) . . ?
C2 C1 N1 120.0 . . ?
C2 C1 H1 120.0 . . ?
N1 C1 H1 120.0 . . ?
C1 C2 C3 120.0 . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 N1 120.0 . . ?
C4 C5 C6 126.4(10) . . ?
N1 C5 C6 113.6(9) . . ?
C6 N2 C10 120.0 . . ?
C6 N2 Cr1 115.8(8) . . ?
C10 N2 Cr1 124.1(8) . . ?
N2 C6 C7 120.0 . . ?
N2 C6 C5 115.9(10) . . ?
C7 C6 C5 124.0(10) . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 C7 120.0 . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 120.0 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 N2 120.0 . . ?
C9 C10 H10 120.0 . . ?
N2 C10 H10 120.0 . . ?
C11 N3 C15 120.0 . . ?
C11 N3 Cr3 123.4(7) . . ?
C15 N3 Cr3 116.5(7) . . ?
N3 C11 C12 120.0 . . ?
N3 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 120.0 . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 N3 120.0 . . ?
C14 C15 C16 126.6(9) . . ?
N3 C15 C16 113.4(9) . . ?
C16 N4 C20 120.0 . . ?
C16 N4 Cr3 112.9(7) . . ?
C20 N4 Cr3 127.0(7) . . ?
C17 C16 N4 120.0 . . ?
C17 C16 C15 122.0(10) . . ?
N4 C16 C15 118.0(10) . . ?
C16 C17 C18 120.0 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C19 C20 N4 120.0 . . ?
C19 C20 H20 120.0 . . ?
N4 C20 H20 120.0 . . ?
O2 C21 O1 123(2) . . ?
O2 C21 C22 122(2) . . ?
O1 C21 C22 115(2) . . ?
O3 C22 O4 129(2) . . ?
O3 C22 C21 117(2) . . ?
O4 C22 C21 114(2) . . ?
O6 C23 O5 126(2) . . ?
O6 C23 C24 122(2) . . ?
O5 C23 C24 111.8(19) . . ?
O7 C24 O8 123(2) . . ?
O7 C24 C23 121(2) . . ?
O8 C24 C23 116(2) . . ?
O10 C25 O9 127(2) . . ?
O10 C25 C26 122(2) . . ?
O9 C25 C26 111(2) . . ?
O11 C26 O12 125(2) . . ?
O11 C26 C25 120(2) . . ?
O12 C26 C25 114.7(17) . . ?
O14 C27 O13 128(3) . . ?
O14 C27 C28 117(3) . . ?
O13 C27 C28 115(2) . . ?
O15 C28 O16 123(3) . . ?
O15 C28 C27 123(2) . . ?
O16 C28 C27 114(2) . . ?
N5 C29 C30 110(2) . . ?
N5 C29 H29A 109.6 . . ?
C30 C29 H29A 109.6 . . ?
N5 C29 H29B 109.6 . . ?
C30 C29 H29B 109.6 . . ?
H29A C29 H29B 108.1 . . ?
N6 C30 C29 107(2) . . ?
N6 C30 H30A 110.3 . . ?
C29 C30 H30A 110.3 . . ?
N6 C30 H30B 110.3 . . ?
C29 C30 H30B 110.3 . . ?
H30A C30 H30B 108.6 . . ?
N5 C31 C32 108(2) . . ?
N5 C31 H31A 110.0 . . ?
C32 C31 H31A 110.0 . . ?
N5 C31 H31B 110.0 . . ?
C32 C31 H31B 110.0 . . ?
H31A C31 H31B 108.4 . . ?
N6 C32 C31 108.4(19) . . ?
N6 C32 H32A 110.0 . . ?
C31 C32 H32A 110.0 . . ?
N6 C32 H32B 110.0 . . ?
C31 C32 H32B 110.0 . . ?
H32A C32 H32B 108.4 . . ?
N5 C33 C34 110(2) . . ?
N5 C33 H33A 109.7 . . ?
C34 C33 H33A 109.7 . . ?
N5 C33 H33B 109.7 . . ?
C34 C33 H33B 109.7 . . ?
H33A C33 H33B 108.2 . . ?
N6 C34 C33 108(2) . . ?
N6 C34 H34A 110.2 . . ?
C33 C34 H34A 110.2 . . ?
N6 C34 H34B 110.2 . . ?
C33 C34 H34B 110.2 . . ?
H34A C34 H34B 108.5 . . ?
C33 N5 C29 112(2) . . ?
C33 N5 C31 107(2) . . ?
C29 N5 C31 110(2) . . ?
C33 N5 H5 109.3 . . ?
C29 N5 H5 109.3 . . ?
C31 N5 H5 109.3 . . ?
C34 N6 C30 111(2) . . ?
C34 N6 C32 108(2) . . ?
C30 N6 C32 111(2) . . ?
C34 N6 H6 108.8 . . ?
C30 N6 H6 108.8 . . ?
C32 N6 H6 108.8 . . ?
C21 O1 Cr1 113.0(14) . . ?
C22 O4 Cr1 114.3(14) . . ?
C23 O5 Cr1 114.6(14) . . ?
C24 O8 Cr1 112.8(15) . . ?
C25 O9 Cr3 116.7(15) . . ?
C26 O12 Cr3 114.4(13) . . ?
C27 O13 Cr3 114.7(16) . . ?
C28 O16 Cr3 114.5(17) . . ?
O8 Cr1 O5 83.3(6) . . ?
O8 Cr1 O1 92.8(6) . . ?
O5 Cr1 O1 90.3(6) . . ?
O8 Cr1 O4 174.1(6) . . ?
O5 Cr1 O4 92.7(6) . . ?
O1 Cr1 O4 82.9(6) . . ?
O8 Cr1 N2 93.7(6) . . ?
O5 Cr1 N2 96.5(6) . . ?
O1 Cr1 N2 171.1(6) . . ?
O4 Cr1 N2 91.0(6) . . ?
O8 Cr1 N1 93.9(5) . . ?
O5 Cr1 N1 174.2(6) . . ?
O1 Cr1 N1 94.9(5) . . ?
O4 Cr1 N1 90.5(5) . . ?
N2 Cr1 N1 78.5(5) . . ?
O9 Cr3 O12 83.0(6) . . ?
O9 Cr3 O16 93.2(6) . . ?
O12 Cr3 O16 96.1(7) . . ?
O9 Cr3 O13 91.6(6) . . ?
O12 Cr3 O13 174.4(6) . . ?
O16 Cr3 O13 82.5(7) . . ?
O9 Cr3 N3 170.3(6) . . ?
O12 Cr3 N3 90.3(6) . . ?
O16 Cr3 N3 94.6(6) . . ?
O13 Cr3 N3 95.2(5) . . ?
O9 Cr3 N4 94.2(6) . . ?
O12 Cr3 N4 91.3(6) . . ?
O16 Cr3 N4 170.1(6) . . ?
O13 Cr3 N4 90.7(6) . . ?
N3 Cr3 N4 78.8(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
C5 N1 C1 C2 0.0 . . . . ?
Cr1 N1 C1 C2 -173.6(8) . . . . ?
N1 C1 C2 C3 0.0 . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 N1 0.0 . . . . ?
C3 C4 C5 C6 -178.2(13) . . . . ?
C1 N1 C5 C4 0.0 . . . . ?
Cr1 N1 C5 C4 174.1(8) . . . . ?
C1 N1 C5 C6 178.4(12) . . . . ?
Cr1 N1 C5 C6 -7.5(11) . . . . ?
C10 N2 C6 C7 0.0 . . . . ?
Cr1 N2 C6 C7 176.0(9) . . . . ?
C10 N2 C6 C5 -176.7(13) . . . . ?
Cr1 N2 C6 C5 -0.7(12) . . . . ?
C4 C5 C6 N2 -176.4(8) . . . . ?
N1 C5 C6 N2 5.4(13) . . . . ?
C4 C5 C6 C7 7.0(15) . . . . ?
N1 C5 C6 C7 -171.2(8) . . . . ?
N2 C6 C7 C8 0.0 . . . . ?
C5 C6 C7 C8 176.5(14) . . . . ?
C6 C7 C8 C9 0.0 . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C8 C9 C10 N2 0.0 . . . . ?
C6 N2 C10 C9 0.0 . . . . ?
Cr1 N2 C10 C9 -175.7(10) . . . . ?
C15 N3 C11 C12 0.0 . . . . ?
Cr3 N3 C11 C12 -175.8(9) . . . . ?
N3 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C13 C14 C15 N3 0.0 . . . . ?
C13 C14 C15 C16 -178.3(13) . . . . ?
C11 N3 C15 C14 0.0 . . . . ?
Cr3 N3 C15 C14 176.1(8) . . . . ?
C11 N3 C15 C16 178.5(11) . . . . ?
Cr3 N3 C15 C16 -5.4(10) . . . . ?
C20 N4 C16 C17 0.0 . . . . ?
Cr3 N4 C16 C17 -178.4(8) . . . . ?
C20 N4 C16 C15 -176.8(12) . . . . ?
Cr3 N4 C16 C15 4.7(11) . . . . ?
C14 C15 C16 C17 1.9(14) . . . . ?
N3 C15 C16 C17 -176.5(7) . . . . ?
C14 C15 C16 N4 178.6(8) . . . . ?
N3 C15 C16 N4 0.3(12) . . . . ?
N4 C16 C17 C18 0.0 . . . . ?
C15 C16 C17 C18 176.7(13) . . . . ?
C16 C17 C18 C19 0.0 . . . . ?
C17 C18 C19 C20 0.0 . . . . ?
C18 C19 C20 N4 0.0 . . . . ?
C16 N4 C20 C19 0.0 . . . . ?
Cr3 N4 C20 C19 178.2(10) . . . . ?
O2 C21 C22 O3 2(3) . . . . ?
O1 C21 C22 O3 -179.3(19) . . . . ?
O2 C21 C22 O4 175.5(19) . . . . ?
O1 C21 C22 O4 -6(3) . . . . ?
O6 C23 C24 O7 -3(4) . . . . ?
O5 C23 C24 O7 -173(2) . . . . ?
O6 C23 C24 O8 177(2) . . . . ?
O5 C23 C24 O8 7(3) . . . . ?
O10 C25 C26 O11 -6(5) . . . . ?
O9 C25 C26 O11 173(3) . . . . ?
O10 C25 C26 O12 -179(3) . . . . ?
O9 C25 C26 O12 0(4) . . . . ?
O14 C27 C28 O15 -2(4) . . . . ?
O13 C27 C28 O15 -180(2) . . . . ?
O14 C27 C28 O16 177(2) . . . . ?
O13 C27 C28 O16 0(3) . . . . ?
N5 C29 C30 N6 -9(3) . . . . ?
N5 C31 C32 N6 -11(3) . . . . ?
N5 C33 C34 N6 -12(3) . . . . ?
C34 C33 N5 C29 -51(3) . . . . ?
C34 C33 N5 C31 70(3) . . . . ?
C30 C29 N5 C33 63(3) . . . . ?
C30 C29 N5 C31 -55(3) . . . . ?
C32 C31 N5 C33 -55(3) . . . . ?
C32 C31 N5 C29 66(3) . . . . ?
C33 C34 N6 C30 68(3) . . . . ?
C33 C34 N6 C32 -54(3) . . . . ?
C29 C30 N6 C34 -55(3) . . . . ?
C29 C30 N6 C32 65(3) . . . . ?
C31 C32 N6 C34 68(3) . . . . ?
C31 C32 N6 C30 -54(3) . . . . ?
O2 C21 O1 Cr1 -170.6(16) . . . . ?
C22 C21 O1 Cr1 11(2) . . . . ?
O3 C22 O4 Cr1 170(2) . . . . ?
C21 C22 O4 Cr1 -2(2) . . . . ?
O6 C23 O5 Cr1 -169(2) . . . . ?
C24 C23 O5 Cr1 1(2) . . . . ?
O7 C24 O8 Cr1 169(2) . . . . ?
C23 C24 O8 Cr1 -11(3) . . . . ?
O10 C25 O9 Cr3 178(3) . . . . ?
C26 C25 O9 Cr3 -1(3) . . . . ?
O11 C26 O12 Cr3 -172(3) . . . . ?
C25 C26 O12 Cr3 1(3) . . . . ?
O14 C27 O13 Cr3 180(2) . . . . ?
C28 C27 O13 Cr3 -3(2) . . . . ?
O15 C28 O16 Cr3 -177(2) . . . . ?
C27 C28 O16 Cr3 3(3) . . . . ?

_refine_diff_density_max         1.602
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.176



####################################################################### 
# 
# 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_comp1H2O
_database_code_depnum_ccdc_archive 'CCDC 2159913'
loop_
_audit_author_name
_audit_author_address
'Lidija Andros Dubraja'
;Rudjer Boskovic Institute
Croatia
;
_audit_update_record             
;
2022-03-18 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            '(H2-DABCO)[Cr(bpy)(ox)2]2 x 12(H2O)'
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C14 H8 Cr N2 O8), C6 H14 N2, 12(H2 O )'
_chemical_formula_sum            'C34 H54 Cr2 N6 O28'
_chemical_formula_weight         1098.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   12.2426(5)
_cell_length_b                   13.2490(6)
_cell_length_c                   15.9614(7)
_cell_angle_alpha                99.315(5)
_cell_angle_beta                 100.091(5)
_cell_angle_gamma                107.873(4)
_cell_volume                     2360.80(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    24282
_cell_measurement_theta_min      3.8980
_cell_measurement_theta_max      77.6370

_exptl_crystal_description       stick-like
_exptl_crystal_colour            'orange and purplish red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_F_000             1144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    4.680
_exptl_absorpt_correction_T_min  0.42676
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.442
_oxdiff_exptl_absorpt_empirical_full_max 2.310
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      140(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            38971
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.602
_diffrn_reflns_theta_max         80.615
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10043
_reflns_number_gt                9364
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_structure_solution    'SIR-2019 (Burla, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Mercury (2020)'
_computing_publication_material  'PLATON (Spek, 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0648P)²+3.9035P] 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     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.00067(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         10043
_refine_ls_number_parameters     710
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0508
_refine_ls_wR_factor_ref         0.1366
_refine_ls_wR_factor_gt          0.1347
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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
C1 C 0.7396(3) 0.5370(2) 0.40751(19) 0.0284(6) Uani 1 1 d . . . . .
H1 H 0.675070 0.510729 0.357479 0.034 Uiso 1 1 calc R U . . .
C2 C 0.7165(3) 0.5459(2) 0.48994(19) 0.0297(6) Uani 1 1 d . . . . .
H2 H 0.637430 0.525627 0.496276 0.036 Uiso 1 1 calc R U . . .
C3 C 0.8104(3) 0.5848(2) 0.56267(19) 0.0288(6) Uani 1 1 d . . . . .
H3 H 0.796768 0.591996 0.619772 0.035 Uiso 1 1 calc R U . . .
C4 C 0.9247(3) 0.6131(2) 0.55124(17) 0.0251(5) Uani 1 1 d . . . . .
H4 H 0.990455 0.639836 0.600384 0.030 Uiso 1 1 calc R U . . .
C5 C 0.9417(2) 0.6019(2) 0.46718(17) 0.0228(5) Uani 1 1 d . . . . .
C6 C 1.0596(2) 0.6290(2) 0.44721(16) 0.0218(5) Uani 1 1 d . . . . .
C7 C 1.1652(2) 0.6776(2) 0.50932(18) 0.0257(5) Uani 1 1 d . . . . .
H7 H 1.165918 0.694077 0.569634 0.031 Uiso 1 1 calc R U . . .
C8 C 1.2699(3) 0.7022(2) 0.48288(19) 0.0283(6) Uani 1 1 d . . . . .
H8 H 1.343350 0.735703 0.524898 0.034 Uiso 1 1 calc R U . . .
C9 C 1.2671(3) 0.6774(2) 0.39422(19) 0.0288(6) Uani 1 1 d . . . . .
H9 H 1.338239 0.694012 0.374711 0.035 Uiso 1 1 calc R U . . .
C10 C 1.1585(2) 0.6281(2) 0.33522(18) 0.0259(5) Uani 1 1 d . . . . .
H10 H 1.155994 0.610673 0.274622 0.031 Uiso 1 1 calc R U . . .
C11 C 0.3535(3) 1.0099(2) 0.48561(18) 0.0281(6) Uani 1 1 d . . . . .
H11 H 0.430802 1.051931 0.519995 0.034 Uiso 1 1 calc R U . . .
C12 C 0.3353(3) 0.9816(3) 0.39562(19) 0.0340(6) Uani 1 1 d . . . . .
H12 H 0.398968 1.004426 0.368532 0.041 Uiso 1 1 calc R U . . .
C13 C 0.2230(3) 0.9197(3) 0.34580(19) 0.0346(7) Uani 1 1 d . . . . .
H13 H 0.209189 0.898127 0.284046 0.041 Uiso 1 1 calc R U . . .
C14 C 0.1307(3) 0.8892(2) 0.38634(18) 0.0301(6) Uani 1 1 d . . . . .
H14 H 0.052711 0.847821 0.352845 0.036 Uiso 1 1 calc R U . . .
C15 C 0.1543(2) 0.9201(2) 0.47672(17) 0.0244(5) Uani 1 1 d . . . . .
C16 C 0.0636(2) 0.8964(2) 0.52770(17) 0.0242(5) Uani 1 1 d . . . . .
C17 C -0.0568(3) 0.8535(2) 0.4905(2) 0.0301(6) Uani 1 1 d . . . . .
H17 H -0.085958 0.833037 0.428816 0.036 Uiso 1 1 calc R U . . .
C18 C -0.1343(3) 0.8409(2) 0.5454(2) 0.0330(6) Uani 1 1 d . . . . .
H18 H -0.217195 0.811829 0.521266 0.040 Uiso 1 1 calc R U . . .
C19 C -0.0905(3) 0.8705(2) 0.6346(2) 0.0340(6) Uani 1 1 d . . . . .
H19 H -0.142525 0.863078 0.672713 0.041 Uiso 1 1 calc R U . . .
C20 C 0.0313(3) 0.9116(2) 0.6681(2) 0.0286(6) Uani 1 1 d . . . . .
H20 H 0.062006 0.931016 0.729684 0.034 Uiso 1 1 calc R U . . .
C21 C 0.8993(2) 0.3314(2) 0.22513(17) 0.0254(5) Uani 1 1 d . . . . .
C22 C 0.9386(3) 0.3934(2) 0.15503(18) 0.0294(6) Uani 1 1 d . . . . .
C23 C 0.8167(2) 0.6783(2) 0.19564(17) 0.0243(5) Uani 1 1 d . . . . .
C24 C 0.7135(2) 0.5679(2) 0.16579(17) 0.0254(5) Uani 1 1 d . . . . .
C25 C 0.3363(2) 0.9297(2) 0.80820(17) 0.0259(5) Uani 1 1 d . . . . .
C26 C 0.3560(2) 0.8539(2) 0.73241(17) 0.0240(5) Uani 1 1 d . . . . .
C27 C 0.3553(3) 1.2288(2) 0.69090(18) 0.0267(5) Uani 1 1 d . . . . .
C28 C 0.4706(3) 1.2021(2) 0.70917(17) 0.0278(6) Uani 1 1 d . . . . .
C29 C 0.4070(3) 0.1212(2) 0.0418(2) 0.0341(7) Uani 1 1 d . . . . .
H29A H 0.371218 0.084696 0.084783 0.041 Uiso 1 1 calc R U . . .
H29B H 0.437846 0.071554 0.007678 0.041 Uiso 1 1 calc R U . . .
C30 C 0.3143(3) 0.1483(2) -0.01932(19) 0.0303(6) Uani 1 1 d . . . . .
H30A H 0.285305 0.094651 -0.076245 0.036 Uiso 1 1 calc R U . . .
H30B H 0.246249 0.146296 0.006783 0.036 Uiso 1 1 calc R U . . .
C31 C 0.5749(3) 0.2683(3) 0.0256(2) 0.0358(7) Uani 1 1 d . . . . .
H31A H 0.620737 0.221454 0.009373 0.043 Uiso 1 1 calc R U . . .
H31B H 0.630809 0.343228 0.052681 0.043 Uiso 1 1 calc R U . . .
C32 C 0.4866(3) 0.2682(3) -0.0558(2) 0.0349(6) Uani 1 1 d . . . . .
H32A H 0.517245 0.336067 -0.075910 0.042 Uiso 1 1 calc R U . . .
H32B H 0.474919 0.205484 -0.103761 0.042 Uiso 1 1 calc R U . . .
C33 C 0.4560(3) 0.3079(2) 0.12588(18) 0.0291(6) Uani 1 1 d . . . . .
H33A H 0.520574 0.371781 0.165373 0.035 Uiso 1 1 calc R U . . .
H33B H 0.399692 0.275794 0.160013 0.035 Uiso 1 1 calc R U . . .
C34 C 0.3928(3) 0.3430(2) 0.05017(18) 0.0288(6) Uani 1 1 d . . . . .
H34A H 0.316402 0.346829 0.060088 0.035 Uiso 1 1 calc R U . . .
H34B H 0.441991 0.415852 0.045727 0.035 Uiso 1 1 calc R U . . .
Cr1 Cr 0.89184(4) 0.53727(3) 0.27744(3) 0.02115(11) Uani 1 1 d . . . . .
Cr2 Cr 0.28640(4) 1.00515(3) 0.65899(3) 0.02111(11) Uani 1 1 d . . . . .
N1 N 0.8498(2) 0.56433(18) 0.39626(14) 0.0226(4) Uani 1 1 d . . . . .
N2 N 1.05689(19) 0.60401(17) 0.36056(14) 0.0217(4) Uani 1 1 d . . . . .
N3 N 0.2651(2) 0.97948(18) 0.52567(14) 0.0230(4) Uani 1 1 d . . . . .
N4 N 0.1069(2) 0.92448(18) 0.61549(15) 0.0241(4) Uani 1 1 d . . . . .
N5 N 0.3725(2) 0.26043(19) -0.03188(15) 0.0264(5) Uani 1 1 d . . . . .
N6 N 0.5051(2) 0.2257(2) 0.08794(16) 0.0298(5) Uani 1 1 d . . . . .
O1 O 0.87672(17) 0.38962(15) 0.28846(12) 0.0260(4) Uani 1 1 d . . . . .
O2 O 0.8930(2) 0.23706(17) 0.21954(14) 0.0348(5) Uani 1 1 d . . . . .
O3 O 0.9572(2) 0.34700(18) 0.08980(14) 0.0407(5) Uani 1 1 d . . . . .
O4 O 0.94830(18) 0.49544(15) 0.17363(12) 0.0267(4) Uani 1 1 d . . . . .
O5 O 0.90478(17) 0.68124(15) 0.25393(12) 0.0253(4) Uani 1 1 d . . . . .
O6 O 0.81047(18) 0.75430(16) 0.16180(13) 0.0297(4) Uani 1 1 d . . . . .
O7 O 0.62757(19) 0.55547(17) 0.10903(14) 0.0344(5) Uani 1 1 d . . . . .
O8 O 0.73039(17) 0.49437(15) 0.20597(12) 0.0267(4) Uani 1 1 d . . . . .
O9 O 0.29589(17) 1.00295(15) 0.78283(12) 0.0256(4) Uani 1 1 d . . . . .
O10 O 0.3609(2) 0.91992(17) 0.88266(13) 0.0323(4) Uani 1 1 d . . . . .
O11 O 0.39342(19) 0.78056(16) 0.74741(12) 0.0294(4) Uani 1 1 d . . . . .
O12 O 0.33104(17) 0.87422(15) 0.65737(12) 0.0259(4) Uani 1 1 d . . . . .
O13 O 0.26046(17) 1.14429(15) 0.66795(12) 0.0261(4) Uani 1 1 d . . . . .
O14 O 0.3592(2) 1.32332(17) 0.69935(16) 0.0386(5) Uani 1 1 d . . . . .
O15 O 0.5662(2) 1.27291(19) 0.74134(15) 0.0401(5) Uani 1 1 d . . . . .
O16 O 0.45367(17) 1.09871(16) 0.68781(13) 0.0278(4) Uani 1 1 d . . . . .
O17 O 0.4588(2) 0.50679(19) 0.33199(16) 0.0386(5) Uani 1 1 d D . . . .
O18 O 0.9180(2) 0.09747(19) 0.07619(17) 0.0419(5) Uani 1 1 d D . . . .
O19 O 0.8331(2) 0.7906(2) 0.86770(18) 0.0451(6) Uani 1 1 d D . . . .
O20 O 0.2323(2) 0.4227(2) 0.22794(17) 0.0474(6) Uani 1 1 d D . . . .
O21 O 0.9909(2) 0.9440(2) 0.15281(18) 0.0456(6) Uani 1 1 d D . . . .
O22 O 0.3001(2) 0.1307(2) 0.24648(18) 0.0447(6) Uani 1 1 d D . . . .
O23 O 0.1541(2) 0.8620(2) 0.09415(18) 0.0468(6) Uani 1 1 d D . . . .
O24 O 0.5550(2) 0.7256(2) 0.47639(16) 0.0417(5) Uani 1 1 d D . . . .
O25 O 0.6144(2) 0.0382(2) 0.81202(18) 0.0463(6) Uani 1 1 d D . . . .
O26 O 0.4852(2) 0.31153(19) 0.35842(15) 0.0377(5) Uani 1 1 d D . . . .
O27 O 0.0743(2) 0.6325(2) 0.07735(16) 0.0459(6) Uani 1 1 d D . . . .
O28 O 0.2717(3) 0.5677(2) 0.1177(2) 0.0578(7) Uani 1 1 d D . . . .
H17A H 0.387(2) 0.481(4) 0.300(3) 0.087 Uiso 1 1 d D U . . .
H17B H 0.505(4) 0.554(4) 0.311(3) 0.087 Uiso 1 1 d D U . . .
H18A H 0.908(5) 0.140(4) 0.119(2) 0.087 Uiso 1 1 d D U . . .
H18B H 0.893(5) 0.103(4) 0.0236(16) 0.087 Uiso 1 1 d D U . . .
H19A H 0.9092(18) 0.819(4) 0.887(3) 0.087 Uiso 1 1 d D U . . .
H19B H 0.806(4) 0.828(4) 0.835(3) 0.087 Uiso 1 1 d D U . . .
H20A H 0.234(5) 0.458(4) 0.187(3) 0.087 Uiso 1 1 d D U . . .
H20B H 0.211(5) 0.3531(16) 0.209(3) 0.087 Uiso 1 1 d D U . . .
H21A H 0.963(4) 0.979(4) 0.119(3) 0.087 Uiso 1 1 d D U . . .
H21B H 0.941(4) 0.886(3) 0.159(4) 0.087 Uiso 1 1 d D U . . .
H22A H 0.348(4) 0.185(3) 0.289(3) 0.087 Uiso 1 1 d D U . . .
H22B H 0.330(4) 0.081(3) 0.230(3) 0.087 Uiso 1 1 d D U . . .
H23A H 0.108(4) 0.896(4) 0.110(4) 0.087 Uiso 1 1 d D U . . .
H23B H 0.125(4) 0.7923(17) 0.090(4) 0.087 Uiso 1 1 d D U . . .
H24A H 0.544(5) 0.718(4) 0.5280(18) 0.087 Uiso 1 1 d D U . . .
H24B H 0.525(5) 0.665(3) 0.437(2) 0.087 Uiso 1 1 d D U . . .
H25A H 0.683(3) 0.083(3) 0.846(3) 0.087 Uiso 1 1 d D U . . .
H25B H 0.579(4) 0.072(4) 0.779(3) 0.087 Uiso 1 1 d D U . . .
H26A H 0.480(5) 0.373(3) 0.351(4) 0.087 Uiso 1 1 d D U . . .
H26B H 0.539(4) 0.294(4) 0.338(4) 0.087 Uiso 1 1 d D U . . .
H27A H 0.026(4) 0.588(4) 0.100(3) 0.087 Uiso 1 1 d D U . . .
H27B H 0.047(4) 0.621(4) 0.0211(14) 0.087 Uiso 1 1 d D U . . .
H28A H 0.210(3) 0.582(4) 0.095(3) 0.087 Uiso 1 1 d D U . . .
H28B H 0.323(4) 0.617(3) 0.160(3) 0.087 Uiso 1 1 d D U . . .
H5N H 0.322(5) 0.269(4) -0.078(4) 0.087 Uiso 1 1 d . U . . .
H6N H 0.553(5) 0.212(4) 0.133(4) 0.087 Uiso 1 1 d . 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
C1 N1 1.338(4) . ?
C1 C2 1.388(4) . ?
C2 C3 1.382(4) . ?
C3 C4 1.387(4) . ?
C4 C5 1.385(4) . ?
C5 N1 1.351(3) . ?
C5 C6 1.481(4) . ?
C6 N2 1.361(3) . ?
C6 C7 1.380(4) . ?
C7 C8 1.380(4) . ?
C8 C9 1.392(4) . ?
C9 C10 1.382(4) . ?
C10 N2 1.337(4) . ?
C11 N3 1.342(4) . ?
C11 C12 1.384(4) . ?
C12 C13 1.381(5) . ?
C13 C14 1.386(5) . ?
C14 C15 1.386(4) . ?
C15 N3 1.358(3) . ?
C15 C16 1.475(4) . ?
C16 N4 1.354(3) . ?
C16 C17 1.386(4) . ?
C17 C18 1.390(5) . ?
C18 C19 1.376(5) . ?
C19 C20 1.391(4) . ?
C20 N4 1.346(4) . ?
C21 O2 1.216(3) . ?
C21 O1 1.292(3) . ?
C21 C22 1.549(4) . ?
C22 O3 1.215(4) . ?
C22 O4 1.300(3) . ?
C23 O6 1.233(3) . ?
C23 O5 1.281(3) . ?
C23 C24 1.547(4) . ?
C24 O7 1.210(3) . ?
C24 O8 1.297(3) . ?
C25 O10 1.212(3) . ?
C25 O9 1.304(3) . ?
C25 C26 1.545(4) . ?
C26 O11 1.233(3) . ?
C26 O12 1.275(3) . ?
C27 O14 1.222(4) . ?
C27 O13 1.287(3) . ?
C27 C28 1.549(4) . ?
C28 O15 1.214(4) . ?
C28 O16 1.298(3) . ?
C29 N6 1.497(4) . ?
C29 C30 1.531(4) . ?
C30 N5 1.500(4) . ?
C31 N6 1.491(4) . ?
C31 C32 1.537(4) . ?
C32 N5 1.490(4) . ?
C33 N6 1.494(4) . ?
C33 C34 1.533(4) . ?
C34 N5 1.493(4) . ?
Cr1 O1 1.9474(19) . ?
Cr1 O8 1.9600(19) . ?
Cr1 O4 1.967(2) . ?
Cr1 O5 1.9676(19) . ?
Cr1 N2 2.052(2) . ?
Cr1 N1 2.056(2) . ?
Cr2 O13 1.9517(19) . ?
Cr2 O9 1.9652(19) . ?
Cr2 O16 1.967(2) . ?
Cr2 O12 1.9700(19) . ?
Cr2 N3 2.056(2) . ?
Cr2 N4 2.059(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.1(3) . . ?
C3 C2 C1 118.9(3) . . ?
C2 C3 C4 119.2(3) . . ?
C5 C4 C3 119.1(3) . . ?
N1 C5 C4 121.6(3) . . ?
N1 C5 C6 114.7(2) . . ?
C4 C5 C6 123.7(2) . . ?
N2 C6 C7 121.2(2) . . ?
N2 C6 C5 114.5(2) . . ?
C7 C6 C5 124.3(2) . . ?
C6 C7 C8 119.3(3) . . ?
C7 C8 C9 119.5(3) . . ?
C10 C9 C8 118.4(3) . . ?
N2 C10 C9 122.2(3) . . ?
N3 C11 C12 121.8(3) . . ?
C13 C12 C11 119.0(3) . . ?
C12 C13 C14 119.7(3) . . ?
C13 C14 C15 118.7(3) . . ?
N3 C15 C14 121.5(3) . . ?
N3 C15 C16 114.3(2) . . ?
C14 C15 C16 124.2(3) . . ?
N4 C16 C17 121.5(3) . . ?
N4 C16 C15 114.6(2) . . ?
C17 C16 C15 123.8(3) . . ?
C16 C17 C18 118.7(3) . . ?
C19 C18 C17 119.8(3) . . ?
C18 C19 C20 118.9(3) . . ?
N4 C20 C19 121.7(3) . . ?
O2 C21 O1 124.8(3) . . ?
O2 C21 C22 121.4(3) . . ?
O1 C21 C22 113.8(2) . . ?
O3 C22 O4 125.5(3) . . ?
O3 C22 C21 120.8(3) . . ?
O4 C22 C21 113.7(2) . . ?
O6 C23 O5 125.3(3) . . ?
O6 C23 C24 119.5(2) . . ?
O5 C23 C24 115.2(2) . . ?
O7 C24 O8 125.7(3) . . ?
O7 C24 C23 120.5(2) . . ?
O8 C24 C23 113.7(2) . . ?
O10 C25 O9 126.3(3) . . ?
O10 C25 C26 120.5(2) . . ?
O9 C25 C26 113.1(2) . . ?
O11 C26 O12 125.2(2) . . ?
O11 C26 C25 119.7(2) . . ?
O12 C26 C25 115.0(2) . . ?
O14 C27 O13 125.6(3) . . ?
O14 C27 C28 120.5(3) . . ?
O13 C27 C28 113.9(2) . . ?
O15 C28 O16 124.7(3) . . ?
O15 C28 C27 121.7(3) . . ?
O16 C28 C27 113.6(2) . . ?
N6 C29 C30 108.0(2) . . ?
N5 C30 C29 107.4(2) . . ?
N6 C31 C32 107.3(2) . . ?
N5 C32 C31 108.1(2) . . ?
N6 C33 C34 108.0(2) . . ?
N5 C34 C33 107.7(2) . . ?
O1 Cr1 O8 93.95(8) . . ?
O1 Cr1 O4 83.04(8) . . ?
O8 Cr1 O4 90.99(8) . . ?
O1 Cr1 O5 174.40(8) . . ?
O8 Cr1 O5 83.52(8) . . ?
O4 Cr1 O5 91.99(8) . . ?
O1 Cr1 N2 93.32(8) . . ?
O8 Cr1 N2 171.07(9) . . ?
O4 Cr1 N2 95.03(9) . . ?
O5 Cr1 N2 89.67(8) . . ?
O1 Cr1 N1 88.48(8) . . ?
O8 Cr1 N1 96.08(9) . . ?
O4 Cr1 N1 169.31(8) . . ?
O5 Cr1 N1 96.75(8) . . ?
N2 Cr1 N1 78.93(9) . . ?
O13 Cr2 O9 95.37(8) . . ?
O13 Cr2 O16 82.95(8) . . ?
O9 Cr2 O16 90.41(8) . . ?
O13 Cr2 O12 173.54(9) . . ?
O9 Cr2 O12 82.64(8) . . ?
O16 Cr2 O12 90.90(8) . . ?
O13 Cr2 N3 92.90(8) . . ?
O9 Cr2 N3 170.39(9) . . ?
O16 Cr2 N3 95.46(9) . . ?
O12 Cr2 N3 89.66(8) . . ?
O13 Cr2 N4 89.78(9) . . ?
O9 Cr2 N4 96.59(9) . . ?
O16 Cr2 N4 170.35(9) . . ?
O12 Cr2 N4 96.55(9) . . ?
N3 Cr2 N4 78.52(9) . . ?
C1 N1 C5 119.2(2) . . ?
C1 N1 Cr1 124.61(19) . . ?
C5 N1 Cr1 115.82(18) . . ?
C10 N2 C6 119.3(2) . . ?
C10 N2 Cr1 124.85(18) . . ?
C6 N2 Cr1 115.77(18) . . ?
C11 N3 C15 119.3(2) . . ?
C11 N3 Cr2 124.52(19) . . ?
C15 N3 Cr2 116.01(18) . . ?
C20 N4 C16 119.4(2) . . ?
C20 N4 Cr2 124.02(19) . . ?
C16 N4 Cr2 115.99(18) . . ?
C32 N5 C34 110.4(2) . . ?
C32 N5 C30 109.8(2) . . ?
C34 N5 C30 109.6(2) . . ?
C31 N6 C33 109.9(2) . . ?
C31 N6 C29 109.9(2) . . ?
C33 N6 C29 110.1(2) . . ?
C21 O1 Cr1 114.97(17) . . ?
C22 O4 Cr1 113.94(17) . . ?
C23 O5 Cr1 112.81(17) . . ?
C24 O8 Cr1 113.16(17) . . ?
C25 O9 Cr2 114.37(16) . . ?
C26 O12 Cr2 114.27(17) . . ?
C27 O13 Cr2 114.90(17) . . ?
C28 O16 Cr2 113.78(18) . . ?

_refine_diff_density_max         0.676
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.082



####################################################################### 
# 
# 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 2159916'
loop_
_audit_author_name
_audit_author_address
'Lidija Andros Dubraja'
;Rudjer Boskovic Institute
Croatia
;
_audit_update_record             
;
2022-03-18 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            (CH3-DABCO)[Cr(bpy)(ox)2]
_chemical_melting_point          ?
_chemical_formula_moiety         '(C14 H8 Cr N2 O8), C7 H16 N2'
_chemical_formula_sum            'C21 H23 Cr N4 O8'
_chemical_formula_weight         511.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   9.5955(4)
_cell_length_b                   9.7701(5)
_cell_length_c                   12.4681(7)
_cell_angle_alpha                91.438(4)
_cell_angle_beta                 100.633(4)
_cell_angle_gamma                107.230(4)
_cell_volume                     1093.28(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4473
_cell_measurement_theta_min      4.7230
_cell_measurement_theta_max      74.4390

_exptl_crystal_description       plate-like
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_F_000             530
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    4.816
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.70674
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.469
_oxdiff_exptl_absorpt_empirical_full_max 2.350
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Ruby
_diffrn_detector_area_resol_mean 10.4323
_diffrn_reflns_number            7468
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.620
_diffrn_reflns_theta_max         74.869
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4281
_reflns_number_gt                3673
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_structure_solution    'SIR-2019 (Burla, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Mercury (2020)'
_computing_publication_material  'PLATON (Spek, 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0886P)²+1.7751P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4281
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1764
_refine_ls_wR_factor_gt          0.1616
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2386(6) 0.5681(6) 0.5227(4) 0.0576(11) Uani 1 1 d . . . . .
H1 H 0.201841 0.644180 0.533908 0.069 Uiso 1 1 calc R U . . .
C2 C 0.2666(6) 0.4886(6) 0.6094(4) 0.0682(14) Uani 1 1 d . . . . .
H2 H 0.246349 0.508528 0.677128 0.082 Uiso 1 1 calc R U . . .
C3 C 0.3250(6) 0.3797(5) 0.5932(4) 0.0654(14) Uani 1 1 d . . . . .
H3 H 0.349039 0.327361 0.651228 0.078 Uiso 1 1 calc R U . . .
C4 C 0.3483(5) 0.3474(4) 0.4914(4) 0.0543(11) Uani 1 1 d . . . . .
H4 H 0.385058 0.271622 0.479254 0.065 Uiso 1 1 calc R U . . .
C5 C 0.3160(4) 0.4301(4) 0.4069(3) 0.0402(8) Uani 1 1 d . . . . .
C6 C 0.3369(4) 0.4064(4) 0.2949(3) 0.0398(8) Uani 1 1 d . . . . .
C7 C 0.3840(5) 0.2952(5) 0.2596(4) 0.0597(12) Uani 1 1 d . . . . .
H7 H 0.402905 0.227955 0.307065 0.072 Uiso 1 1 calc R U . . .
C8 C 0.4020(6) 0.2859(6) 0.1537(5) 0.0720(16) Uani 1 1 d . . . . .
H8 H 0.431852 0.210937 0.128212 0.086 Uiso 1 1 calc R U . . .
C9 C 0.3761(6) 0.3873(6) 0.0848(4) 0.0680(14) Uani 1 1 d . . . . .
H9 H 0.391465 0.383581 0.013398 0.082 Uiso 1 1 calc R U . . .
C10 C 0.3273(5) 0.4941(5) 0.1229(3) 0.0502(10) Uani 1 1 d . . . . .
H10 H 0.307006 0.561238 0.075900 0.060 Uiso 1 1 calc R U . . .
C11 C 0.4030(5) 0.9238(4) 0.3598(3) 0.0424(8) Uani 1 1 d . . . . .
C12 C 0.2504(5) 0.9133(4) 0.3885(3) 0.0441(9) Uani 1 1 d . . . . .
C13 C -0.0623(5) 0.5422(4) 0.1608(3) 0.0431(8) Uani 1 1 d . . . . .
C14 C 0.0284(5) 0.6582(4) 0.0961(4) 0.0493(10) Uani 1 1 d . . . . .
C15 C 0.8013(5) 0.9358(4) 0.2849(4) 0.0510(10) Uani 1 1 d . . . . .
H15A H 0.741675 0.934834 0.340014 0.061 Uiso 1 1 calc R U . . .
H15B H 0.879052 0.893937 0.313415 0.061 Uiso 1 1 calc R U . . .
C16 C 0.7030(6) 0.8482(5) 0.1794(4) 0.0565(11) Uani 1 1 d . . . . .
H16A H 0.741079 0.770546 0.162146 0.068 Uiso 1 1 calc R U . . .
H16B H 0.602568 0.805944 0.191184 0.068 Uiso 1 1 calc R U . . .
C17 C 0.9564(6) 1.0848(6) 0.1715(5) 0.0639(13) Uani 1 1 d . . . . .
H17A H 1.034962 1.042446 0.196675 0.077 Uiso 1 1 calc R U . . .
H17B H 1.001942 1.182081 0.154100 0.077 Uiso 1 1 calc R U . . .
C18 C 0.8501(7) 0.9954(6) 0.0688(4) 0.0686(14) Uani 1 1 d . . . . .
H18A H 0.849408 1.055732 0.008198 0.082 Uiso 1 1 calc R U . . .
H18B H 0.885999 0.917255 0.048966 0.082 Uiso 1 1 calc R U . . .
C19 C 0.7468(5) 1.1502(5) 0.2173(4) 0.0548(11) Uani 1 1 d . . . . .
H19A H 0.788686 1.247344 0.197955 0.066 Uiso 1 1 calc R U . . .
H19B H 0.689601 1.153814 0.273207 0.066 Uiso 1 1 calc R U . . .
C20 C 0.6463(7) 1.0547(6) 0.1160(5) 0.0720(15) Uani 1 1 d . . . . .
H20A H 0.546431 1.015990 0.129869 0.086 Uiso 1 1 calc R U . . .
H20B H 0.641062 1.113076 0.054470 0.086 Uiso 1 1 calc R U . . .
C21 C 0.9662(5) 1.1740(5) 0.3606(4) 0.0593(12) Uani 1 1 d . . . . .
H21A H 1.009540 1.270971 0.343937 0.089 Uiso 1 1 calc R U . . .
H21B H 0.907604 1.174077 0.415232 0.089 Uiso 1 1 calc R U . . .
H21C H 1.043859 1.132987 0.387731 0.089 Uiso 1 1 calc R U . . .
N1 N 0.2622(4) 0.5401(3) 0.4231(3) 0.0393(7) Uani 1 1 d . . . . .
N2 N 0.3081(4) 0.5041(3) 0.2257(3) 0.0391(7) Uani 1 1 d . . . . .
N3 N 0.8691(4) 1.0870(3) 0.2593(3) 0.0419(7) Uani 1 1 d . . . . .
N4 N 0.6991(4) 0.9367(4) 0.0873(3) 0.0526(9) Uani 1 1 d . . . . .
O1 O 0.4129(3) 0.8015(3) 0.3240(2) 0.0447(6) Uani 1 1 d . . . . .
O2 O 0.5017(4) 1.0387(3) 0.3698(3) 0.0609(9) Uani 1 1 d . . . . .
O3 O 0.2284(4) 1.0187(3) 0.4269(4) 0.0698(10) Uani 1 1 d . . . . .
O4 O 0.1544(3) 0.7876(3) 0.3673(3) 0.0466(7) Uani 1 1 d . . . . .
O5 O 0.0170(3) 0.5150(3) 0.2484(2) 0.0412(6) Uani 1 1 d . . . . .
O6 O -0.1952(4) 0.4855(4) 0.1298(3) 0.0628(9) Uani 1 1 d . . . . .
O7 O -0.0277(4) 0.6845(5) 0.0073(3) 0.0789(12) Uani 1 1 d . . . . .
O8 O 0.1652(3) 0.7200(3) 0.1465(2) 0.0465(7) Uani 1 1 d . . . . .
Cr01 Cr 0.21945(7) 0.64984(6) 0.28812(5) 0.0350(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.339(5) . ?
C1 C2 1.379(7) . ?
C2 C3 1.368(8) . ?
C3 C4 1.373(8) . ?
C4 C5 1.389(5) . ?
C5 N1 1.348(5) . ?
C5 C6 1.469(6) . ?
C6 N2 1.357(5) . ?
C6 C7 1.385(6) . ?
C7 C8 1.368(8) . ?
C8 C9 1.376(8) . ?
C9 C10 1.372(6) . ?
C10 N2 1.333(5) . ?
C11 O2 1.222(5) . ?
C11 O1 1.300(5) . ?
C11 C12 1.546(6) . ?
C12 O3 1.215(5) . ?
C12 O4 1.284(5) . ?
C13 O6 1.213(5) . ?
C13 O5 1.292(5) . ?
C13 C14 1.554(5) . ?
C14 O7 1.207(5) . ?
C14 O8 1.300(5) . ?
C15 N3 1.496(5) . ?
C15 C16 1.536(6) . ?
C16 N4 1.456(6) . ?
C17 N3 1.501(6) . ?
C17 C18 1.541(8) . ?
C18 N4 1.456(7) . ?
C19 N3 1.500(5) . ?
C19 C20 1.534(7) . ?
C20 N4 1.452(6) . ?
C21 N3 1.493(6) . ?
N1 Cr01 2.061(3) . ?
N2 Cr01 2.064(3) . ?
O1 Cr01 1.967(3) . ?
O4 Cr01 1.959(3) . ?
O5 Cr01 1.962(3) . ?
O8 Cr01 1.947(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.6(5) . . ?
C3 C2 C1 118.4(5) . . ?
C2 C3 C4 120.1(4) . . ?
C3 C4 C5 118.8(4) . . ?
N1 C5 C4 121.3(4) . . ?
N1 C5 C6 115.0(3) . . ?
C4 C5 C6 123.7(4) . . ?
N2 C6 C7 120.8(4) . . ?
N2 C6 C5 114.9(3) . . ?
C7 C6 C5 124.3(4) . . ?
C8 C7 C6 118.8(5) . . ?
C7 C8 C9 120.0(4) . . ?
C10 C9 C8 119.0(5) . . ?
N2 C10 C9 121.7(4) . . ?
O2 C11 O1 125.0(4) . . ?
O2 C11 C12 121.3(4) . . ?
O1 C11 C12 113.7(3) . . ?
O3 C12 O4 125.2(4) . . ?
O3 C12 C11 120.4(4) . . ?
O4 C12 C11 114.4(3) . . ?
O6 C13 O5 124.9(4) . . ?
O6 C13 C14 121.4(4) . . ?
O5 C13 C14 113.7(3) . . ?
O7 C14 O8 125.4(4) . . ?
O7 C14 C13 121.0(4) . . ?
O8 C14 C13 113.7(3) . . ?
N3 C15 C16 108.7(3) . . ?
N4 C16 C15 111.9(3) . . ?
N3 C17 C18 108.7(4) . . ?
N4 C18 C17 111.6(4) . . ?
N3 C19 C20 108.0(3) . . ?
N4 C20 C19 112.7(4) . . ?
C1 N1 C5 118.7(4) . . ?
C1 N1 Cr01 125.4(3) . . ?
C5 N1 Cr01 115.9(3) . . ?
C10 N2 C6 119.6(3) . . ?
C10 N2 Cr01 124.9(3) . . ?
C6 N2 Cr01 115.3(3) . . ?
C21 N3 C15 109.6(3) . . ?
C21 N3 C19 109.6(3) . . ?
C15 N3 C19 109.0(3) . . ?
C21 N3 C17 111.2(4) . . ?
C15 N3 C17 108.7(3) . . ?
C19 N3 C17 108.7(4) . . ?
C20 N4 C18 108.7(4) . . ?
C20 N4 C16 108.4(4) . . ?
C18 N4 C16 108.4(4) . . ?
C11 O1 Cr01 113.1(2) . . ?
C12 O4 Cr01 113.9(2) . . ?
C13 O5 Cr01 114.0(2) . . ?
C14 O8 Cr01 114.5(2) . . ?
O8 Cr01 O4 93.42(13) . . ?
O8 Cr01 O5 83.31(11) . . ?
O4 Cr01 O5 92.56(12) . . ?
O8 Cr01 O1 92.75(12) . . ?
O4 Cr01 O1 82.95(11) . . ?
O5 Cr01 O1 173.86(11) . . ?
O8 Cr01 N1 169.84(12) . . ?
O4 Cr01 N1 94.42(13) . . ?
O5 Cr01 N1 89.88(12) . . ?
O1 Cr01 N1 94.62(12) . . ?
O8 Cr01 N2 94.06(13) . . ?
O4 Cr01 N2 171.75(13) . . ?
O5 Cr01 N2 91.76(12) . . ?
O1 Cr01 N2 93.22(12) . . ?
N1 Cr01 N2 78.56(13) . . ?

_refine_diff_density_max         0.661
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.106



####################################################################### 
# 
# 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_comp3MeOH
_database_code_depnum_ccdc_archive 'CCDC 2159915'
loop_
_audit_author_name
_audit_author_address
'Lidija Andros Dubraja'
;Rudjer Boskovic Institute
Croatia
;
_audit_update_record             
;
2022-03-18 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            '(CH3-DABCO)[Cr(bpy)(ox)2] x CH3OH'
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H8 Cr N2 O8, C7 H15 N2, C H4 O'
_chemical_formula_sum            'C22 H27 Cr N4 O9'
_chemical_formula_weight         543.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   15.8377(2)
_cell_length_b                   14.9630(2)
_cell_length_c                   9.93770(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.6670(10)
_cell_angle_gamma                90
_cell_volume                     2350.21(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    11406
_cell_measurement_theta_min      4.0820
_cell_measurement_theta_max      76.9960

_exptl_crystal_description       plate-like
_exptl_crystal_colour            'orange and purplish red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_F_000             1132
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    4.548
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.43892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.593
_oxdiff_exptl_absorpt_empirical_full_max 1.798
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      223(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            15683
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         5.351
_diffrn_reflns_theta_max         77.164
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4799
_reflns_number_gt                4570
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_structure_solution    'SIR-2019 (Burla, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Mercury (2020)'
_computing_publication_material  'PLATON (Spek, 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0603P)²+0.6411P] 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     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.00081(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4799
_refine_ls_number_parameters     355
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0946
_refine_ls_wR_factor_gt          0.0935
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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
C1 C 0.80391(11) 0.33614(11) 0.94286(17) 0.0305(3) Uani 1 1 d . . . . .
H1 H 0.773939 0.306207 0.871654 0.037 Uiso 1 1 calc R U . . .
C2 C 0.81874(12) 0.29230(12) 1.06472(19) 0.0368(4) Uani 1 1 d . . . . .
H2 H 0.799642 0.233493 1.076371 0.044 Uiso 1 1 calc R U . . .
C3 C 0.86233(12) 0.33727(12) 1.16871(18) 0.0350(4) Uani 1 1 d . . . . .
H3 H 0.873104 0.309051 1.252556 0.042 Uiso 1 1 calc R U . . .
C4 C 0.89022(11) 0.42381(12) 1.14990(16) 0.0294(3) Uani 1 1 d . . . . .
H4 H 0.919761 0.454965 1.220291 0.035 Uiso 1 1 calc R U . . .
C5 C 0.87363(9) 0.46342(11) 1.02511(15) 0.0227(3) Uani 1 1 d . . . . .
C6 C 0.90066(9) 0.55489(10) 0.99180(15) 0.0223(3) Uani 1 1 d . . . . .
C7 C 0.94193(10) 0.61267(11) 1.08380(17) 0.0287(3) Uani 1 1 d . . . . .
H7 H 0.955128 0.594536 1.173245 0.034 Uiso 1 1 calc R U . . .
C8 C 0.96323(11) 0.69745(12) 1.04128(18) 0.0322(4) Uani 1 1 d . . . . .
H8 H 0.991341 0.737400 1.101853 0.039 Uiso 1 1 calc R U . . .
C9 C 0.94299(11) 0.72317(11) 0.90930(19) 0.0324(4) Uani 1 1 d . . . . .
H9 H 0.956123 0.780819 0.879404 0.039 Uiso 1 1 calc R U . . .
C10 C 0.90300(10) 0.66202(11) 0.82253(17) 0.0278(3) Uani 1 1 d . . . . .
H10 H 0.889781 0.678764 0.732470 0.033 Uiso 1 1 calc R U . . .
C11 C 0.63877(11) 0.50270(10) 0.75862(17) 0.0252(3) Uani 1 1 d . . . . .
C12 C 0.65467(10) 0.42490(11) 0.66001(15) 0.0253(3) Uani 1 1 d . . . . .
C13 C 0.91344(9) 0.44521(10) 0.54018(15) 0.0234(3) Uani 1 1 d . . . . .
C14 C 0.86228(10) 0.52958(11) 0.49163(15) 0.0240(3) Uani 1 1 d . . . . .
C15 C 0.38162(12) 0.13317(12) 0.02638(17) 0.0328(4) Uani 1 1 d . . . . .
H15A H 0.437074 0.128168 -0.011432 0.039 Uiso 1 1 calc R U . . .
H15B H 0.338222 0.119953 -0.045609 0.039 Uiso 1 1 calc R U . . .
C16 C 0.37567(13) 0.06481(12) 0.14026(18) 0.0348(4) Uani 1 1 d . . . . .
H16A H 0.325230 0.027519 0.123503 0.042 Uiso 1 1 calc R U . . .
H16B H 0.425548 0.025901 0.144712 0.042 Uiso 1 1 calc R U . . .
C17 C 0.28959(12) 0.22915(13) 0.1395(2) 0.0400(4) Uani 1 1 d . . . . .
H17A H 0.243567 0.209878 0.075419 0.048 Uiso 1 1 calc R U . . .
H17B H 0.278623 0.291172 0.164833 0.048 Uiso 1 1 calc R U . . .
C18 C 0.43914(12) 0.24574(12) 0.1747(2) 0.0376(4) Uani 1 1 d . . . . .
H18A H 0.429517 0.305005 0.212747 0.045 Uiso 1 1 calc R U . . .
H18B H 0.492637 0.247586 0.130322 0.045 Uiso 1 1 calc R U . . .
C19 C 0.44580(11) 0.17651(13) 0.28870(18) 0.0348(4) Uani 1 1 d . . . . .
H19A H 0.498404 0.142365 0.285047 0.042 Uiso 1 1 calc R U . . .
H19B H 0.446141 0.206564 0.376353 0.042 Uiso 1 1 calc R U . . .
C20 C 0.29104(12) 0.17007(14) 0.2650(2) 0.0395(4) Uani 1 1 d . . . . .
H20A H 0.289611 0.207304 0.345926 0.047 Uiso 1 1 calc R U . . .
H20B H 0.241367 0.130878 0.260754 0.047 Uiso 1 1 calc R U . . .
C21 C 0.37157(17) 0.05086(18) 0.3865(2) 0.0552(6) Uani 1 1 d . . . . .
H21A H 0.324922 0.009179 0.372540 0.083 Uiso 1 1 calc R U . . .
H21B H 0.365744 0.083598 0.469630 0.083 Uiso 1 1 calc R U . . .
H21C H 0.424596 0.018230 0.392212 0.083 Uiso 1 1 calc R U . . .
C22 C 0.64135(19) 0.31922(19) 0.2877(3) 0.0615(6) Uani 1 1 d D . . . .
Cr1 Cr 0.81274(2) 0.48907(2) 0.74425(2) 0.01944(10) Uani 1 1 d . . . . .
N1 N 0.83072(8) 0.41960(9) 0.92277(13) 0.0233(3) Uani 1 1 d . . . . .
N2 N 0.88239(8) 0.57957(8) 0.86243(13) 0.0225(3) Uani 1 1 d . . . . .
N3 N 0.37071(9) 0.11483(10) 0.27122(14) 0.0319(3) Uani 1 1 d . . . . .
N4 N 0.37005(10) 0.22445(10) 0.07465(16) 0.0339(3) Uani 1 1 d . . . . .
O1 O 0.70765(7) 0.54213(7) 0.80405(11) 0.0257(2) Uani 1 1 d . . . . .
O2 O 0.56762(8) 0.52212(9) 0.78667(15) 0.0396(3) Uani 1 1 d . . . . .
O3 O 0.59584(8) 0.38944(10) 0.59514(14) 0.0398(3) Uani 1 1 d . . . . .
O4 O 0.73328(7) 0.40375(7) 0.65453(11) 0.0272(2) Uani 1 1 d . . . . .
O5 O 0.90752(7) 0.42783(7) 0.66732(11) 0.0250(2) Uani 1 1 d . . . . .
O6 O 0.95329(8) 0.40194(8) 0.46247(12) 0.0332(3) Uani 1 1 d . . . . .
O7 O 0.86638(9) 0.55915(9) 0.37886(12) 0.0362(3) Uani 1 1 d . . . . .
O8 O 0.81527(7) 0.56217(7) 0.58238(11) 0.0252(2) Uani 1 1 d . . . . .
O9A O 0.61926(15) 0.26465(15) 0.3900(3) 0.0581(8) Uani 0.807(7) 1 d . . P . .
O9B O 0.7051(6) 0.3459(6) 0.3621(9) 0.050(3) Uani 0.193(7) 1 d . . P . .
H9A H 0.616(3) 0.294(3) 0.461(4) 0.076 Uiso 0.807(7) 1 d . U P . .
H22A H 0.692(2) 0.358(3) 0.306(5) 0.076 Uiso 0.807(7) 1 d D U P . .
H22B H 0.5977(17) 0.3664(17) 0.267(3) 0.076 Uiso 1 1 d D U . . .
H22C H 0.658(2) 0.2825(19) 0.211(2) 0.076 Uiso 1 1 d D U . . .
H9B H 0.681(12) 0.347(12) 0.44(2) 0.076 Uiso 0.193(7) 1 d . U P . .
H22D H 0.597(9) 0.303(13) 0.348(15) 0.076 Uiso 0.193(7) 1 d D U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.338(2) . ?
C1 C2 1.384(2) . ?
C2 C3 1.381(3) . ?
C3 C4 1.385(3) . ?
C4 C5 1.384(2) . ?
C5 N1 1.356(2) . ?
C5 C6 1.478(2) . ?
C6 N2 1.351(2) . ?
C6 C7 1.391(2) . ?
C7 C8 1.386(2) . ?
C8 C9 1.385(3) . ?
C9 C10 1.383(2) . ?
C10 N2 1.343(2) . ?
C11 O2 1.213(2) . ?
C11 O1 1.296(2) . ?
C11 C12 1.553(2) . ?
C12 O3 1.220(2) . ?
C12 O4 1.289(2) . ?
C13 O6 1.215(2) . ?
C13 O5 1.2992(18) . ?
C13 C14 1.560(2) . ?
C14 O7 1.210(2) . ?
C14 O8 1.3005(19) . ?
C15 N4 1.463(2) . ?
C15 C16 1.533(3) . ?
C16 N3 1.508(2) . ?
C17 N4 1.466(2) . ?
C17 C20 1.528(3) . ?
C18 N4 1.465(2) . ?
C18 C19 1.534(3) . ?
C19 N3 1.507(2) . ?
C20 N3 1.506(2) . ?
C21 N3 1.492(3) . ?
C22 O9B 1.276(9) . ?
C22 O9A 1.367(4) . ?
Cr1 O8 1.9478(11) . ?
Cr1 O5 1.9555(11) . ?
Cr1 O4 1.9659(11) . ?
Cr1 O1 1.9699(11) . ?
Cr1 N1 2.0602(13) . ?
Cr1 N2 2.0649(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.35(16) . . ?
C3 C2 C1 118.21(16) . . ?
C2 C3 C4 120.22(16) . . ?
C5 C4 C3 118.51(16) . . ?
N1 C5 C4 121.49(15) . . ?
N1 C5 C6 114.74(13) . . ?
C4 C5 C6 123.77(14) . . ?
N2 C6 C7 121.25(14) . . ?
N2 C6 C5 114.75(13) . . ?
C7 C6 C5 124.00(14) . . ?
C8 C7 C6 118.82(15) . . ?
C9 C8 C7 119.81(15) . . ?
C10 C9 C8 118.42(16) . . ?
N2 C10 C9 122.29(16) . . ?
O2 C11 O1 125.77(16) . . ?
O2 C11 C12 121.00(15) . . ?
O1 C11 C12 113.23(13) . . ?
O3 C12 O4 125.30(15) . . ?
O3 C12 C11 120.69(15) . . ?
O4 C12 C11 114.00(13) . . ?
O6 C13 O5 125.74(14) . . ?
O6 C13 C14 121.02(14) . . ?
O5 C13 C14 113.24(13) . . ?
O7 C14 O8 124.88(15) . . ?
O7 C14 C13 121.65(14) . . ?
O8 C14 C13 113.46(13) . . ?
N4 C15 C16 111.47(14) . . ?
N3 C16 C15 108.37(14) . . ?
N4 C17 C20 111.28(15) . . ?
N4 C18 C19 111.55(15) . . ?
N3 C19 C18 108.18(14) . . ?
N3 C20 C17 108.67(15) . . ?
O9B C22 O9A 89.2(5) . . ?
O8 Cr1 O5 83.31(5) . . ?
O8 Cr1 O4 92.09(5) . . ?
O5 Cr1 O4 90.20(5) . . ?
O8 Cr1 O1 94.89(5) . . ?
O5 Cr1 O1 172.45(5) . . ?
O4 Cr1 O1 82.52(5) . . ?
O8 Cr1 N1 170.23(5) . . ?
O5 Cr1 N1 91.89(5) . . ?
O4 Cr1 N1 96.44(5) . . ?
O1 Cr1 N1 90.94(5) . . ?
O8 Cr1 N2 93.61(5) . . ?
O5 Cr1 N2 97.71(5) . . ?
O4 Cr1 N2 170.73(5) . . ?
O1 Cr1 N2 89.71(5) . . ?
N1 Cr1 N2 78.56(5) . . ?
C1 N1 C5 119.22(14) . . ?
C1 N1 Cr1 124.86(11) . . ?
C5 N1 Cr1 115.91(10) . . ?
C10 N2 C6 119.40(13) . . ?
C10 N2 Cr1 124.46(11) . . ?
C6 N2 Cr1 115.86(10) . . ?
C21 N3 C20 110.50(16) . . ?
C21 N3 C19 109.64(15) . . ?
C20 N3 C19 108.75(14) . . ?
C21 N3 C16 110.23(16) . . ?
C20 N3 C16 109.06(14) . . ?
C19 N3 C16 108.62(13) . . ?
C15 N4 C18 108.75(14) . . ?
C15 N4 C17 108.63(14) . . ?
C18 N4 C17 108.90(15) . . ?
C11 O1 Cr1 114.84(10) . . ?
C12 O4 Cr1 114.42(10) . . ?
C13 O5 Cr1 113.03(9) . . ?
C14 O8 Cr1 113.89(10) . . ?

_refine_diff_density_max         0.295
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.055



####################################################################### 
# 
# 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_comp4H2O
_database_code_depnum_ccdc_archive 'CCDC 2159918'
loop_
_audit_author_name
_audit_author_address
'Lidija Andros Dubraja'
;Rudjer Boskovic Institute
Croatia
;
_audit_update_record             
;
2022-03-18 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            '[H-(O)ABCO][Cr(bpy)(ox)2] x H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H8 Cr N2 O8, C7 H12 N O, H2 O'
_chemical_formula_sum            'C21 H22 Cr N3 O10'
_chemical_formula_weight         528.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   15.4312(4)
_cell_length_b                   11.8305(3)
_cell_length_c                   13.3558(4)
_cell_angle_alpha                90
_cell_angle_beta                 110.515(3)
_cell_angle_gamma                90
_cell_volume                     2283.59(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    5262
_cell_measurement_theta_min      5.1020
_cell_measurement_theta_max      75.7320

_exptl_crystal_description       plate-like
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_F_000             1092
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    4.688
_exptl_absorpt_correction_T_min  0.27626
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.411
_oxdiff_exptl_absorpt_empirical_full_max 3.256
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      298(2)
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Ruby
_diffrn_detector_area_resol_mean 10.4323
_diffrn_reflns_number            12391
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.058
_diffrn_reflns_theta_max         75.871
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4716
_reflns_number_gt                4160
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SIR-2019 (Burla, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Mercury (2020)'
_computing_publication_material  'PLATON (Spek, 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1210P)²+0.0956P] 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_number_reflns         4716
_refine_ls_number_parameters     332
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0600
_refine_ls_wR_factor_ref         0.1729
_refine_ls_wR_factor_gt          0.1620
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1057(2) 0.0152(2) 0.3004(2) 0.0471(6) Uani 1 1 d . . . . .
H1 H 0.131240 0.067986 0.354301 0.057 Uiso 1 1 calc R U . . .
C2 C 0.0424(2) -0.0621(3) 0.3115(2) 0.0544(7) Uani 1 1 d . . . . .
H2 H 0.025003 -0.060634 0.371484 0.065 Uiso 1 1 calc R U . . .
C3 C 0.0053(3) -0.1414(3) 0.2320(3) 0.0520(7) Uani 1 1 d . . . . .
H3 H -0.037408 -0.194186 0.237755 0.062 Uiso 1 1 calc R U . . .
C4 C 0.0326(2) -0.1412(2) 0.1437(2) 0.0455(6) Uani 1 1 d . . . . .
H4 H 0.008740 -0.194088 0.089487 0.055 Uiso 1 1 calc R U . . .
C5 C 0.09595(17) -0.0613(2) 0.13700(19) 0.0373(5) Uani 1 1 d . . . . .
C6 C 0.13028(17) -0.0537(2) 0.04668(19) 0.0371(5) Uani 1 1 d . . . . .
C7 C 0.1043(2) -0.1265(2) -0.0399(2) 0.0470(6) Uani 1 1 d . . . . .
H7 H 0.063580 -0.185782 -0.044003 0.056 Uiso 1 1 calc R U . . .
C8 C 0.1399(2) -0.1095(3) -0.1200(2) 0.0539(7) Uani 1 1 d . . . . .
H8 H 0.122886 -0.156943 -0.179270 0.065 Uiso 1 1 calc R U . . .
C9 C 0.2008(2) -0.0220(3) -0.1122(3) 0.0550(7) Uani 1 1 d . . . . .
H9 H 0.225089 -0.009627 -0.165951 0.066 Uiso 1 1 calc R U . . .
C10 C 0.2253(2) 0.0467(3) -0.0235(2) 0.0490(6) Uani 1 1 d . . . . .
H10 H 0.267494 0.104789 -0.016999 0.059 Uiso 1 1 calc R U . . .
C11 C 0.12277(18) 0.3193(2) 0.06142(19) 0.0395(5) Uani 1 1 d . . . . .
C12 C 0.2277(2) 0.3390(2) 0.0857(2) 0.0430(5) Uani 1 1 d . . . . .
C13 C 0.3783(2) 0.1191(2) 0.3498(2) 0.0425(5) Uani 1 1 d . . . . .
C14 C 0.32434(18) 0.2191(2) 0.3755(2) 0.0408(5) Uani 1 1 d . . . . .
C15 C 0.4978(2) -0.1598(3) 0.3188(3) 0.0600(8) Uani 1 1 d . . . . .
H15A H 0.560216 -0.174636 0.320913 0.072 Uiso 1 1 calc R U . . .
H15B H 0.495171 -0.082927 0.342865 0.072 Uiso 1 1 calc R U . . .
C16 C 0.4301(3) -0.1747(3) 0.2068(3) 0.0598(7) Uani 1 1 d . . . . .
C17 C 0.3548(2) -0.2564(3) 0.2019(3) 0.0573(7) Uani 1 1 d . . . . .
C18 C 0.3096(2) -0.2162(3) 0.2802(3) 0.0568(7) Uani 1 1 d . . . . .
H18A H 0.283998 -0.141176 0.259969 0.068 Uiso 1 1 calc R U . . .
H18B H 0.259220 -0.266643 0.277409 0.068 Uiso 1 1 calc R U . . .
C19 C 0.3795(2) -0.2132(3) 0.3931(3) 0.0608(8) Uani 1 1 d . . . . .
H19A H 0.380527 -0.138697 0.423774 0.073 Uiso 1 1 calc R U . . .
H19B H 0.362741 -0.267745 0.437364 0.073 Uiso 1 1 calc R U . . .
C20 C 0.4005(3) -0.3715(3) 0.2402(3) 0.0643(9) Uani 1 1 d . . . . .
H20A H 0.354008 -0.425666 0.242284 0.077 Uiso 1 1 calc R U . . .
H20B H 0.428832 -0.399195 0.190536 0.077 Uiso 1 1 calc R U . . .
C21 C 0.4738(3) -0.3601(3) 0.3510(4) 0.0750(13) Uani 1 1 d . . . . .
H21A H 0.461088 -0.412528 0.399962 0.090 Uiso 1 1 calc R U . . .
H21B H 0.534368 -0.377504 0.348275 0.090 Uiso 1 1 calc R U . . .
N1 N 0.13143(15) 0.01642(18) 0.21465(16) 0.0382(4) Uani 1 1 d . . . . .
N2 N 0.18960(15) 0.03195(17) 0.05386(16) 0.0383(4) Uani 1 1 d . . . . .
N3 N 0.47242(19) -0.2408(2) 0.3893(2) 0.0551(6) Uani 1 1 d . . . . .
O1 O 0.10491(12) 0.22929(15) 0.10555(14) 0.0409(4) Uani 1 1 d . . . . .
O2 O 0.06482(16) 0.38329(19) 0.00471(19) 0.0539(5) Uani 1 1 d . . . . .
O3 O 0.25469(18) 0.4281(2) 0.0605(2) 0.0666(6) Uani 1 1 d . . . . .
O4 O 0.27887(13) 0.25492(16) 0.13156(15) 0.0439(4) Uani 1 1 d . . . . .
O5 O 0.33172(13) 0.06420(15) 0.26444(15) 0.0443(4) Uani 1 1 d . . . . .
O6 O 0.45657(16) 0.0989(2) 0.40822(19) 0.0616(6) Uani 1 1 d . . . . .
O7 O 0.36491(15) 0.2829(2) 0.44782(18) 0.0581(6) Uani 1 1 d . . . . .
O8 O 0.23884(13) 0.22489(16) 0.31603(14) 0.0426(4) Uani 1 1 d . . . . .
O9 O 0.4374(3) -0.1237(3) 0.1320(3) 0.0945(11) Uani 1 1 d . . . . .
O10 O 0.1418(2) -0.3845(3) 0.1113(3) 0.0815(9) Uani 1 1 d D . . . .
Cr1 Cr 0.21444(3) 0.13837(3) 0.18319(3) 0.03515(17) Uani 1 1 d . . . . .
H3N H 0.513(3) -0.241(3) 0.451(3) 0.055(10) Uiso 1 1 d . . . . .
H10A H 0.168(4) -0.402(7) 0.063(4) 0.13(3) Uiso 1 1 d D . . . .
H10B H 0.0805(14) -0.391(5) 0.075(4) 0.086(15) Uiso 1 1 d D . . . .
H17 H 0.312(4) -0.254(4) 0.132(4) 0.086(15) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.337(4) . ?
C1 C2 1.384(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.381(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.385(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(4) . ?
C4 H4 0.9300 . ?
C5 N1 1.350(3) . ?
C5 C6 1.481(3) . ?
C6 N2 1.346(3) . ?
C6 C7 1.384(4) . ?
C7 C8 1.379(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.377(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.377(4) . ?
C9 H9 0.9300 . ?
C10 N2 1.341(4) . ?
C10 H10 0.9300 . ?
C11 O2 1.213(4) . ?
C11 O1 1.293(3) . ?
C11 C12 1.554(4) . ?
C12 O3 1.224(4) . ?
C12 O4 1.283(3) . ?
C13 O6 1.210(4) . ?
C13 O5 1.290(3) . ?
C13 C14 1.553(4) . ?
C14 O7 1.213(3) . ?
C14 O8 1.281(3) . ?
C15 N3 1.488(5) . ?
C15 C16 1.506(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 O9 1.205(5) . ?
C16 C17 1.496(5) . ?
C17 C18 1.523(5) . ?
C17 C20 1.536(5) . ?
C17 H17 0.93(5) . ?
C18 C19 1.516(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 N3 1.488(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.522(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 N3 1.503(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
N1 Cr1 2.068(2) . ?
N2 Cr1 2.062(2) . ?
N3 H3N 0.84(4) . ?
O1 Cr1 1.9648(18) . ?
O4 Cr1 1.9612(19) . ?
O5 Cr1 1.9611(19) . ?
O8 Cr1 1.9670(18) . ?
O10 H10A 0.90(2) . ?
O10 H10B 0.902(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.1(3) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C3 C2 C1 119.0(3) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 119.0(3) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N1 C5 C4 121.4(2) . . ?
N1 C5 C6 114.9(2) . . ?
C4 C5 C6 123.8(2) . . ?
N2 C6 C7 121.3(2) . . ?
N2 C6 C5 114.6(2) . . ?
C7 C6 C5 124.2(2) . . ?
C8 C7 C6 118.7(3) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
C9 C8 C7 119.9(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 C9 C8 118.9(3) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
N2 C10 C9 121.6(3) . . ?
N2 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
O2 C11 O1 124.8(3) . . ?
O2 C11 C12 121.6(2) . . ?
O1 C11 C12 113.6(2) . . ?
O3 C12 O4 126.0(3) . . ?
O3 C12 C11 120.1(3) . . ?
O4 C12 C11 113.9(2) . . ?
O6 C13 O5 126.3(3) . . ?
O6 C13 C14 120.0(2) . . ?
O5 C13 C14 113.7(2) . . ?
O7 C14 O8 126.3(2) . . ?
O7 C14 C13 118.9(2) . . ?
O8 C14 C13 114.8(2) . . ?
N3 C15 C16 108.0(3) . . ?
N3 C15 H15A 110.1 . . ?
C16 C15 H15A 110.1 . . ?
N3 C15 H15B 110.1 . . ?
C16 C15 H15B 110.1 . . ?
H15A C15 H15B 108.4 . . ?
O9 C16 C17 125.8(4) . . ?
O9 C16 C15 122.1(4) . . ?
C17 C16 C15 112.1(3) . . ?
C16 C17 C18 107.7(3) . . ?
C16 C17 C20 107.4(3) . . ?
C18 C17 C20 108.5(3) . . ?
C16 C17 H17 107(3) . . ?
C18 C17 H17 110(3) . . ?
C20 C17 H17 116(3) . . ?
C19 C18 C17 110.6(3) . . ?
C19 C18 H18A 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
N3 C19 C18 108.7(3) . . ?
N3 C19 H19A 110.0 . . ?
C18 C19 H19A 110.0 . . ?
N3 C19 H19B 110.0 . . ?
C18 C19 H19B 110.0 . . ?
H19A C19 H19B 108.3 . . ?
C21 C20 C17 110.1(3) . . ?
C21 C20 H20A 109.6 . . ?
C17 C20 H20A 109.6 . . ?
C21 C20 H20B 109.6 . . ?
C17 C20 H20B 109.6 . . ?
H20A C20 H20B 108.2 . . ?
N3 C21 C20 108.6(3) . . ?
N3 C21 H21A 110.0 . . ?
C20 C21 H21A 110.0 . . ?
N3 C21 H21B 110.0 . . ?
C20 C21 H21B 110.0 . . ?
H21A C21 H21B 108.3 . . ?
C1 N1 C5 119.2(2) . . ?
C1 N1 Cr1 124.92(18) . . ?
C5 N1 Cr1 115.61(17) . . ?
C10 N2 C6 119.7(2) . . ?
C10 N2 Cr1 124.03(18) . . ?
C6 N2 Cr1 116.20(17) . . ?
C19 N3 C15 110.5(3) . . ?
C19 N3 C21 110.3(3) . . ?
C15 N3 C21 110.6(3) . . ?
C19 N3 H3N 111(3) . . ?
C15 N3 H3N 111(3) . . ?
C21 N3 H3N 103(3) . . ?
C11 O1 Cr1 114.22(16) . . ?
C12 O4 Cr1 114.18(17) . . ?
C13 O5 Cr1 112.60(16) . . ?
C14 O8 Cr1 111.17(16) . . ?
H10A O10 H10B 105(4) . . ?
O5 Cr1 O4 91.48(8) . . ?
O5 Cr1 O1 173.35(8) . . ?
O4 Cr1 O1 82.98(8) . . ?
O5 Cr1 O8 83.45(8) . . ?
O4 Cr1 O8 89.48(8) . . ?
O1 Cr1 O8 92.78(8) . . ?
O5 Cr1 N2 93.15(8) . . ?
O4 Cr1 N2 95.91(8) . . ?
O1 Cr1 N2 91.10(8) . . ?
O8 Cr1 N2 173.71(8) . . ?
O5 Cr1 N1 95.32(9) . . ?
O4 Cr1 N1 171.30(8) . . ?
O1 Cr1 N1 90.55(8) . . ?
O8 Cr1 N1 96.67(8) . . ?
N2 Cr1 N1 78.33(8) . . ?

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
N1 C1 C2 C3 0.8(5) . . . . ?
C1 C2 C3 C4 0.0(5) . . . . ?
C2 C3 C4 C5 -0.3(5) . . . . ?
C3 C4 C5 N1 -0.1(4) . . . . ?
C3 C4 C5 C6 179.7(3) . . . . ?
N1 C5 C6 N2 -2.0(3) . . . . ?
C4 C5 C6 N2 178.2(2) . . . . ?
N1 C5 C6 C7 178.6(3) . . . . ?
C4 C5 C6 C7 -1.2(4) . . . . ?
N2 C6 C7 C8 -0.4(4) . . . . ?
C5 C6 C7 C8 178.9(3) . . . . ?
C6 C7 C8 C9 0.7(5) . . . . ?
C7 C8 C9 C10 0.3(5) . . . . ?
C8 C9 C10 N2 -1.5(5) . . . . ?
O2 C11 C12 O3 10.5(4) . . . . ?
O1 C11 C12 O3 -170.6(3) . . . . ?
O2 C11 C12 O4 -168.9(3) . . . . ?
O1 C11 C12 O4 10.1(3) . . . . ?
O6 C13 C14 O7 7.6(4) . . . . ?
O5 C13 C14 O7 -172.8(3) . . . . ?
O6 C13 C14 O8 -172.1(3) . . . . ?
O5 C13 C14 O8 7.5(4) . . . . ?
N3 C15 C16 O9 -175.9(4) . . . . ?
N3 C15 C16 C17 5.1(4) . . . . ?
O9 C16 C17 C18 -124.1(4) . . . . ?
C15 C16 C17 C18 54.9(4) . . . . ?
O9 C16 C17 C20 119.3(4) . . . . ?
C15 C16 C17 C20 -61.8(4) . . . . ?
C16 C17 C18 C19 -60.7(4) . . . . ?
C20 C17 C18 C19 55.3(4) . . . . ?
C17 C18 C19 N3 5.2(4) . . . . ?
C16 C17 C20 C21 55.8(5) . . . . ?
C18 C17 C20 C21 -60.3(4) . . . . ?
C17 C20 C21 N3 3.8(6) . . . . ?
C2 C1 N1 C5 -1.2(4) . . . . ?
C2 C1 N1 Cr1 173.1(2) . . . . ?
C4 C5 N1 C1 0.8(4) . . . . ?
C6 C5 N1 C1 -178.9(2) . . . . ?
C4 C5 N1 Cr1 -174.0(2) . . . . ?
C6 C5 N1 Cr1 6.2(3) . . . . ?
C9 C10 N2 C6 1.8(4) . . . . ?
C9 C10 N2 Cr1 -175.0(2) . . . . ?
C7 C6 N2 C10 -0.8(4) . . . . ?
C5 C6 N2 C10 179.9(2) . . . . ?
C7 C6 N2 Cr1 176.2(2) . . . . ?
C5 C6 N2 Cr1 -3.1(3) . . . . ?
C18 C19 N3 C15 57.9(4) . . . . ?
C18 C19 N3 C21 -64.7(4) . . . . ?
C16 C15 N3 C19 -64.1(4) . . . . ?
C16 C15 N3 C21 58.3(4) . . . . ?
C20 C21 N3 C19 59.3(5) . . . . ?
C20 C21 N3 C15 -63.2(5) . . . . ?
O2 C11 O1 Cr1 175.4(2) . . . . ?
C12 C11 O1 Cr1 -3.5(3) . . . . ?
O3 C12 O4 Cr1 169.3(3) . . . . ?
C11 C12 O4 Cr1 -11.4(3) . . . . ?
O6 C13 O5 Cr1 -171.9(3) . . . . ?
C14 C13 O5 Cr1 8.5(3) . . . . ?
O7 C14 O8 Cr1 161.1(3) . . . . ?
C13 C14 O8 Cr1 -19.2(3) . . . . ?

_refine_diff_density_max         0.763
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.095



####################################################################### 
# 
# 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_comp2H2O
_database_code_depnum_ccdc_archive 'CCDC 2159914'
loop_
_audit_author_name
_audit_author_address
'Lidija Andros Dubraja'
;Rudjer Boskovic Institute
Croatia
;
_audit_update_record             
;
2022-03-18 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            '(H2-DABCO)[Cr(phen)(ox)2]2 x 9(H2O)'
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H8 Cr N2 O8), C6 H14 N2, 9(H2 O )'
_chemical_formula_sum            'C38 H48 Cr2 N6 O25'
_chemical_formula_weight         1092.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   10.4903(2)
_cell_length_b                   13.9080(2)
_cell_length_c                   17.7129(4)
_cell_angle_alpha                97.152(2)
_cell_angle_beta                 100.620(2)
_cell_angle_gamma                92.735(2)
_cell_volume                     2513.64(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    15902
_cell_measurement_theta_min      3.8330
_cell_measurement_theta_max      76.0330

_exptl_crystal_description       plate-like
_exptl_crystal_colour            'orange and purplish red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_F_000             1114
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    4.351
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.58125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.712
_oxdiff_exptl_absorpt_empirical_full_max 1.525
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Ruby
_diffrn_detector_area_resol_mean 10.4323
_diffrn_reflns_number            26104
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.211
_diffrn_reflns_theta_max         76.472
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             10392
_reflns_number_gt                9692
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SIR-2019 (Burla, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Mercury (2020)'
_computing_publication_material  'PLATON (Spek, 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1366P)²+0.3395P] 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_number_reflns         10392
_refine_ls_number_parameters     721
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1783
_refine_ls_wR_factor_gt          0.1737
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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
C1 C 0.8918(2) 0.14494(16) 0.93650(14) 0.0494(5) Uani 1 1 d . . . . .
H1 H 0.824886 0.152061 0.895592 0.059 Uiso 1 1 calc R U . . .
C2 C 0.8630(3) 0.14163(18) 1.01058(16) 0.0550(5) Uani 1 1 d . . . . .
H2 H 0.778529 0.148271 1.018514 0.066 Uiso 1 1 calc R U . . .
C3 C 0.9597(3) 0.12859(17) 1.07103(14) 0.0534(5) Uani 1 1 d . . . . .
H3 H 0.941401 0.126529 1.120230 0.064 Uiso 1 1 calc R U . . .
C4 C 1.0874(2) 0.11830(15) 1.05811(13) 0.0465(4) Uani 1 1 d . . . . .
C5 C 1.1951(3) 0.10285(18) 1.11657(14) 0.0555(5) Uani 1 1 d . . . . .
H5 H 1.181620 0.095766 1.166091 0.067 Uiso 1 1 calc R U . . .
C6 C 1.3176(3) 0.09833(18) 1.10083(15) 0.0559(5) Uani 1 1 d . . . . .
H6 H 1.386204 0.088438 1.139845 0.067 Uiso 1 1 calc R U . . .
C7 C 1.3416(2) 0.10850(15) 1.02578(14) 0.0481(5) Uani 1 1 d . . . . .
C8 C 1.4660(2) 0.11095(17) 1.00599(16) 0.0556(5) Uani 1 1 d . . . . .
H8 H 1.539413 0.105773 1.043331 0.067 Uiso 1 1 calc R U . . .
C9 C 1.4782(2) 0.12094(18) 0.93194(16) 0.0561(5) Uani 1 1 d . . . . .
H9 H 1.560180 0.124072 0.919009 0.067 Uiso 1 1 calc R U . . .
C10 C 1.3672(2) 0.12648(17) 0.87540(15) 0.0512(5) Uani 1 1 d . . . . .
H10 H 1.376662 0.131101 0.824763 0.061 Uiso 1 1 calc R U . . .
C11 C 1.2361(2) 0.11821(14) 0.96620(12) 0.0425(4) Uani 1 1 d . . . . .
C12 C 1.1082(2) 0.12412(14) 0.98278(12) 0.0421(4) Uani 1 1 d . . . . .
C13 C 0.5979(2) 0.65143(17) 0.85906(15) 0.0530(5) Uani 1 1 d . . . . .
H13 H 0.602473 0.658271 0.808048 0.064 Uiso 1 1 calc R U . . .
C14 C 0.7139(2) 0.64829(19) 0.91295(17) 0.0578(6) Uani 1 1 d . . . . .
H14 H 0.793698 0.652339 0.897389 0.069 Uiso 1 1 calc R U . . .
C15 C 0.7086(2) 0.63933(17) 0.98754(16) 0.0557(5) Uani 1 1 d . . . . .
H15 H 0.784978 0.638563 1.023624 0.067 Uiso 1 1 calc R U . . .
C16 C 0.5873(2) 0.63117(14) 1.01057(13) 0.0476(5) Uani 1 1 d . . . . .
C17 C 0.5717(3) 0.62034(17) 1.08785(14) 0.0569(6) Uani 1 1 d . . . . .
H17 H 0.644723 0.619360 1.126435 0.068 Uiso 1 1 calc R U . . .
C18 C 0.4522(3) 0.61156(18) 1.10515(14) 0.0596(6) Uani 1 1 d . . . . .
H18 H 0.444323 0.604927 1.155722 0.072 Uiso 1 1 calc R U . . .
C19 C 0.3377(3) 0.61221(15) 1.04770(13) 0.0501(5) Uani 1 1 d . . . . .
C20 C 0.2109(3) 0.60158(18) 1.06170(16) 0.0599(6) Uani 1 1 d . . . . .
H20 H 0.197296 0.594532 1.111200 0.072 Uiso 1 1 calc R U . . .
C21 C 0.1070(3) 0.60160(19) 1.00209(18) 0.0631(6) Uani 1 1 d . . . . .
H21 H 0.022768 0.595732 1.011335 0.076 Uiso 1 1 calc R U . . .
C22 C 0.1275(2) 0.61043(17) 0.92742(16) 0.0546(5) Uani 1 1 d . . . . .
H22 H 0.056117 0.609417 0.887397 0.066 Uiso 1 1 calc R U . . .
C23 C 0.3502(2) 0.62222(14) 0.97166(12) 0.0430(4) Uani 1 1 d . . . . .
C24 C 0.4762(2) 0.63364(13) 0.95308(12) 0.0415(4) Uani 1 1 d . . . . .
C25 C 1.0623(3) -0.03832(16) 0.73188(13) 0.0534(5) Uani 1 1 d . . . . .
C26 C 1.1266(3) 0.03370(18) 0.68870(13) 0.0563(5) Uani 1 1 d . . . . .
C27 C 1.0204(2) 0.33315(16) 0.81546(14) 0.0508(5) Uani 1 1 d . . . . .
C28 C 0.9002(3) 0.27067(19) 0.76849(14) 0.0567(5) Uani 1 1 d . . . . .
C29 C 0.1043(3) 0.53380(18) 0.70395(14) 0.0562(5) Uani 1 1 d . . . . .
C30 C 0.2126(3) 0.46504(17) 0.72443(13) 0.0539(5) Uani 1 1 d . . . . .
C31 C 0.3310(3) 0.83660(18) 0.79260(16) 0.0601(6) Uani 1 1 d . . . . .
C32 C 0.3689(4) 0.7780(2) 0.72143(19) 0.0755(8) Uani 1 1 d . . . . .
C33A C 0.9994(11) 0.3593(4) 0.4957(5) 0.080(3) Uani 0.599(11) 1 d . . P A 1
H33A H 1.077877 0.395714 0.490768 0.096 Uiso 0.599(11) 1 calc R U P A 1
H33B H 0.933293 0.404696 0.501306 0.096 Uiso 0.599(11) 1 calc R U P A 1
C34A C 0.9538(13) 0.2870(5) 0.4244(4) 0.089(3) Uani 0.599(11) 1 d . . P A 1
H34A H 0.869317 0.302423 0.398043 0.107 Uiso 0.599(11) 1 calc R U P A 1
H34B H 1.014254 0.290423 0.389328 0.107 Uiso 0.599(11) 1 calc R U P A 1
C37A C 0.9085(19) 0.2596(11) 0.5729(6) 0.147(7) Uani 0.599(11) 1 d . . P A 1
H37A H 0.843212 0.304734 0.581244 0.177 Uiso 0.599(11) 1 calc R U P A 1
H37B H 0.928149 0.225906 0.617956 0.177 Uiso 0.599(11) 1 calc R U P A 1
C38A C 0.8573(17) 0.1859(10) 0.4996(6) 0.162(8) Uani 0.599(11) 1 d . . P A 1
H38A H 0.854178 0.120479 0.513242 0.194 Uiso 0.599(11) 1 calc R U P A 1
H38B H 0.770022 0.199504 0.476301 0.194 Uiso 0.599(11) 1 calc R U P A 1
C35A C 1.1322(13) 0.2381(6) 0.5489(5) 0.114(4) Uani 0.599(11) 1 d . . P A 1
H35A H 1.209763 0.273098 0.541004 0.137 Uiso 0.599(11) 1 calc R U P A 1
H35B H 1.155240 0.205182 0.594188 0.137 Uiso 0.599(11) 1 calc R U P A 1
C36A C 1.0771(15) 0.1639(8) 0.4776(6) 0.124(4) Uani 0.599(11) 1 d . . P A 1
H36A H 1.133325 0.163605 0.439792 0.149 Uiso 0.599(11) 1 calc R U P A 1
H36B H 1.070133 0.099164 0.492205 0.149 Uiso 0.599(11) 1 calc R U P A 1
C33B C 1.080(4) 0.349(2) 0.5065(12) 0.24(2) Uani 0.401(11) 1 d . . P A 2
H33C H 1.173930 0.358002 0.523956 0.282 Uiso 0.401(11) 1 calc R U P A 2
H33D H 1.047395 0.411047 0.497754 0.282 Uiso 0.401(11) 1 calc R U P A 2
C36B C 0.848(3) 0.2606(19) 0.4447(17) 0.23(2) Uani 0.401(11) 1 d . . P A 2
H36C H 0.766250 0.226988 0.447189 0.277 Uiso 0.401(11) 1 calc R U P A 2
H36D H 0.836771 0.290131 0.397325 0.277 Uiso 0.401(11) 1 calc R U P A 2
C34B C 1.048(3) 0.2776(14) 0.4313(9) 0.140(8) Uani 0.401(11) 1 d . . P A 2
H34C H 1.126141 0.249362 0.419610 0.168 Uiso 0.401(11) 1 calc R U P A 2
H34D H 1.010400 0.310890 0.388466 0.168 Uiso 0.401(11) 1 calc R U P A 2
C35B C 0.889(4) 0.340(2) 0.5154(16) 0.23(2) Uani 0.401(11) 1 d . . P A 2
H35C H 0.823591 0.341475 0.548004 0.272 Uiso 0.401(11) 1 calc R U P A 2
H35D H 0.898304 0.403206 0.498797 0.272 Uiso 0.401(11) 1 calc R U P A 2
C38B C 1.0006(17) 0.1505(7) 0.5043(6) 0.086(4) Uani 0.401(11) 1 d . . P A 2
H38C H 1.086835 0.132465 0.498564 0.104 Uiso 0.401(11) 1 calc R U P A 2
H38D H 0.948301 0.092580 0.508276 0.104 Uiso 0.401(11) 1 calc R U P A 2
C37B C 1.008(4) 0.2290(10) 0.5788(8) 0.21(2) Uani 0.401(11) 1 d . . P A 2
H37C H 0.928468 0.223475 0.598690 0.253 Uiso 0.401(11) 1 calc R U P A 2
H37D H 1.079852 0.217318 0.618993 0.253 Uiso 0.401(11) 1 calc R U P A 2
N1 N 1.01133(18) 0.13824(12) 0.92327(10) 0.0426(4) Uani 1 1 d . . . . .
N2 N 1.24913(18) 0.12530(13) 0.89211(11) 0.0441(4) Uani 1 1 d . . . . .
N3 N 0.48211(18) 0.64493(13) 0.87891(10) 0.0442(4) Uani 1 1 d . . . . .
N4 N 0.24663(18) 0.62025(13) 0.91212(11) 0.0453(4) Uani 1 1 d . . . . .
N5 N 1.0245(5) 0.3114(2) 0.56170(15) 0.1001(12) Uani 1 1 d D . . . .
N6 N 0.9453(4) 0.1939(2) 0.44428(15) 0.0923(11) Uani 1 1 d D . . . .
O1 O 1.03015(18) 0.00173(11) 0.79442(9) 0.0513(4) Uani 1 1 d . . . . .
O2 O 1.0454(3) -0.12467(13) 0.70676(11) 0.0708(5) Uani 1 1 d . . . . .
O3 O 1.1524(3) 0.00571(16) 0.62500(12) 0.0820(7) Uani 1 1 d . . . . .
O4 O 1.14784(19) 0.12066(12) 0.72417(9) 0.0550(4) Uani 1 1 d . . . . .
O5 O 1.11430(17) 0.28228(11) 0.84125(10) 0.0526(4) Uani 1 1 d . . . . .
O6 O 1.0192(2) 0.42072(13) 0.82874(15) 0.0746(6) Uani 1 1 d . . . . .
O7 O 0.8044(3) 0.30820(19) 0.73950(18) 0.0953(8) Uani 1 1 d . . . . .
O8 O 0.90995(18) 0.17778(12) 0.76495(10) 0.0560(4) Uani 1 1 d . . . . .
O9 O 0.12444(18) 0.61850(12) 0.74517(11) 0.0578(4) Uani 1 1 d . . . . .
O10 O 0.0123(2) 0.50686(16) 0.65208(13) 0.0780(6) Uani 1 1 d . . . . .
O11 O 0.2004(2) 0.38076(14) 0.69383(12) 0.0721(6) Uani 1 1 d . . . . .
O12 O 0.31172(18) 0.50482(12) 0.77368(10) 0.0534(4) Uani 1 1 d . . . . .
O13 O 0.29044(18) 0.78215(12) 0.83852(10) 0.0548(4) Uani 1 1 d . . . . .
O14 O 0.3440(3) 0.92430(14) 0.80409(17) 0.0868(7) Uani 1 1 d . . . . .
O15 O 0.3965(6) 0.8188(3) 0.6688(2) 0.1451(18) Uani 1 1 d . . . . .
O16 O 0.3689(2) 0.68638(14) 0.72268(10) 0.0637(5) Uani 1 1 d . . . . .
O17 O 0.6163(5) 0.1707(5) 0.7889(3) 0.171(2) Uani 1 1 d . . . . .
O18 O -0.1207(4) 0.7018(4) 0.7679(3) 0.1438(16) Uani 1 1 d . . . . .
O19 O 0.7635(7) 0.5127(4) 0.7526(4) 0.190(3) Uani 1 1 d . . . . .
O20 O 0.4154(7) 0.2643(6) 0.7018(4) 0.228(4) Uani 1 1 d . . . . .
O21 O 0.8118(8) 0.0298(6) 0.6290(4) 0.218(3) Uani 1 1 d . . . . .
O22 O 0.7227(9) 0.8165(9) 0.6763(5) 0.289(5) Uani 1 1 d . . . . .
Cr1 Cr 1.07622(3) 0.14119(2) 0.81945(2) 0.04238(13) Uani 1 1 d . . . . .
Cr2 Cr 0.30035(3) 0.64296(2) 0.80888(2) 0.04395(13) Uani 1 1 d . . . . .
O23A O 0.5281(15) 0.4230(12) 0.6557(10) 0.201(7) Uani 0.420(8) 1 d . . P B 1
O24A O 0.260(2) 0.4441(15) 0.4281(11) 0.229(8) Uiso 0.420(8) 1 d . . P B 1
O25A O 0.3551(18) 0.0837(17) 0.5588(17) 0.299(14) Uani 0.420(8) 1 d . . P B 1
O23B O 0.566(6) 0.289(3) 0.538(3) 0.65(3) Uiso 0.580(8) 1 d . . P B 2
O24B O 0.3111(13) 0.5435(8) 0.5795(5) 0.187(5) Uani 0.580(8) 1 d . . P B 2
O25B O 0.516(2) 0.0098(10) 0.7001(11) 0.351(13) Uani 0.580(8) 1 d . . P B 2
H6N H 0.924(6) 0.157(4) 0.4008(19) 0.131(19) Uiso 1 1 d D . . . .
H5N H 1.052(4) 0.351(3) 0.6057(17) 0.098(13) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.323(3) . ?
C1 C2 1.405(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.369(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.411(4) . ?
C3 H3 0.9300 . ?
C4 C12 1.402(3) . ?
C4 C5 1.429(3) . ?
C5 C6 1.367(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.420(4) . ?
C6 H6 0.9300 . ?
C7 C11 1.406(3) . ?
C7 C8 1.413(4) . ?
C8 C9 1.365(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.401(4) . ?
C9 H9 0.9300 . ?
C10 N2 1.326(3) . ?
C10 H10 0.9300 . ?
C11 N2 1.359(3) . ?
C11 C12 1.429(3) . ?
C12 N1 1.363(3) . ?
C13 N3 1.327(3) . ?
C13 C14 1.408(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.353(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.410(4) . ?
C15 H15 0.9300 . ?
C16 C24 1.404(3) . ?
C16 C17 1.434(4) . ?
C17 C18 1.347(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.426(4) . ?
C18 H18 0.9300 . ?
C19 C23 1.400(3) . ?
C19 C20 1.402(4) . ?
C20 C21 1.370(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.398(4) . ?
C21 H21 0.9300 . ?
C22 N4 1.331(3) . ?
C22 H22 0.9300 . ?
C23 N4 1.364(3) . ?
C23 C24 1.426(3) . ?
C24 N3 1.355(3) . ?
C25 O2 1.220(3) . ?
C25 O1 1.286(3) . ?
C25 C26 1.536(3) . ?
C26 O3 1.229(3) . ?
C26 O4 1.281(3) . ?
C27 O6 1.213(3) . ?
C27 O5 1.288(3) . ?
C27 C28 1.538(4) . ?
C28 O7 1.214(4) . ?
C28 O8 1.295(3) . ?
C29 O10 1.212(3) . ?
C29 O9 1.293(3) . ?
C29 C30 1.541(4) . ?
C30 O11 1.219(3) . ?
C30 O12 1.280(3) . ?
C31 O14 1.208(3) . ?
C31 O13 1.291(3) . ?
C31 C32 1.540(4) . ?
C32 O15 1.220(4) . ?
C32 O16 1.278(4) . ?
C33A N5 1.406(8) . ?
C33A C34A 1.500(10) . ?
C33A H33A 0.9700 . ?
C33A H33B 0.9700 . ?
C34A N6 1.387(8) . ?
C34A H34A 0.9700 . ?
C34A H34B 0.9700 . ?
C37A N5 1.442(16) . ?
C37A C38A 1.544(13) . ?
C37A H37A 0.9700 . ?
C37A H37B 0.9700 . ?
C38A N6 1.475(11) . ?
C38A H38A 0.9700 . ?
C38A H38B 0.9700 . ?
C35A C36A 1.532(10) . ?
C35A N5 1.585(11) . ?
C35A H35A 0.9700 . ?
C35A H35B 0.9700 . ?
C36A N6 1.500(12) . ?
C36A H36A 0.9700 . ?
C36A H36B 0.9700 . ?
C33B N5 1.37(2) . ?
C33B C34B 1.53(2) . ?
C33B H33C 0.9700 . ?
C33B H33D 0.9700 . ?
C36B N6 1.41(2) . ?
C36B C35B 1.543(19) . ?
C36B H36C 0.9700 . ?
C36B H36D 0.9700 . ?
C34B N6 1.62(2) . ?
C34B H34C 0.9700 . ?
C34B H34D 0.9700 . ?
C35B N5 1.60(2) . ?
C35B H35C 0.9700 . ?
C35B H35D 0.9700 . ?
C38B N6 1.341(10) . ?
C38B C37B 1.59(2) . ?
C38B H38C 0.9700 . ?
C38B H38D 0.9700 . ?
C37B N5 1.232(14) . ?
C37B H37C 0.9700 . ?
C37B H37D 0.9700 . ?
N1 Cr1 2.0795(18) . ?
N2 Cr1 2.0601(19) . ?
N3 Cr2 2.0711(19) . ?
N4 Cr2 2.066(2) . ?
N5 H5N 0.890(19) . ?
N6 H6N 0.85(2) . ?
O1 Cr1 1.9518(16) . ?
O4 Cr1 1.9653(17) . ?
O5 Cr1 1.9594(16) . ?
O8 Cr1 1.9545(18) . ?
O9 Cr2 1.9676(17) . ?
O12 Cr2 1.9609(16) . ?
O13 Cr2 1.9546(16) . ?
O16 Cr2 1.9510(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 121.9(2) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C3 C2 C1 119.8(2) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 119.5(2) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C12 C4 C3 117.0(2) . . ?
C12 C4 C5 118.8(2) . . ?
C3 C4 C5 124.2(2) . . ?
C6 C5 C4 121.0(2) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C7 121.0(2) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C11 C7 C8 116.4(2) . . ?
C11 C7 C6 119.0(2) . . ?
C8 C7 C6 124.6(2) . . ?
C9 C8 C7 119.8(2) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 120.0(2) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
N2 C10 C9 121.8(2) . . ?
N2 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
N2 C11 C7 123.2(2) . . ?
N2 C11 C12 116.83(19) . . ?
C7 C11 C12 120.0(2) . . ?
N1 C12 C4 122.9(2) . . ?
N1 C12 C11 117.00(19) . . ?
C4 C12 C11 120.1(2) . . ?
N3 C13 C14 121.9(2) . . ?
N3 C13 H13 119.0 . . ?
C14 C13 H13 119.0 . . ?
C15 C14 C13 119.6(2) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 120.0(2) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C24 C16 C15 116.8(2) . . ?
C24 C16 C17 119.1(2) . . ?
C15 C16 C17 124.1(2) . . ?
C18 C17 C16 120.7(2) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 121.5(2) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C23 C19 C20 116.8(2) . . ?
C23 C19 C18 119.0(2) . . ?
C20 C19 C18 124.2(2) . . ?
C21 C20 C19 119.7(2) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C20 C21 C22 120.1(2) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
N4 C22 C21 121.7(2) . . ?
N4 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
N4 C23 C19 123.4(2) . . ?
N4 C23 C24 116.65(19) . . ?
C19 C23 C24 120.0(2) . . ?
N3 C24 C16 123.0(2) . . ?
N3 C24 C23 117.27(19) . . ?
C16 C24 C23 119.8(2) . . ?
O2 C25 O1 125.5(2) . . ?
O2 C25 C26 120.9(2) . . ?
O1 C25 C26 113.54(19) . . ?
O3 C26 O4 125.5(2) . . ?
O3 C26 C25 119.8(2) . . ?
O4 C26 C25 114.7(2) . . ?
O6 C27 O5 125.8(2) . . ?
O6 C27 C28 121.0(2) . . ?
O5 C27 C28 113.03(19) . . ?
O7 C28 O8 124.4(3) . . ?
O7 C28 C27 120.8(2) . . ?
O8 C28 C27 114.7(2) . . ?
O10 C29 O9 126.1(2) . . ?
O10 C29 C30 119.9(2) . . ?
O9 C29 C30 114.0(2) . . ?
O11 C30 O12 125.4(2) . . ?
O11 C30 C29 120.3(2) . . ?
O12 C30 C29 114.3(2) . . ?
O14 C31 O13 125.0(3) . . ?
O14 C31 C32 122.0(3) . . ?
O13 C31 C32 112.9(2) . . ?
O15 C32 O16 124.2(3) . . ?
O15 C32 C31 120.7(3) . . ?
O16 C32 C31 115.1(2) . . ?
N5 C33A C34A 110.2(5) . . ?
N5 C33A H33A 109.6 . . ?
C34A C33A H33A 109.6 . . ?
N5 C33A H33B 109.6 . . ?
C34A C33A H33B 109.6 . . ?
H33A C33A H33B 108.1 . . ?
N6 C34A C33A 110.2(5) . . ?
N6 C34A H34A 109.6 . . ?
C33A C34A H34A 109.6 . . ?
N6 C34A H34B 109.6 . . ?
C33A C34A H34B 109.6 . . ?
H34A C34A H34B 108.1 . . ?
N5 C37A C38A 108.2(8) . . ?
N5 C37A H37A 110.1 . . ?
C38A C37A H37A 110.1 . . ?
N5 C37A H37B 110.1 . . ?
C38A C37A H37B 110.1 . . ?
H37A C37A H37B 108.4 . . ?
N6 C38A C37A 108.6(8) . . ?
N6 C38A H38A 110.0 . . ?
C37A C38A H38A 110.0 . . ?
N6 C38A H38B 110.0 . . ?
C37A C38A H38B 110.0 . . ?
H38A C38A H38B 108.4 . . ?
C36A C35A N5 108.3(7) . . ?
C36A C35A H35A 110.0 . . ?
N5 C35A H35A 110.0 . . ?
C36A C35A H35B 110.0 . . ?
N5 C35A H35B 110.0 . . ?
H35A C35A H35B 108.4 . . ?
N6 C36A C35A 106.8(6) . . ?
N6 C36A H36A 110.4 . . ?
C35A C36A H36A 110.4 . . ?
N6 C36A H36B 110.4 . . ?
C35A C36A H36B 110.4 . . ?
H36A C36A H36B 108.6 . . ?
N5 C33B C34B 108.8(14) . . ?
N5 C33B H33C 109.9 . . ?
C34B C33B H33C 109.9 . . ?
N5 C33B H33D 109.9 . . ?
C34B C33B H33D 109.9 . . ?
H33C C33B H33D 108.3 . . ?
N6 C36B C35B 109.5(14) . . ?
N6 C36B H36C 109.8 . . ?
C35B C36B H36C 109.8 . . ?
N6 C36B H36D 109.8 . . ?
C35B C36B H36D 109.8 . . ?
H36C C36B H36D 108.2 . . ?
C33B C34B N6 107.1(13) . . ?
C33B C34B H34C 110.3 . . ?
N6 C34B H34C 110.3 . . ?
C33B C34B H34D 110.3 . . ?
N6 C34B H34D 110.3 . . ?
H34C C34B H34D 108.6 . . ?
C36B C35B N5 106.0(13) . . ?
C36B C35B H35C 110.5 . . ?
N5 C35B H35C 110.5 . . ?
C36B C35B H35D 110.5 . . ?
N5 C35B H35D 110.5 . . ?
H35C C35B H35D 108.7 . . ?
N6 C38B C37B 105.2(10) . . ?
N6 C38B H38C 110.7 . . ?
C37B C38B H38C 110.7 . . ?
N6 C38B H38D 110.7 . . ?
C37B C38B H38D 110.7 . . ?
H38C C38B H38D 108.8 . . ?
N5 C37B C38B 109.9(13) . . ?
N5 C37B H37C 109.7 . . ?
C38B C37B H37C 109.7 . . ?
N5 C37B H37D 109.7 . . ?
C38B C37B H37D 109.7 . . ?
H37C C37B H37D 108.2 . . ?
C1 N1 C12 118.79(19) . . ?
C1 N1 Cr1 128.59(16) . . ?
C12 N1 Cr1 112.58(14) . . ?
C10 N2 C11 118.8(2) . . ?
C10 N2 Cr1 127.67(16) . . ?
C11 N2 Cr1 113.48(14) . . ?
C13 N3 C24 118.6(2) . . ?
C13 N3 Cr2 128.34(16) . . ?
C24 N3 Cr2 112.95(14) . . ?
C22 N4 C23 118.3(2) . . ?
C22 N4 Cr2 128.50(18) . . ?
C23 N4 Cr2 113.04(15) . . ?
C37B N5 C33B 134(2) . . ?
C33A N5 C37A 111.2(8) . . ?
C33A N5 C35A 107.2(6) . . ?
C37A N5 C35A 110.3(8) . . ?
C37B N5 C35B 108(2) . . ?
C33B N5 C35B 86.7(19) . . ?
C37B N5 H5N 107(3) . . ?
C33B N5 H5N 106(3) . . ?
C33A N5 H5N 114(3) . . ?
C37A N5 H5N 105(3) . . ?
C35A N5 H5N 109(3) . . ?
C35B N5 H5N 112(3) . . ?
C38B N6 C36B 126.4(16) . . ?
C34A N6 C38A 111.6(8) . . ?
C34A N6 C36A 110.9(8) . . ?
C38A N6 C36A 109.9(9) . . ?
C38B N6 C34B 108.3(11) . . ?
C36B N6 C34B 90.7(18) . . ?
C38B N6 H6N 116(4) . . ?
C34A N6 H6N 104(4) . . ?
C36B N6 H6N 106(4) . . ?
C38A N6 H6N 117(4) . . ?
C36A N6 H6N 103(4) . . ?
C34B N6 H6N 105(4) . . ?
C25 O1 Cr1 114.92(14) . . ?
C26 O4 Cr1 113.89(15) . . ?
C27 O5 Cr1 115.29(15) . . ?
C28 O8 Cr1 114.21(16) . . ?
C29 O9 Cr2 113.61(16) . . ?
C30 O12 Cr2 114.44(15) . . ?
C31 O13 Cr2 114.57(16) . . ?
C32 O16 Cr2 113.8(2) . . ?
O1 Cr1 O8 94.50(8) . . ?
O1 Cr1 O5 177.14(7) . . ?
O8 Cr1 O5 82.66(7) . . ?
O1 Cr1 O4 82.67(7) . . ?
O8 Cr1 O4 93.06(8) . . ?
O5 Cr1 O4 97.16(7) . . ?
O1 Cr1 N2 94.20(7) . . ?
O8 Cr1 N2 169.04(7) . . ?
O5 Cr1 N2 88.66(7) . . ?
O4 Cr1 N2 94.65(8) . . ?
O1 Cr1 N1 88.88(7) . . ?
O8 Cr1 N1 93.48(8) . . ?
O5 Cr1 N1 91.57(7) . . ?
O4 Cr1 N1 169.69(7) . . ?
N2 Cr1 N1 80.04(7) . . ?
O16 Cr2 O13 83.09(8) . . ?
O16 Cr2 O12 93.93(8) . . ?
O13 Cr2 O12 176.94(7) . . ?
O16 Cr2 O9 91.41(9) . . ?
O13 Cr2 O9 96.56(7) . . ?
O12 Cr2 O9 82.76(7) . . ?
O16 Cr2 N4 169.23(8) . . ?
O13 Cr2 N4 88.19(8) . . ?
O12 Cr2 N4 94.85(7) . . ?
O9 Cr2 N4 95.86(8) . . ?
O16 Cr2 N3 93.94(9) . . ?
O13 Cr2 N3 91.86(7) . . ?
O12 Cr2 N3 89.06(7) . . ?
O9 Cr2 N3 170.52(7) . . ?
N4 Cr2 N3 79.99(7) . . ?

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
N1 C1 C2 C3 -1.7(4) . . . . ?
C1 C2 C3 C4 -0.2(4) . . . . ?
C2 C3 C4 C12 1.2(3) . . . . ?
C2 C3 C4 C5 -179.0(2) . . . . ?
C12 C4 C5 C6 3.1(4) . . . . ?
C3 C4 C5 C6 -176.7(2) . . . . ?
C4 C5 C6 C7 -0.2(4) . . . . ?
C5 C6 C7 C11 -3.4(3) . . . . ?
C5 C6 C7 C8 175.8(2) . . . . ?
C11 C7 C8 C9 -0.9(3) . . . . ?
C6 C7 C8 C9 180.0(2) . . . . ?
C7 C8 C9 C10 -1.5(4) . . . . ?
C8 C9 C10 N2 2.1(4) . . . . ?
C8 C7 C11 N2 2.9(3) . . . . ?
C6 C7 C11 N2 -177.90(19) . . . . ?
C8 C7 C11 C12 -175.12(19) . . . . ?
C6 C7 C11 C12 4.1(3) . . . . ?
C3 C4 C12 N1 -0.5(3) . . . . ?
C5 C4 C12 N1 179.68(19) . . . . ?
C3 C4 C12 C11 177.51(19) . . . . ?
C5 C4 C12 C11 -2.3(3) . . . . ?
N2 C11 C12 N1 -1.3(3) . . . . ?
C7 C11 C12 N1 176.88(18) . . . . ?
N2 C11 C12 C4 -179.40(18) . . . . ?
C7 C11 C12 C4 -1.3(3) . . . . ?
N3 C13 C14 C15 -0.7(4) . . . . ?
C13 C14 C15 C16 1.3(4) . . . . ?
C14 C15 C16 C24 -0.5(3) . . . . ?
C14 C15 C16 C17 179.3(2) . . . . ?
C24 C16 C17 C18 0.7(3) . . . . ?
C15 C16 C17 C18 -179.0(2) . . . . ?
C16 C17 C18 C19 0.3(4) . . . . ?
C17 C18 C19 C23 0.0(4) . . . . ?
C17 C18 C19 C20 178.8(2) . . . . ?
C23 C19 C20 C21 -0.1(3) . . . . ?
C18 C19 C20 C21 -178.9(2) . . . . ?
C19 C20 C21 C22 1.2(4) . . . . ?
C20 C21 C22 N4 -0.9(4) . . . . ?
C20 C19 C23 N4 -1.2(3) . . . . ?
C18 C19 C23 N4 177.6(2) . . . . ?
C20 C19 C23 C24 179.82(19) . . . . ?
C18 C19 C23 C24 -1.3(3) . . . . ?
C15 C16 C24 N3 -1.1(3) . . . . ?
C17 C16 C24 N3 179.10(19) . . . . ?
C15 C16 C24 C23 177.73(18) . . . . ?
C17 C16 C24 C23 -2.0(3) . . . . ?
N4 C23 C24 N3 2.3(3) . . . . ?
C19 C23 C24 N3 -178.71(18) . . . . ?
N4 C23 C24 C16 -176.66(18) . . . . ?
C19 C23 C24 C16 2.4(3) . . . . ?
O2 C25 C26 O3 5.6(4) . . . . ?
O1 C25 C26 O3 -174.3(3) . . . . ?
O2 C25 C26 O4 -174.8(3) . . . . ?
O1 C25 C26 O4 5.3(3) . . . . ?
O6 C27 C28 O7 4.7(4) . . . . ?
O5 C27 C28 O7 -179.0(3) . . . . ?
O6 C27 C28 O8 -173.5(2) . . . . ?
O5 C27 C28 O8 2.7(3) . . . . ?
O10 C29 C30 O11 -6.9(4) . . . . ?
O9 C29 C30 O11 174.4(3) . . . . ?
O10 C29 C30 O12 172.3(3) . . . . ?
O9 C29 C30 O12 -6.4(3) . . . . ?
O14 C31 C32 O15 -10.2(6) . . . . ?
O13 C31 C32 O15 172.5(4) . . . . ?
O14 C31 C32 O16 169.7(3) . . . . ?
O13 C31 C32 O16 -7.5(4) . . . . ?
N5 C33A C34A N6 2.0(14) . . . . ?
N5 C37A C38A N6 0(2) . . . . ?
N5 C35A C36A N6 3.8(13) . . . . ?
N5 C33B C34B N6 7(4) . . . . ?
N6 C36B C35B N5 -2(5) . . . . ?
N6 C38B C37B N5 -33(3) . . . . ?
C2 C1 N1 C12 2.5(3) . . . . ?
C2 C1 N1 Cr1 179.94(17) . . . . ?
C4 C12 N1 C1 -1.3(3) . . . . ?
C11 C12 N1 C1 -179.41(18) . . . . ?
C4 C12 N1 Cr1 -179.20(16) . . . . ?
C11 C12 N1 Cr1 2.7(2) . . . . ?
C9 C10 N2 C11 -0.2(3) . . . . ?
C9 C10 N2 Cr1 175.85(17) . . . . ?
C7 C11 N2 C10 -2.4(3) . . . . ?
C12 C11 N2 C10 175.71(19) . . . . ?
C7 C11 N2 Cr1 -178.97(15) . . . . ?
C12 C11 N2 Cr1 -0.9(2) . . . . ?
C14 C13 N3 C24 -0.9(3) . . . . ?
C14 C13 N3 Cr2 -177.60(17) . . . . ?
C16 C24 N3 C13 1.8(3) . . . . ?
C23 C24 N3 C13 -177.08(19) . . . . ?
C16 C24 N3 Cr2 179.00(15) . . . . ?
C23 C24 N3 Cr2 0.1(2) . . . . ?
C21 C22 N4 C23 -0.4(3) . . . . ?
C21 C22 N4 Cr2 -175.78(18) . . . . ?
C19 C23 N4 C22 1.5(3) . . . . ?
C24 C23 N4 C22 -179.50(19) . . . . ?
C19 C23 N4 Cr2 177.57(15) . . . . ?
C24 C23 N4 Cr2 -3.4(2) . . . . ?
C38B C37B N5 C33B -27(4) . . . . ?
C38B C37B N5 C35B 76(3) . . . . ?
C34B C33B N5 C37B 38(5) . . . . ?
C34B C33B N5 C35B -74(3) . . . . ?
C34A C33A N5 C37A -61.7(11) . . . . ?
C34A C33A N5 C35A 59.0(11) . . . . ?
C38A C37A N5 C33A 58.5(15) . . . . ?
C38A C37A N5 C35A -60.3(15) . . . . ?
C36A C35A N5 C33A -62.0(11) . . . . ?
C36A C35A N5 C37A 59.2(10) . . . . ?
C36B C35B N5 C37B -58(3) . . . . ?
C36B C35B N5 C33B 78(3) . . . . ?
C37B C38B N6 C36B -35(3) . . . . ?
C37B C38B N6 C34B 70.4(19) . . . . ?
C33A C34A N6 C38A 57.5(11) . . . . ?
C33A C34A N6 C36A -65.3(11) . . . . ?
C35B C36B N6 C38B 49(4) . . . . ?
C35B C36B N6 C34B -65(3) . . . . ?
C37A C38A N6 C34A -58.6(15) . . . . ?
C37A C38A N6 C36A 64.8(15) . . . . ?
C35A C36A N6 C34A 58.9(11) . . . . ?
C35A C36A N6 C38A -64.9(11) . . . . ?
C33B C34B N6 C38B -59(3) . . . . ?
C33B C34B N6 C36B 70(2) . . . . ?
O2 C25 O1 Cr1 178.1(2) . . . . ?
C26 C25 O1 Cr1 -1.9(3) . . . . ?
O3 C26 O4 Cr1 173.7(3) . . . . ?
C25 C26 O4 Cr1 -5.9(3) . . . . ?
O6 C27 O5 Cr1 172.7(2) . . . . ?
C28 C27 O5 Cr1 -3.4(2) . . . . ?
O7 C28 O8 Cr1 -178.9(3) . . . . ?
C27 C28 O8 Cr1 -0.7(3) . . . . ?
O10 C29 O9 Cr2 -168.4(3) . . . . ?
C30 C29 O9 Cr2 10.2(3) . . . . ?
O11 C30 O12 Cr2 178.4(2) . . . . ?
C29 C30 O12 Cr2 -0.8(3) . . . . ?
O14 C31 O13 Cr2 -173.0(3) . . . . ?
C32 C31 O13 Cr2 4.1(3) . . . . ?
O15 C32 O16 Cr2 -173.0(4) . . . . ?
C31 C32 O16 Cr2 7.0(4) . . . . ?

_refine_diff_density_max         1.062
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.082



# start Validation Reply Form
_vrf_PLAT043_comp2H2O            
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      18.13 Check 
RESPONSE: Alert is related to the undetermined positions of hydrogen 
atoms in water molecules.
;
_vrf_PLAT250_comp2H2O            
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        5.6 Note  
RESPONSE: Large U3/U1 Ratio is related to the disordered DABCO molecule.
;
_vrf_PLAT260_comp2H2O            
;
PROBLEM: Large Average Ueq of Residue Including      O25B      0.350 Check 
RESPONSE: Alert is related to the disordered water molecule of crystallization.
;
_vrf_PLAT306_comp2H2O            
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O17 Check 
RESPONSE: This is related to the undetermined positions of hydrogen 
atoms in water molecules.
;
_vrf_PLAT430_comp2H2O            
;
PROBLEM: Short Inter D...A Contact  O3       ..O25A     .       2.84 Ang.  
RESPONSE: This is related to the undetermined positions of hydrogen 
atoms in water molecules.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4-400K
_database_code_depnum_ccdc_archive 'CCDC 2159919'
loop_
_audit_author_name
_audit_author_address
'Lidija Andros Dubraja'
;Rudjer Boskovic Institute
Croatia
;
_audit_update_record             
;
2022-03-18 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            '[H-(O)ABCO][Cr(bpy)(ox)2]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H8 Cr N2 O8, C7 H12 N O'
_chemical_formula_sum            'C21 H20 Cr N3 O9'
_chemical_formula_weight         510.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   15.875(2)
_cell_length_b                   10.3250(19)
_cell_length_c                   14.072(2)
_cell_angle_alpha                90
_cell_angle_beta                 112.220(17)
_cell_angle_gamma                90
_cell_volume                     2135.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    399.98(19)
_cell_measurement_reflns_used    3969
_cell_measurement_theta_min      5.2950
_cell_measurement_theta_max      75.7440

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_F_000             1052
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    4.956
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.63350
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.241
_oxdiff_exptl_absorpt_empirical_full_max 4.099
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      399(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_ambient_environment      air
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            9496
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_av_R_equivalents  0.1069
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         5.236
_diffrn_reflns_theta_max         78.668
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measured_fraction_theta_full 0.915
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_Laue_measured_fraction_full 0.915
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_point_group_measured_fraction_full 0.915
_reflns_number_total             3778
_reflns_number_gt                2477
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SIR-2019 (Burla, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Mercury (2020)'
_computing_publication_material  'PLATON (Spek, 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0827P)²+19.0524P] 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_number_reflns         3778
_refine_ls_number_parameters     333
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.2094
_refine_ls_R_factor_gt           0.1564
_refine_ls_wR_factor_ref         0.3565
_refine_ls_wR_factor_gt          0.3230
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_restrained_S_all      1.152
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3988(10) 0.1008(17) 0.2019(10) 0.093(4) Uani 1 1 d . . . . .
H1 H 0.371943 0.171130 0.160162 0.112 Uiso 1 1 calc R U . . .
C2 C 0.4628(11) 0.030(2) 0.1799(13) 0.107(5) Uani 1 1 d . . . . .
H2 H 0.478051 0.048501 0.123769 0.128 Uiso 1 1 calc R U . . .
C3 C 0.5029(12) -0.072(2) 0.2463(16) 0.112(6) Uani 1 1 d . . . . .
H3 H 0.549302 -0.118404 0.237045 0.135 Uiso 1 1 calc R U . . .
C4 C 0.4771(11) -0.1044(18) 0.3238(14) 0.105(5) Uani 1 1 d . . . . .
H4 H 0.501311 -0.176756 0.364250 0.126 Uiso 1 1 calc R U . . .
C5 C 0.4117(7) -0.0248(13) 0.3417(10) 0.071(3) Uani 1 1 d . . . . .
C6 C 0.3775(8) -0.0502(14) 0.4223(10) 0.078(4) Uani 1 1 d . . . . .
C7 C 0.3964(11) -0.1574(15) 0.4858(12) 0.096(5) Uani 1 1 d . . . . .
H7 H 0.434286 -0.222890 0.479670 0.115 Uiso 1 1 calc R U . . .
C8 C 0.3592(12) -0.1648(16) 0.5561(13) 0.104(5) Uani 1 1 d . . . . .
H8 H 0.369880 -0.237553 0.597945 0.125 Uiso 1 1 calc R U . . .
C9 C 0.3046(11) -0.0655(18) 0.5679(12) 0.102(5) Uani 1 1 d . . . . .
H9 H 0.281035 -0.069326 0.619094 0.123 Uiso 1 1 calc R U . . .
C10 C 0.2865(9) 0.0383(15) 0.5020(11) 0.087(4) Uani 1 1 d . . . . .
H10 H 0.248151 0.103332 0.507755 0.105 Uiso 1 1 calc R U . . .
C11 C 0.3494(10) 0.416(2) 0.4177(12) 0.098(5) Uani 1 1 d . . . . .
C12 C 0.2578(10) 0.3974(19) 0.4297(11) 0.089(4) Uani 1 1 d . . . . .
C13 C 0.1251(9) 0.1557(15) 0.1547(11) 0.082(4) Uani 1 1 d . . . . .
C14 C 0.1690(8) 0.2817(13) 0.1369(10) 0.074(3) Uani 1 1 d . . . . .
C15 C 0.0078(10) -0.1660(15) 0.1664(13) 0.098(5) Uani 1 1 d . . . . .
H15A H -0.052371 -0.188967 0.163587 0.118 Uiso 1 1 calc R U . . .
H15B H 0.006793 -0.076510 0.144908 0.118 Uiso 1 1 calc R U . . .
C16 C 0.0787(11) -0.1850(19) 0.2747(15) 0.102(5) Uani 1 1 d D . . . .
C17 C 0.1550(11) -0.2737(15) 0.2776(12) 0.096(5) Uani 1 1 d . . . . .
H17 H 0.201288 -0.281168 0.347160 0.116 Uiso 1 1 calc R U . . .
C18 C 0.1938(12) -0.2247(19) 0.2053(13) 0.102(5) Uani 1 1 d D . . . .
C19 C 0.1234(11) -0.2091(18) 0.0955(12) 0.107(5) Uani 1 1 d . . . . .
H19A H 0.119422 -0.119424 0.073771 0.128 Uiso 1 1 calc R U . . .
H19B H 0.139612 -0.261935 0.048004 0.128 Uiso 1 1 calc R U . . .
C20 C 0.1097(13) -0.4076(19) 0.2362(15) 0.145(8) Uani 1 1 d . . . . .
H20A H 0.155942 -0.469001 0.236302 0.174 Uiso 1 1 calc R U . . .
H20B H 0.080835 -0.440949 0.280950 0.174 Uiso 1 1 calc R U . . .
C21 C 0.0400(14) -0.3936(15) 0.1294(16) 0.164(10) Uani 1 1 d . . . . .
H21A H -0.018996 -0.422359 0.126784 0.197 Uiso 1 1 calc R U . . .
H21B H 0.056842 -0.446100 0.082150 0.197 Uiso 1 1 calc R U . . .
N1 N 0.3737(6) 0.0744(12) 0.2790(8) 0.076(3) Uani 1 1 d . . . . .
N2 N 0.3216(7) 0.0493(11) 0.4308(7) 0.072(3) Uani 1 1 d . . . . .
N3 N 0.0357(9) -0.2529(13) 0.0995(11) 0.102(4) Uani 1 1 d . . . . .
O1 O 0.1755(5) 0.0948(9) 0.2379(7) 0.082(3) Uani 1 1 d . . . . .
O2 O 0.0513(6) 0.1204(10) 0.0976(8) 0.101(3) Uani 1 1 d . . . . .
O3 O 0.1270(6) 0.3500(9) 0.0616(7) 0.089(3) Uani 1 1 d . . . . .
O4 O 0.2486(5) 0.3042(9) 0.2016(6) 0.084(3) Uani 1 1 d . . . . .
O5 O 0.3820(6) 0.3122(11) 0.3958(7) 0.084(3) Uani 1 1 d . . . . .
O6 O 0.3841(9) 0.5216(14) 0.4311(10) 0.132(4) Uani 1 1 d . . . . .
O7 O 0.2276(9) 0.4715(14) 0.4761(9) 0.135(5) Uani 1 1 d . . . . .
O8 O 0.2180(6) 0.2911(10) 0.3858(7) 0.084(3) Uani 1 1 d . . . . .
Cr1 Cr 0.28602(12) 0.1904(2) 0.32227(16) 0.0692(7) Uani 1 1 d . . . . .
O9A O 0.271(2) -0.202(3) 0.219(2) 0.108(15) Uani 0.34(3) 1 d . . P A 1
O9B O 0.0721(17) -0.131(2) 0.3493(19) 0.143(10) Uani 0.66(3) 1 d . . P A 2
H16A H 0.06(4) -0.19(5) 0.33(3) 0.172 Uiso 0.34(3) 1 d D U P A 1
H16B H 0.09(4) -0.094(13) 0.26(4) 0.172 Uiso 0.34(3) 1 d D U P A 1
H18A H 0.215(17) -0.142(14) 0.24(2) 0.172 Uiso 0.66(3) 1 d D U P A 2
H18B H 0.238(15) -0.26(3) 0.18(2) 0.172 Uiso 0.66(3) 1 d D U P A 2
H4N H -0.005(7) -0.255(9) 0.039(7) 0.04(3) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.317(16) . ?
C1 C2 1.38(2) . ?
C1 H1 0.9300 . ?
C2 C3 1.39(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.34(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.419(19) . ?
C4 H4 0.9300 . ?
C5 N1 1.337(16) . ?
C5 C6 1.455(18) . ?
C6 C7 1.383(18) . ?
C6 N2 1.391(16) . ?
C7 C8 1.33(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.39(2) . ?
C8 H8 0.9300 . ?
C9 C10 1.37(2) . ?
C9 H9 0.9300 . ?
C10 N2 1.324(16) . ?
C10 H10 0.9300 . ?
C11 O6 1.201(19) . ?
C11 O5 1.28(2) . ?
C11 C12 1.54(2) . ?
C12 O7 1.217(17) . ?
C12 O8 1.300(18) . ?
C13 O2 1.201(14) . ?
C13 O1 1.303(15) . ?
C13 C14 1.540(19) . ?
C14 O3 1.236(14) . ?
C14 O4 1.269(14) . ?
C15 N3 1.484(19) . ?
C15 C16 1.53(2) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 O9B 1.23(2) . ?
C16 C17 1.51(2) . ?
C16 H16A 0.97(2) . ?
C16 H16B 0.97(2) . ?
C17 C18 1.46(2) . ?
C17 C20 1.57(2) . ?
C17 H17 0.9800 . ?
C18 O9A 1.19(3) . ?
C18 C19 1.53(2) . ?
C18 H18A 0.97(2) . ?
C18 H18B 0.97(2) . ?
C19 N3 1.485(19) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.50(2) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 N3 1.51(2) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
N1 Cr1 2.094(10) . ?
N2 Cr1 2.030(10) . ?
N3 H4N 0.85(10) . ?
O1 Cr1 1.972(8) . ?
O4 Cr1 1.964(8) . ?
O5 Cr1 1.944(9) . ?
O8 Cr1 1.944(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.5(16) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 116.1(16) . . ?
C1 C2 H2 122.0 . . ?
C3 C2 H2 122.0 . . ?
C4 C3 C2 122.2(17) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C3 C4 C5 117.8(17) . . ?
C3 C4 H4 121.1 . . ?
C5 C4 H4 121.1 . . ?
N1 C5 C4 120.3(13) . . ?
N1 C5 C6 116.4(11) . . ?
C4 C5 C6 123.2(14) . . ?
C7 C6 N2 121.7(13) . . ?
C7 C6 C5 126.5(14) . . ?
N2 C6 C5 111.8(12) . . ?
C8 C7 C6 118.5(15) . . ?
C8 C7 H7 120.8 . . ?
C6 C7 H7 120.8 . . ?
C7 C8 C9 121.2(15) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C10 C9 C8 118.3(15) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
N2 C10 C9 122.5(14) . . ?
N2 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
O6 C11 O5 126.5(17) . . ?
O6 C11 C12 120(2) . . ?
O5 C11 C12 113.9(15) . . ?
O7 C12 O8 124.5(16) . . ?
O7 C12 C11 124.0(19) . . ?
O8 C12 C11 111.5(15) . . ?
O2 C13 O1 124.5(14) . . ?
O2 C13 C14 122.3(13) . . ?
O1 C13 C14 113.1(11) . . ?
O3 C14 O4 125.4(12) . . ?
O3 C14 C13 119.4(11) . . ?
O4 C14 C13 115.3(11) . . ?
N3 C15 C16 105.7(13) . . ?
N3 C15 H15A 110.6 . . ?
C16 C15 H15A 110.6 . . ?
N3 C15 H15B 110.6 . . ?
C16 C15 H15B 110.6 . . ?
H15A C15 H15B 108.7 . . ?
O9B C16 C17 125.5(19) . . ?
O9B C16 C15 121.7(19) . . ?
C17 C16 C15 112.8(15) . . ?
C17 C16 H16A 116(10) . . ?
C15 C16 H16A 119(10) . . ?
C17 C16 H16B 115(10) . . ?
C15 C16 H16B 80(10) . . ?
H16A C16 H16B 109(5) . . ?
C18 C17 C16 108.4(14) . . ?
C18 C17 C20 107.6(15) . . ?
C16 C17 C20 106.0(14) . . ?
C18 C17 H17 111.5 . . ?
C16 C17 H17 111.5 . . ?
C20 C17 H17 111.5 . . ?
O9A C18 C17 130(2) . . ?
O9A C18 C19 117(2) . . ?
C17 C18 C19 113.4(14) . . ?
C17 C18 H18A 98(10) . . ?
C19 C18 H18A 112(10) . . ?
C17 C18 H18B 134(10) . . ?
C19 C18 H18B 91(10) . . ?
H18A C18 H18B 109(5) . . ?
N3 C19 C18 105.5(14) . . ?
N3 C19 H19A 110.6 . . ?
C18 C19 H19A 110.6 . . ?
N3 C19 H19B 110.6 . . ?
C18 C19 H19B 110.6 . . ?
H19A C19 H19B 108.8 . . ?
C21 C20 C17 110.4(14) . . ?
C21 C20 H20A 109.6 . . ?
C17 C20 H20A 109.6 . . ?
C21 C20 H20B 109.6 . . ?
C17 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
C20 C21 N3 108.2(14) . . ?
C20 C21 H21A 110.1 . . ?
N3 C21 H21A 110.1 . . ?
C20 C21 H21B 110.1 . . ?
N3 C21 H21B 110.1 . . ?
H21A C21 H21B 108.4 . . ?
C1 N1 C5 120.0(12) . . ?
C1 N1 Cr1 124.2(11) . . ?
C5 N1 Cr1 115.5(8) . . ?
C10 N2 C6 117.8(12) . . ?
C10 N2 Cr1 123.6(10) . . ?
C6 N2 Cr1 118.1(8) . . ?
C15 N3 C19 110.4(12) . . ?
C15 N3 C21 113.5(16) . . ?
C19 N3 C21 111.0(15) . . ?
C15 N3 H4N 111(7) . . ?
C19 N3 H4N 110(6) . . ?
C21 N3 H4N 101(7) . . ?
C13 O1 Cr1 113.8(8) . . ?
C14 O4 Cr1 113.8(8) . . ?
C11 O5 Cr1 111.4(9) . . ?
C12 O8 Cr1 114.5(9) . . ?
O8 Cr1 O5 82.5(4) . . ?
O8 Cr1 O4 92.2(4) . . ?
O5 Cr1 O4 89.6(4) . . ?
O8 Cr1 O1 91.3(4) . . ?
O5 Cr1 O1 169.8(4) . . ?
O4 Cr1 O1 82.5(4) . . ?
O8 Cr1 N2 94.8(4) . . ?
O5 Cr1 N2 97.2(4) . . ?
O4 Cr1 N2 170.8(4) . . ?
O1 Cr1 N2 91.4(4) . . ?
O8 Cr1 N1 170.4(4) . . ?
O5 Cr1 N1 92.9(4) . . ?
O4 Cr1 N1 96.2(4) . . ?
O1 Cr1 N1 94.4(4) . . ?
N2 Cr1 N1 77.4(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
N1 C1 C2 C3 -2(2) . . . . ?
C1 C2 C3 C4 4(3) . . . . ?
C2 C3 C4 C5 -5(3) . . . . ?
C3 C4 C5 N1 4(2) . . . . ?
C3 C4 C5 C6 179.5(14) . . . . ?
N1 C5 C6 C7 169.8(13) . . . . ?
C4 C5 C6 C7 -6(2) . . . . ?
N1 C5 C6 N2 -10.7(16) . . . . ?
C4 C5 C6 N2 173.5(12) . . . . ?
N2 C6 C7 C8 1(2) . . . . ?
C5 C6 C7 C8 179.9(14) . . . . ?
C6 C7 C8 C9 -2(3) . . . . ?
C7 C8 C9 C10 3(3) . . . . ?
C8 C9 C10 N2 -3(2) . . . . ?
O6 C11 C12 O7 -19(2) . . . . ?
O5 C11 C12 O7 159.3(15) . . . . ?
O6 C11 C12 O8 162.1(15) . . . . ?
O5 C11 C12 O8 -19.4(18) . . . . ?
O2 C13 C14 O3 0(2) . . . . ?
O1 C13 C14 O3 -178.3(12) . . . . ?
O2 C13 C14 O4 -177.6(13) . . . . ?
O1 C13 C14 O4 3.7(17) . . . . ?
N3 C15 C16 O9B -176(2) . . . . ?
N3 C15 C16 C17 4.4(18) . . . . ?
O9B C16 C17 C18 -125(2) . . . . ?
C15 C16 C17 C18 53.9(17) . . . . ?
O9B C16 C17 C20 119(2) . . . . ?
C15 C16 C17 C20 -61.3(18) . . . . ?
C16 C17 C18 O9A 128(3) . . . . ?
C20 C17 C18 O9A -117(3) . . . . ?
C16 C17 C18 C19 -55.9(19) . . . . ?
C20 C17 C18 C19 58.3(18) . . . . ?
O9A C18 C19 N3 176(2) . . . . ?
C17 C18 C19 N3 -1(2) . . . . ?
C18 C17 C20 C21 -57(2) . . . . ?
C16 C17 C20 C21 59(2) . . . . ?
C17 C20 C21 N3 -2(3) . . . . ?
C2 C1 N1 C5 1(2) . . . . ?
C2 C1 N1 Cr1 174.1(11) . . . . ?
C4 C5 N1 C1 -1.9(19) . . . . ?
C6 C5 N1 C1 -177.7(11) . . . . ?
C4 C5 N1 Cr1 -175.6(10) . . . . ?
C6 C5 N1 Cr1 8.6(14) . . . . ?
C9 C10 N2 C6 1(2) . . . . ?
C9 C10 N2 Cr1 173.1(11) . . . . ?
C7 C6 N2 C10 -0.1(18) . . . . ?
C5 C6 N2 C10 -179.6(11) . . . . ?
C7 C6 N2 Cr1 -172.5(10) . . . . ?
C5 C6 N2 Cr1 8.1(13) . . . . ?
C16 C15 N3 C19 -66.0(15) . . . . ?
C16 C15 N3 C21 59.4(15) . . . . ?
C18 C19 N3 C15 64.4(16) . . . . ?
C18 C19 N3 C21 -62.4(18) . . . . ?
C20 C21 N3 C15 -61(2) . . . . ?
C20 C21 N3 C19 64(2) . . . . ?
O2 C13 O1 Cr1 -173.0(12) . . . . ?
C14 C13 O1 Cr1 5.7(14) . . . . ?
O3 C14 O4 Cr1 171.0(11) . . . . ?
C13 C14 O4 Cr1 -11.2(15) . . . . ?
O6 C11 O5 Cr1 -154.0(15) . . . . ?
C12 C11 O5 Cr1 27.6(15) . . . . ?
O7 C12 O8 Cr1 -177.8(12) . . . . ?
C11 C12 O8 Cr1 0.9(14) . . . . ?

_refine_diff_density_max         0.411
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.103



####################################################################### 
# 
# 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_3H2O
_database_code_depnum_ccdc_archive 'CCDC 2159917'
loop_
_audit_author_name
_audit_author_address
'Lidija Andros Dubraja'
;Rudjer Boskovic Institute
Croatia
;
_audit_update_record             
;
2022-03-18 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;
_chemical_name_common            '(CH3-DABCO)[Cr(bpy)(ox)2] x 5(H2O)'
_chemical_formula_moiety         'C14 H8 Cr1 N2 O8, C7 H15 N2, 5(H2 O)'
_chemical_formula_sum            'C21 H33 Cr1 N4 O13'
_chemical_formula_weight         601.51
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/a'
_symmetry_Int_Tables_number      14
_space_group_name_Hall           '-P 2yab'
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
3 1/2-x,1/2+y,-z
4 1/2+x,1/2-y,z
_cell_length_a                   19.47288(78)
_cell_length_b                   12.65513(45)
_cell_length_c                   10.82217(37)
_cell_angle_alpha                90
_cell_angle_beta                 94.16066(26)
_cell_angle_gamma                90
_cell_volume                     2659.9
_cell_formula_units_Z            4
_cell_measurement_temperature    293
_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.502
_diffrn_ambient_temperature      293
_diffrn_radiation_type           'Cu K\a'
_diffrn_measurement_device_type  'Empyrean, Malvern Panalytical'
_diffrn_radiation_wavelength     1.54060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_shift/su_max          <0.01
_refine_ls_number_parameters     70
_pd_proc_ls_prof_R_factor        0.041
_pd_proc_ls_prof_wR_factor       0.048
_pd_proc_ls_prof_wR_expected     0.016
_refine_ls_structure_factor_coef Fsqd

_computing_data_collection       Panalytical
_computing_data_reduction        none
_computing_cell_refinement       Topas
_computing_structure_solution    Topas
_computing_structure_refinement  Topas

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_thermal_displace_type
C1 C 0.066130(92) -0.27840(3) 0.58870(37) 0.0716 Uiso
H2 H 0.093843(5) -0.32748(42) 0.55200(99) 0.0716 Uiso
C3 C 0.008195(42) -0.31364(58) 0.64257(16) 0.0716 Uiso
H4 H -0.00269(45) -0.38521(93) 0.64333(8) 0.0716 Uiso
C5 C -0.03304(28) -0.24024(66) 0.69546(13) 0.0716 Uiso
H6 H -0.07282(34) -0.26179(32) 0.73088(99) 0.0716 Uiso
C7 C -0.01512(37) -0.13397(44) 0.69549(70) 0.0716 Uiso
H8 H -0.04228(78) -0.08385(63) 0.73159(93) 0.0716 Uiso
C9 C 0.044137(92) -0.10423(93) 0.64067(98) 0.0716 Uiso
C10 C 0.069029(8) 0.006081304(12) 0.63639(39) 0.0716 Uiso
C11 C 0.034173(38) 0.0909199(42) 0.68165(96) 0.0716 Uiso
H12 H -0.00718(26) 0.08158935(87) 0.71825(2) 0.0716 Uiso
C13 C 0.062757(35) 0.19074(71) 0.67100(16) 0.0716 Uiso
H14 H 0.040222(55) 0.24931(94) 0.70057(69) 0.0716 Uiso
C15 C 0.12342(3) 0.203798(32) 0.61755(64) 0.0716 Uiso
H16 H 0.14245(81) 0.270662(95) 0.61013(27) 0.0716 Uiso
C17 C 0.15635(5) 0.114939(11) 0.57437(19) 0.0716 Uiso
H18 H 0.19790(32) 0.123158(33) 0.53820(52) 0.0716 Uiso
N23 N 0.08401(28) -0.17557(28) 0.58719(48) 0.0716 Uiso
N24 N 0.12965(44) 0.017721(26) 0.58344(29) 0.0716 Uiso
C19 C 0.16297(90) -0.15931(8) 0.27290(98) 0.0716 Uiso
C20 C 0.19603(28) -0.25958(77) 0.33633(59) 0.0716 Uiso
C21 C 0.28583(71) -0.10923(66) 0.69549(59) 0.0716 Uiso
C22 C 0.31042(64) -0.06577(81) 0.57160(85) 0.0716 Uiso
O25 O 0.13813(52) -0.09418(19) 0.35054(69) 0.0716 Uiso
O26 O 0.16224(64) -0.14771(24) 0.16124(61) 0.0716 Uiso
O27 O 0.21616(5) -0.33267(42) 0.27638(32) 0.0716 Uiso
O28 O 0.19979(13) -0.25542(43) 0.45670(81) 0.0716 Uiso
O29 O 0.22231(16) -0.14055(95) 0.68594(28) 0.0716 Uiso
O30 O 0.32384(42) -0.11137(8) 0.78900(37) 0.0716 Uiso
O31 O 0.37115(85) -0.04782(87) 0.56263(53) 0.0716 Uiso
O32 O 0.26186(70) -0.05509(89) 0.48554(38) 0.0716 Uiso
Cr1 Cr 0.17375(21) -0.11885(43) 0.52179(16) 0.0689 Uiso
C34 C 0.25378(6) 0.51192(74) 1.020305(19) 0.0127 Uiso
H35 H 0.25527(71) 0.51865(55) 1.10971(12) 0.0127 Uiso
H36 H 0.27992(5) 0.44976(78) 1.0003563(38) 0.0127 Uiso
C37 C 0.21102(35) 0.57083(67) 0.77547(97) 0.0127 Uiso
H38 H 0.19839(41) 0.61995(68) 0.70888(94) 0.0127 Uiso
H39 H 0.20895(89) 0.49995(77) 0.74133(72) 0.0127 Uiso
C40 C 0.17944(4) 0.50112(16) 0.96728(99) 0.0127 Uiso
H41 H 0.17256(68) 0.43097(65) 0.93242(3) 0.0127 Uiso
H42 H 0.14889(22) 0.50914(29) 1.03346(23) 0.0127 Uiso
N43 N 0.16189(81) 0.57995(57) 0.87114(15) 0.0127 Uiso
C44 C 0.16790(77) 0.68585(31) 0.92488(29) 0.0127 Uiso
H45 H 0.13299(51) 0.69531(64) 0.98344(57) 0.0127 Uiso
H46 H 0.16003(68) 0.73813(51) 0.85979(81) 0.0127 Uiso
C47 C 0.23970(50) 0.70267(90) 0.99112(99) 0.0127 Uiso
H48 H 0.25996(69) 0.76716(65) 0.96160(87) 0.0127 Uiso
H49 H 0.23594(29) 0.70919(27) 1.07965(67) 0.0127 Uiso
C50 C 0.28417(50) 0.59399(73) 0.82764(97) 0.0127 Uiso
H51 H 0.31415(86) 0.53573(5) 0.80954(58) 0.0127 Uiso
H52 H 0.30110(81) 0.65737(88) 0.78947(87) 0.0127 Uiso
C53 C 0.35598(37) 0.62503(56) 1.01983(54) 0.0127 Uiso
H54 H 0.35458(25) 0.64862(55) 1.10390(81) 0.0127 Uiso
H55 H 0.38075(78) 0.55955(55) 1.01824(35) 0.0127 Uiso
H56 H 0.37868(35) 0.67722(15) 0.97293(51) 0.0127 Uiso
N57 N 0.28448(17) 0.60925(33) 0.96446(12) 0.0127 Uiso
O1W O 0.99169(23) 0.26760(73) 0.04930(14) 0.1498 Uiso
H28 H 1.04268 0.2676 0.0493 . .
H29 H 0.972943 0.331667 0.00593147 . .
O2W O 0.44884(68) 0.053061(96) 0.82092(25) 0.1498 Uiso
H30 H 0.499834 0.053061 0.82092 . .
H31 H 0.430093 0.117128 0.777551 . .
O3W O 0.43838(74) 0.81783(48) 0.15895(93) 0.1498 Uiso
H26 H 0.489374 0.81783 0.15895 . .
H27 H 0.419633 0.881897 0.115581 . .
O4W O 0.91800(61) 0.50817(27) 0.35374(36) 0.1498 Uiso
H32 H 0.968994 0.50817 0.35374 . .
H33 H 0.899253 0.572237 0.310371 . .
O5W O 0.035821(12) 0.89695(43) 0.01978005(35) 0.1498 Uiso
H24 H 0.086815 0.89695 0.0197801 . .
H25 H 0.0170743 0.961017 -0.0235885 . .

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 H2 0.931(7)
C1 C3 1.381(4)
C1 N23 1.348(4)
C3 H4 0.93(1)
C3 C5 1.379(8)
C5 H6 0.930(9)
C5 C7 1.39(1)
C7 H8 0.93(1)
C7 C9 1.39(1)
C9 C10 1.48(1)
C9 N23 1.35(1)
C10 C11 1.379(4)
C10 N24 1.357(8)
C11 H12 0.930(7)
C11 C13 1.389(8)
C13 H14 0.93(1)
C13 C15 1.363(4)
C15 H16 0.930(7)
C15 C17 1.392(3)
C17 H18 0.930(6)
C17 N24 1.342(3)
N23 Cr1 2.061(7)
N24 Cr1 2.062(6)
C19 C20 1.56(1)
C19 O25 1.30(1)
C19 O26 1.22(1)
C20 O27 1.21(1)
C20 O28 1.30(1)
C21 C22 1.56(1)
C21 O29 1.30(1)
C21 O30 1.21(1)
C22 O31 1.21(2)
C22 O32 1.29(1)
O25 Cr1 1.956(8)
O28 Cr1 1.947(8)
O29 Cr1 1.970(4)
O32 Cr1 1.96(1)
C34 H35 0.970(2)
C34 H36 0.97(1)
C34 C40 1.524(4)
C34 N57 1.514(8)
C37 H38 0.97(1)
C37 H39 0.97(1)
C37 N43 1.46(1)
C37 C50 1.52(1)
C40 H41 0.970(9)
C40 H42 0.969(9)
C40 N43 1.46(1)
N43 C44 1.462(8)
C44 H45 0.97(1)
C44 H46 0.970(9)
C44 C47 1.54(2)
C47 H48 0.97(1)
C47 H49 0.97(1)
C47 N57 1.51(1)
C50 H51 0.97(1)
C50 H52 0.97(2)
C50 N57 1.49(1)
C53 H54 0.96(1)
C53 H55 0.96(1)
C53 H56 0.960(8)
C53 N57 1.489(8)
O1W H28 0.993
O1W H29 0.993
O2W H30 0.99
O2W H31 0.993
O3W H26 0.99
O3W H27 0.993
O4W H32 0.99
O4W H33 0.993
O5W H24 0.993
O5W H25 0.993

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
H2 C1 C3 118.8(4)
H2 C1 N23 118.8(4)
C3 C1 N23 122.5(3)
C1 C3 H4 120.8(5)
C1 C3 C5 118.4(3)
H4 C3 C5 120.8(6)
C3 C5 H6 120.1(6)
C3 C5 C7 119.9(5)
H6 C5 C7 120.0(7)
C5 C7 H8 120.7(9)
C5 C7 C9 118.6(6)
H8 C7 C9 121(1)
C7 C9 C10 123.6(6)
C7 C9 N23 121.6(7)
C10 C9 N23 114.7(6)
C9 C10 C11 123.6(4)
C9 C10 N24 114.4(4)
C11 C10 N24 122.1(3)
C10 C11 H12 121.1(4)
C10 C11 C13 117.9(3)
H12 C11 C13 121.0(4)
C11 C13 H14 119.6(6)
C11 C13 C15 120.7(3)
H14 C13 C15 119.7(6)
C13 C15 H16 120.7(5)
C13 C15 C17 118.6(3)
H16 C15 C17 120.7(5)
C15 C17 H18 119.1(3)
C15 C17 N24 121.7(2)
H18 C17 N24 119.1(3)
C1 N23 C9 119.0(5)
C1 N23 Cr1 124.5(3)
C9 N23 Cr1 116.3(5)
C10 N24 C17 118.9(3)
C10 N24 Cr1 116.2(3)
C17 N24 Cr1 124.9(3)
C20 C19 O25 113.2(8)
C20 C19 O26 120.7(8)
O25 C19 O26 126.1(9)
C19 C20 O27 121.7(7)
C19 C20 O28 113.5(7)
O27 C20 O28 124.8(7)
C22 C21 O29 113.0(8)
C22 C21 O30 121.4(8)
O29 C21 O30 125.6(8)
C21 C22 O31 120(1)
C21 C22 O32 113.9(9)
O31 C22 O32 126(1)
C19 O25 Cr1 112.9(6)
C20 O28 Cr1 113.6(5)
C21 O29 Cr1 115.0(6)
C22 O32 Cr1 114.8(8)
N23 Cr1 N24 78.3(2)
N23 Cr1 O25 97.5(3)
N23 Cr1 O28 93.7(3)
N23 Cr1 O29 90.3(3)
N23 Cr1 O32 171.0(4)
N24 Cr1 O25 92.6(3)
N24 Cr1 O28 170.5(3)
N24 Cr1 O29 90.5(3)
N24 Cr1 O32 96.4(3)
O25 Cr1 O28 83.3(3)
O25 Cr1 O29 172.1(3)
O25 Cr1 O32 90.0(4)
O28 Cr1 O29 94.7(3)
O28 Cr1 O32 92.2(4)
O29 Cr1 O32 82.4(4)
H35 C34 H36 108.4(6)
H35 C34 C40 110.0(5)
H35 C34 N57 110.0(5)
H36 C34 C40 110.1(4)
H36 C34 N57 110.0(4)
C40 C34 N57 108.3(3)
H38 C37 H39 108(1)
H38 C37 N43 109.4(9)
H38 C37 C50 109.4(9)
H39 C37 N43 109(1)
H39 C37 C50 109(1)
N43 C37 C50 111.4(7)
C34 C40 H41 109.2(6)
C34 C40 H42 109.2(4)
C34 C40 N43 111.9(5)
H41 C40 H42 108.0(6)
H41 C40 N43 109.2(6)
H42 C40 N43 109.3(5)
C37 N43 C40 108.5(6)
C37 N43 C44 108.4(7)
C40 N43 C44 109.5(6)
N43 C44 H45 109.5(8)
N43 C44 H46 109.4(9)
N43 C44 C47 110.8(7)
H45 C44 H46 108(1)
H45 C44 C47 109.6(9)
H46 C44 C47 109.5(9)
C44 C47 H48 110(1)
C44 C47 H49 109.9(9)
C44 C47 N57 108.7(7)
H48 C47 H49 108(1)
H48 C47 N57 110(1)
H49 C47 N57 110.0(9)
C37 C50 H51 110(1)
C37 C50 H52 110(1)
C37 C50 N57 109.2(7)
H51 C50 H52 108(1)
H51 C50 N57 109.9(9)
H52 C50 N57 110(1)
H54 C53 H55 109.5(9)
H54 C53 H56 109.4(8)
H54 C53 N57 109.5(7)
H55 C53 H56 109.5(9)
H55 C53 N57 109.5(8)
H56 C53 N57 109.4(6)
C34 N57 C47 108.1(5)
C34 N57 C50 108.5(4)
C34 N57 C53 109.5(3)
C47 N57 C50 109.3(6)
C47 N57 C53 110.8(5)
C50 N57 C53 110.7(5)
#END
####################################################################### 
# 
# 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_comp6H2O
_database_code_depnum_ccdc_archive 'CCDC 2159921'
loop_
_audit_author_name
_audit_author_address
'Lidija Andros Dubraja'
;Rudjer Boskovic Institute
Croatia
;
_audit_update_record             
;
2022-03-18 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            '[H-(OH)2ABCO][Cr(phen)(ox)2] x 2(H2O)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H8 Cr N2 O8, C7 H14 N O2, 2(H2 O)'
_chemical_formula_sum            'C23 H26 Cr N3 O12'
_chemical_formula_weight         588.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   15.80320(10)
_cell_length_b                   10.41290(10)
_cell_length_c                   14.82910(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.6120(10)
_cell_angle_gamma                90
_cell_volume                     2435.39(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    7571
_cell_measurement_theta_min      5.0710
_cell_measurement_theta_max      75.6670

_exptl_crystal_description       plate-like
_exptl_crystal_colour            'orange and purplish red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_F_000             1220
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    4.525
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.55778
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.645
_oxdiff_exptl_absorpt_empirical_full_max 2.036
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      298(2)
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Ruby
_diffrn_detector_area_resol_mean 10.4323
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            13372
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         5.090
_diffrn_reflns_theta_max         75.846
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5020
_reflns_number_gt                4683
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SIR-2019 (Burla, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Mercury (2020)'
_computing_publication_material  'PLATON (Spek, 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0489P)²+0.8738P] 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_number_reflns         5020
_refine_ls_number_parameters     384
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1050
_refine_ls_wR_factor_gt          0.1026
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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
C1 C 0.56426(13) -0.0867(2) 0.16556(15) 0.0386(4) Uani 1 1 d . . . . .
H1 H 0.607430 -0.140871 0.187962 0.046 Uiso 1 1 calc R U . . .
C2 C 0.48496(15) -0.1394(2) 0.13909(17) 0.0435(5) Uani 1 1 d . . . . .
H2 H 0.475830 -0.227090 0.145117 0.052 Uiso 1 1 calc R U . . .
C3 C 0.42085(13) -0.0620(2) 0.10437(16) 0.0431(5) Uani 1 1 d . . . . .
H3 H 0.368367 -0.096882 0.086144 0.052 Uiso 1 1 calc R U . . .
C4 C 0.43509(12) 0.0706(2) 0.09654(14) 0.0363(4) Uani 1 1 d . . . . .
C5 C 0.37283(13) 0.1611(3) 0.06204(16) 0.0428(5) Uani 1 1 d . . . . .
H5 H 0.320136 0.131792 0.039322 0.051 Uiso 1 1 calc R U . . .
C6 C 0.38947(13) 0.2884(2) 0.06200(15) 0.0426(5) Uani 1 1 d . . . . .
H6 H 0.347420 0.345248 0.040717 0.051 Uiso 1 1 calc R U . . .
C7 C 0.47063(13) 0.3378(2) 0.09410(14) 0.0370(4) Uani 1 1 d . . . . .
C8 C 0.49181(14) 0.4690(2) 0.10030(15) 0.0430(5) Uani 1 1 d . . . . .
H8 H 0.450843 0.531146 0.086246 0.052 Uiso 1 1 calc R U . . .
C9 C 0.57300(16) 0.5047(2) 0.12712(17) 0.0455(5) Uani 1 1 d . . . . .
H9 H 0.587244 0.591244 0.131737 0.055 Uiso 1 1 calc R U . . .
C10 C 0.63429(14) 0.4106(2) 0.14751(16) 0.0412(4) Uani 1 1 d . . . . .
H10 H 0.689953 0.435780 0.161958 0.049 Uiso 1 1 calc R U . . .
C11 C 0.53454(12) 0.25009(19) 0.12173(13) 0.0316(4) Uani 1 1 d . . . . .
C12 C 0.51577(12) 0.1162(2) 0.12552(13) 0.0320(4) Uani 1 1 d . . . . .
C13 C 0.84612(12) 0.2087(2) 0.12741(14) 0.0359(4) Uani 1 1 d . . . . .
C14 C 0.80123(13) 0.1273(2) 0.05130(14) 0.0368(4) Uani 1 1 d . . . . .
C15 C 0.75800(12) -0.0150(2) 0.32611(14) 0.0345(4) Uani 1 1 d . . . . .
C16 C 0.71197(12) 0.0976(2) 0.37100(14) 0.0356(4) Uani 1 1 d . . . . .
C17 C 1.05445(14) -0.3346(3) 0.09405(19) 0.0493(5) Uani 1 1 d . . . . .
H17A H 1.104280 -0.297307 0.125391 0.059 Uiso 1 1 calc R U . . .
H17B H 1.073040 -0.396267 0.050428 0.059 Uiso 1 1 calc R U . . .
C18 C 1.00052(14) -0.4017(2) 0.16152(17) 0.0461(5) Uani 1 1 d . . . . .
H18A H 1.031584 -0.407277 0.219923 0.055 Uiso 1 1 calc R U . . .
H18B H 0.986940 -0.488156 0.140973 0.055 Uiso 1 1 calc R U . . .
C19 C 0.91893(13) -0.3247(2) 0.16984(14) 0.0396(4) Uani 1 1 d . . . . .
C20 C 0.94185(14) -0.1851(2) 0.19123(16) 0.0456(5) Uani 1 1 d . . . . .
H20A H 0.980415 -0.181031 0.244689 0.055 Uiso 1 1 calc R U . . .
H20B H 0.891111 -0.137108 0.203040 0.055 Uiso 1 1 calc R U . . .
C21 C 0.98393(16) -0.1264(2) 0.1104(2) 0.0503(6) Uani 1 1 d . . . . .
H21A H 0.946252 -0.064130 0.080374 0.060 Uiso 1 1 calc R U . . .
H21B H 1.035913 -0.082940 0.130938 0.060 Uiso 1 1 calc R U . . .
C22 C 0.92243(14) -0.2868(3) 0.00443(16) 0.0489(5) Uani 1 1 d . . . . .
H22A H 0.935150 -0.358980 -0.033795 0.059 Uiso 1 1 calc R U . . .
H22B H 0.892750 -0.222426 -0.032761 0.059 Uiso 1 1 calc R U . . .
C23 C 0.86609(12) -0.3315(2) 0.07991(14) 0.0382(4) Uani 1 1 d . . . . .
N1 N 0.57950(10) 0.03823(16) 0.15956(11) 0.0322(3) Uani 1 1 d . . . . .
N2 N 0.61559(10) 0.28678(16) 0.14689(11) 0.0334(3) Uani 1 1 d . . . . .
N3 N 1.00292(11) -0.23159(19) 0.04659(13) 0.0396(4) Uani 1 1 d . . . . .
O1 O 0.79889(8) 0.23403(15) 0.19339(10) 0.0361(3) Uani 1 1 d . . . . .
O2 O 0.91961(10) 0.2404(2) 0.12239(12) 0.0528(4) Uani 1 1 d . . . . .
O3 O 0.83964(11) 0.1004(2) -0.01539(12) 0.0525(4) Uani 1 1 d . . . . .
O4 O 0.72524(9) 0.09431(15) 0.06538(10) 0.0368(3) Uani 1 1 d . . . . .
O5 O 0.75007(9) -0.01547(14) 0.23943(10) 0.0367(3) Uani 1 1 d . . . . .
O6 O 0.79445(12) -0.09767(19) 0.37210(12) 0.0538(4) Uani 1 1 d . . . . .
O7 O 0.71265(13) 0.1058(2) 0.45238(12) 0.0580(5) Uani 1 1 d . . . . .
O8 O 0.67218(9) 0.17186(15) 0.31359(10) 0.0379(3) Uani 1 1 d . . . . .
O9 O 0.79605(10) -0.2492(2) 0.07707(13) 0.0529(4) Uani 1 1 d D . . . .
O10 O 0.84053(12) -0.45994(19) 0.06751(13) 0.0549(4) Uani 1 1 d D . . . .
O11 O 0.71810(12) -0.30722(19) 0.24061(14) 0.0550(4) Uani 1 1 d D . . . .
O12 O 0.79433(17) 0.0320(2) -0.19278(15) 0.0683(6) Uani 1 1 d D . . . .
Cr1 Cr 0.69259(2) 0.13505(3) 0.18729(2) 0.02892(10) Uani 1 1 d . . . . .
H3N H 1.0336(17) -0.198(3) 0.002(2) 0.042(7) Uiso 1 1 d . . . . .
H9O H 0.772(2) -0.262(4) 0.1266(18) 0.080(12) Uiso 1 1 d D . . . .
H10O H 0.812(3) -0.467(6) 0.017(2) 0.125(19) Uiso 1 1 d D . . . .
H11A H 0.736(2) -0.381(2) 0.261(3) 0.081(12) Uiso 1 1 d D . . . .
H11B H 0.741(3) -0.246(3) 0.273(3) 0.093(14) Uiso 1 1 d D . . . .
H12A H 0.796(3) 0.044(4) -0.1356(13) 0.082(12) Uiso 1 1 d D . . . .
H12B H 0.800(3) 0.101(3) -0.223(3) 0.114(18) Uiso 1 1 d D . . . .
H19 H 0.8879(18) -0.357(3) 0.216(2) 0.046(7) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.327(3) . ?
C1 C2 1.401(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.369(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.405(3) . ?
C3 H3 0.9300 . ?
C4 C12 1.402(3) . ?
C4 C5 1.433(3) . ?
C5 C6 1.351(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.435(3) . ?
C6 H6 0.9300 . ?
C7 C11 1.403(3) . ?
C7 C8 1.408(3) . ?
C8 C9 1.371(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.398(3) . ?
C9 H9 0.9300 . ?
C10 N2 1.322(3) . ?
C10 H10 0.9300 . ?
C11 N2 1.366(3) . ?
C11 C12 1.428(3) . ?
C12 N1 1.365(3) . ?
C13 O2 1.214(3) . ?
C13 O1 1.295(2) . ?
C13 C14 1.547(3) . ?
C14 O3 1.225(3) . ?
C14 O4 1.279(3) . ?
C15 O6 1.220(3) . ?
C15 O5 1.284(3) . ?
C15 C16 1.552(3) . ?
C16 O7 1.209(3) . ?
C16 O8 1.285(3) . ?
C17 N3 1.496(3) . ?
C17 C18 1.524(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.530(3) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.526(3) . ?
C19 C23 1.530(3) . ?
C19 H19 0.94(3) . ?
C20 C21 1.533(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 N3 1.490(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 N3 1.496(3) . ?
C22 C23 1.545(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 O9 1.398(3) . ?
C23 O10 1.406(3) . ?
N1 Cr1 2.0705(16) . ?
N2 Cr1 2.0602(16) . ?
N3 H3N 0.91(3) . ?
O1 Cr1 1.9680(14) . ?
O4 Cr1 1.9575(15) . ?
O5 Cr1 1.9470(14) . ?
O8 Cr1 1.9583(15) . ?
O9 H9O 0.860(19) . ?
O10 H10O 0.857(19) . ?
O11 H11A 0.863(18) . ?
O11 H11B 0.867(19) . ?
O12 H12A 0.856(18) . ?
O12 H12B 0.856(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 121.8(2) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 120.2(2) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C2 C3 C4 119.4(2) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C12 C4 C3 117.01(19) . . ?
C12 C4 C5 118.5(2) . . ?
C3 C4 C5 124.5(2) . . ?
C6 C5 C4 121.1(2) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C7 121.40(19) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C11 C7 C8 116.63(19) . . ?
C11 C7 C6 118.4(2) . . ?
C8 C7 C6 124.95(19) . . ?
C9 C8 C7 119.79(19) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 119.7(2) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
N2 C10 C9 122.1(2) . . ?
N2 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
N2 C11 C7 122.90(19) . . ?
N2 C11 C12 117.14(17) . . ?
C7 C11 C12 119.96(18) . . ?
N1 C12 C4 123.21(19) . . ?
N1 C12 C11 116.42(17) . . ?
C4 C12 C11 120.36(18) . . ?
O2 C13 O1 126.2(2) . . ?
O2 C13 C14 120.05(19) . . ?
O1 C13 C14 113.78(16) . . ?
O3 C14 O4 126.0(2) . . ?
O3 C14 C13 119.11(19) . . ?
O4 C14 C13 114.85(18) . . ?
O6 C15 O5 124.8(2) . . ?
O6 C15 C16 120.72(19) . . ?
O5 C15 C16 114.43(17) . . ?
O7 C16 O8 126.3(2) . . ?
O7 C16 C15 120.4(2) . . ?
O8 C16 C15 113.18(17) . . ?
N3 C17 C18 109.10(17) . . ?
N3 C17 H17A 109.9 . . ?
C18 C17 H17A 109.9 . . ?
N3 C17 H17B 109.9 . . ?
C18 C17 H17B 109.9 . . ?
H17A C17 H17B 108.3 . . ?
C17 C18 C19 108.75(19) . . ?
C17 C18 H18A 109.9 . . ?
C19 C18 H18A 109.9 . . ?
C17 C18 H18B 109.9 . . ?
C19 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
C20 C19 C23 109.56(19) . . ?
C20 C19 C18 109.02(18) . . ?
C23 C19 C18 108.77(18) . . ?
C20 C19 H19 108.8(18) . . ?
C23 C19 H19 110.0(18) . . ?
C18 C19 H19 110.6(18) . . ?
C19 C20 C21 109.02(18) . . ?
C19 C20 H20A 109.9 . . ?
C21 C20 H20A 109.9 . . ?
C19 C20 H20B 109.9 . . ?
C21 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
N3 C21 C20 108.56(19) . . ?
N3 C21 H21A 110.0 . . ?
C20 C21 H21A 110.0 . . ?
N3 C21 H21B 110.0 . . ?
C20 C21 H21B 110.0 . . ?
H21A C21 H21B 108.4 . . ?
N3 C22 C23 109.05(18) . . ?
N3 C22 H22A 109.9 . . ?
C23 C22 H22A 109.9 . . ?
N3 C22 H22B 109.9 . . ?
C23 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
O9 C23 O10 111.02(18) . . ?
O9 C23 C19 112.66(19) . . ?
O10 C23 C19 107.15(19) . . ?
O9 C23 C22 106.5(2) . . ?
O10 C23 C22 111.5(2) . . ?
C19 C23 C22 108.04(17) . . ?
C1 N1 C12 118.35(17) . . ?
C1 N1 Cr1 128.46(14) . . ?
C12 N1 Cr1 113.05(13) . . ?
C10 N2 C11 118.68(17) . . ?
C10 N2 Cr1 128.17(14) . . ?
C11 N2 Cr1 113.05(13) . . ?
C21 N3 C17 110.7(2) . . ?
C21 N3 C22 110.36(18) . . ?
C17 N3 C22 110.1(2) . . ?
C21 N3 H3N 108.3(18) . . ?
C17 N3 H3N 108.4(17) . . ?
C22 N3 H3N 108.9(18) . . ?
C13 O1 Cr1 112.92(13) . . ?
C14 O4 Cr1 113.41(13) . . ?
C15 O5 Cr1 114.10(13) . . ?
C16 O8 Cr1 114.37(13) . . ?
C23 O9 H9O 106(3) . . ?
C23 O10 H10O 109(4) . . ?
H11A O11 H11B 110(3) . . ?
H12A O12 H12B 114(4) . . ?
O5 Cr1 O4 92.80(6) . . ?
O5 Cr1 O8 83.03(6) . . ?
O4 Cr1 O8 174.02(6) . . ?
O5 Cr1 O1 91.59(6) . . ?
O4 Cr1 O1 83.22(6) . . ?
O8 Cr1 O1 92.58(6) . . ?
O5 Cr1 N2 170.10(7) . . ?
O4 Cr1 N2 94.75(7) . . ?
O8 Cr1 N2 89.90(7) . . ?
O1 Cr1 N2 95.65(7) . . ?
O5 Cr1 N1 93.57(6) . . ?
O4 Cr1 N1 89.17(6) . . ?
O8 Cr1 N1 95.34(6) . . ?
O1 Cr1 N1 171.01(6) . . ?
N2 Cr1 N1 80.15(7) . . ?

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
N1 C1 C2 C3 1.2(4) . . . . ?
C1 C2 C3 C4 -0.7(4) . . . . ?
C2 C3 C4 C12 -0.1(3) . . . . ?
C2 C3 C4 C5 -179.4(2) . . . . ?
C12 C4 C5 C6 -3.7(3) . . . . ?
C3 C4 C5 C6 175.6(2) . . . . ?
C4 C5 C6 C7 1.7(3) . . . . ?
C5 C6 C7 C11 3.1(3) . . . . ?
C5 C6 C7 C8 -176.9(2) . . . . ?
C11 C7 C8 C9 3.8(3) . . . . ?
C6 C7 C8 C9 -176.2(2) . . . . ?
C7 C8 C9 C10 0.4(4) . . . . ?
C8 C9 C10 N2 -4.0(4) . . . . ?
C8 C7 C11 N2 -5.1(3) . . . . ?
C6 C7 C11 N2 174.96(19) . . . . ?
C8 C7 C11 C12 174.12(19) . . . . ?
C6 C7 C11 C12 -5.9(3) . . . . ?
C3 C4 C12 N1 0.5(3) . . . . ?
C5 C4 C12 N1 179.90(19) . . . . ?
C3 C4 C12 C11 -178.52(19) . . . . ?
C5 C4 C12 C11 0.9(3) . . . . ?
N2 C11 C12 N1 4.1(3) . . . . ?
C7 C11 C12 N1 -175.17(18) . . . . ?
N2 C11 C12 C4 -176.87(18) . . . . ?
C7 C11 C12 C4 3.9(3) . . . . ?
O2 C13 C14 O3 -3.1(3) . . . . ?
O1 C13 C14 O3 178.3(2) . . . . ?
O2 C13 C14 O4 176.9(2) . . . . ?
O1 C13 C14 O4 -1.7(3) . . . . ?
O6 C15 C16 O7 1.0(3) . . . . ?
O5 C15 C16 O7 177.6(2) . . . . ?
O6 C15 C16 O8 -175.82(19) . . . . ?
O5 C15 C16 O8 0.8(2) . . . . ?
N3 C17 C18 C19 -10.5(3) . . . . ?
C17 C18 C19 C20 -52.9(3) . . . . ?
C17 C18 C19 C23 66.5(3) . . . . ?
C23 C19 C20 C21 -53.3(2) . . . . ?
C18 C19 C20 C21 65.6(2) . . . . ?
C19 C20 C21 N3 -10.7(3) . . . . ?
C20 C19 C23 O9 -52.5(2) . . . . ?
C18 C19 C23 O9 -171.58(19) . . . . ?
C20 C19 C23 O10 -174.89(17) . . . . ?
C18 C19 C23 O10 66.0(2) . . . . ?
C20 C19 C23 C22 64.9(2) . . . . ?
C18 C19 C23 C22 -54.2(3) . . . . ?
N3 C22 C23 O9 111.7(2) . . . . ?
N3 C22 C23 O10 -127.1(2) . . . . ?
N3 C22 C23 C19 -9.6(3) . . . . ?
C2 C1 N1 C12 -0.8(3) . . . . ?
C2 C1 N1 Cr1 -176.07(17) . . . . ?
C4 C12 N1 C1 -0.1(3) . . . . ?
C11 C12 N1 C1 178.98(18) . . . . ?
C4 C12 N1 Cr1 175.93(15) . . . . ?
C11 C12 N1 Cr1 -5.0(2) . . . . ?
C9 C10 N2 C11 2.9(3) . . . . ?
C9 C10 N2 Cr1 -173.01(17) . . . . ?
C7 C11 N2 C10 1.8(3) . . . . ?
C12 C11 N2 C10 -177.42(19) . . . . ?
C7 C11 N2 Cr1 178.26(15) . . . . ?
C12 C11 N2 Cr1 -0.9(2) . . . . ?
C20 C21 N3 C17 -54.4(2) . . . . ?
C20 C21 N3 C22 67.8(2) . . . . ?
C18 C17 N3 C21 67.4(3) . . . . ?
C18 C17 N3 C22 -54.9(3) . . . . ?
C23 C22 N3 C21 -55.6(3) . . . . ?
C23 C22 N3 C17 66.9(3) . . . . ?
O2 C13 O1 Cr1 -167.8(2) . . . . ?
C14 C13 O1 Cr1 10.7(2) . . . . ?
O3 C14 O4 Cr1 171.7(2) . . . . ?
C13 C14 O4 Cr1 -8.3(2) . . . . ?
O6 C15 O5 Cr1 -177.39(18) . . . . ?
C16 C15 O5 Cr1 6.2(2) . . . . ?
O7 C16 O8 Cr1 176.1(2) . . . . ?
C15 C16 O8 Cr1 -7.3(2) . . . . ?

_refine_diff_density_max         0.311
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.058



####################################################################### 
# 
# 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_comp5H2O
_database_code_depnum_ccdc_archive 'CCDC 2159920'
loop_
_audit_author_name
_audit_author_address
'Lidija Andros Dubraja'
;Rudjer Boskovic Institute
Croatia
;
_audit_update_record             
;
2022-03-18 deposited with the CCDC.	2022-05-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            '[H-(COOH)(OH)ABCO][Cr(bpy)(ox)2] x 2(H2O)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H8 Cr N2 O8, C8 H14 N O3, 2(H2 O)'
_chemical_formula_sum            'C22 H26 Cr N3 O13'
_chemical_formula_weight         592.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

_cell_length_a                   12.56540(10)
_cell_length_b                   19.09800(10)
_cell_length_c                   20.56840(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4935.88(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    17033
_cell_measurement_theta_min      3.5260
_cell_measurement_theta_max      75.654
_exptl_crystal_description       plate-like
_exptl_crystal_colour            'orange and purplish red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_F_000             2456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    4.500
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.44706
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.654
_oxdiff_exptl_absorpt_empirical_full_max 1.634


_diffrn_ambient_temperature      298(2)
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Ruby
_diffrn_detector_area_resol_mean 10.4323
_diffrn_reflns_number            28808
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         4.730
_diffrn_reflns_theta_max         75.888
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5119
_reflns_number_gt                4872
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SIR-2019 (Burla, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Mercury (2020)'
_computing_publication_material  'PLATON (Spek, 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0928P)²+2.6894P] 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_number_reflns         5119
_refine_ls_number_parameters     364
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1419
_refine_ls_wR_factor_gt          0.1400
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.002
_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 0.10720(3) 0.17578(2) 0.50664(2) 0.02761(13) Uani 1 1 d . . . . .
C1 C -0.12671(18) 0.14518(12) 0.52941(12) 0.0390(5) Uani 1 1 d . . . . .
H1 H -0.139071 0.185892 0.505776 0.047 Uiso 1 1 calc R U . . .
C2 C -0.21248(19) 0.10987(14) 0.55584(14) 0.0488(6) Uani 1 1 d . . . . .
H2 H -0.281436 0.126298 0.549765 0.059 Uiso 1 1 calc R U . . .
C3 C -0.1940(2) 0.04987(14) 0.59135(15) 0.0523(6) Uani 1 1 d . . . . .
H3 H -0.250395 0.025474 0.609870 0.063 Uiso 1 1 calc R U . . .
C4 C -0.0906(2) 0.02626(13) 0.59917(14) 0.0464(6) Uani 1 1 d . . . . .
H4 H -0.076794 -0.014120 0.623002 0.056 Uiso 1 1 calc R U . . .
C5 C -0.00807(17) 0.06341(10) 0.57117(11) 0.0342(4) Uani 1 1 d . . . . .
C6 C 0.10482(17) 0.04185(11) 0.57412(12) 0.0361(5) Uani 1 1 d . . . . .
C7 C 0.1398(2) -0.01882(13) 0.60435(16) 0.0539(6) Uani 1 1 d . . . . .
H7 H 0.091997 -0.047779 0.625999 0.065 Uiso 1 1 calc R U . . .
C8 C 0.2462(3) -0.03559(14) 0.60186(17) 0.0597(7) Uani 1 1 d . . . . .
H8 H 0.271058 -0.075628 0.622645 0.072 Uiso 1 1 calc R U . . .
C9 C 0.3153(2) 0.00664(14) 0.56881(15) 0.0516(6) Uani 1 1 d . . . . .
H9 H 0.386991 -0.005045 0.565574 0.062 Uiso 1 1 calc R U . . .
C10 C 0.27657(18) 0.06734(12) 0.54016(12) 0.0400(5) Uani 1 1 d . . . . .
H10 H 0.323462 0.096743 0.518282 0.048 Uiso 1 1 calc R U . . .
N1 N -0.02667(14) 0.12280(9) 0.53667(9) 0.0315(4) Uani 1 1 d . . . . .
N2 N 0.17333(14) 0.08464(9) 0.54322(9) 0.0321(4) Uani 1 1 d . . . . .
C11 C 0.1842(2) 0.15349(12) 0.38269(11) 0.0405(5) Uani 1 1 d . . . . .
C12 C 0.26771(17) 0.19952(11) 0.41777(10) 0.0349(4) Uani 1 1 d . . . . .
C13 C 0.03519(17) 0.31139(11) 0.52700(11) 0.0321(4) Uani 1 1 d . . . . .
C14 C 0.08332(17) 0.28643(11) 0.59236(10) 0.0317(4) Uani 1 1 d . . . . .
O1 O 0.10231(12) 0.13858(8) 0.41770(8) 0.0367(3) Uani 1 1 d . . . . .
O2 O 0.2005(2) 0.13363(15) 0.32733(10) 0.0747(7) Uani 1 1 d . . . . .
O3 O 0.34751(13) 0.22013(10) 0.38993(8) 0.0449(4) Uani 1 1 d . . . . .
O4 O 0.24486(13) 0.21264(8) 0.47758(7) 0.0368(3) Uani 1 1 d . . . . .
O5 O 0.03523(13) 0.26342(8) 0.48219(7) 0.0345(3) Uani 1 1 d . . . . .
O6 O 0.00321(16) 0.37071(8) 0.51989(9) 0.0472(4) Uani 1 1 d . . . . .
O7 O 0.08974(16) 0.32554(9) 0.63840(9) 0.0465(4) Uani 1 1 d . . . . .
O8 O 0.11530(12) 0.22204(8) 0.59135(7) 0.0329(3) Uani 1 1 d . . . . .
C15 C 0.4931(2) 0.22343(16) 0.75153(13) 0.0500(6) Uani 1 1 d . . . . .
H15A H 0.514596 0.193709 0.787458 0.060 Uiso 1 1 calc R U . . .
H15B H 0.541613 0.262909 0.749552 0.060 Uiso 1 1 calc R U . . .
C16 C 0.49853(17) 0.18180(11) 0.68744(11) 0.0344(4) Uani 1 1 d . . . . .
C17 C 0.39034(17) 0.18934(14) 0.65330(12) 0.0385(5) Uani 1 1 d . . . . .
H17 H 0.392601 0.166438 0.610689 0.046 Uiso 1 1 calc R U . . .
C18 C 0.3669(2) 0.26722(15) 0.64506(12) 0.0455(5) Uani 1 1 d . . . . .
H18A H 0.425804 0.289939 0.623072 0.055 Uiso 1 1 calc R U . . .
H18B H 0.303378 0.273464 0.618882 0.055 Uiso 1 1 calc R U . . .
C19 C 0.3507(4) 0.29964(18) 0.71149(15) 0.0731(10) Uani 1 1 d . . . . .
H19A H 0.392976 0.341956 0.715234 0.088 Uiso 1 1 calc R U . . .
H19B H 0.276452 0.312070 0.717222 0.088 Uiso 1 1 calc R U . . .
C20 C 0.3080(3) 0.1883(2) 0.76330(16) 0.0684(9) Uani 1 1 d . . . . .
H20A H 0.237744 0.203858 0.776508 0.082 Uiso 1 1 calc R U . . .
H20B H 0.332342 0.153397 0.794198 0.082 Uiso 1 1 calc R U . . .
C21 C 0.3030(2) 0.15651(16) 0.69515(14) 0.0519(6) Uani 1 1 d . . . . .
H21A H 0.233843 0.165516 0.675914 0.062 Uiso 1 1 calc R U . . .
H21B H 0.313117 0.106222 0.697569 0.062 Uiso 1 1 calc R U . . .
C22 C 0.5228(2) 0.10404(14) 0.69896(15) 0.0532(6) Uani 1 1 d . . . . .
N3 N 0.3831(2) 0.24884(12) 0.76225(11) 0.0485(5) Uani 1 1 d . . . . .
H3N H 0.3836(7) 0.2659(18) 0.7983(18) 0.058 Uiso 1 1 d R U . . .
O9 O 0.58253(13) 0.21046(10) 0.64985(9) 0.0448(4) Uani 1 1 d D . . . .
H9O H 0.5628(12) 0.2115(18) 0.6115(9) 0.067 Uiso 1 1 d DR U . . .
O10 O 0.5423(2) 0.07118(12) 0.64488(13) 0.0740(7) Uani 1 1 d D . . . .
O11 O 0.5211(4) 0.07765(14) 0.75121(17) 0.1223(15) Uani 1 1 d . . . . .
H10O H 0.537(6) 0.0306(18) 0.662(3) 0.183 Uiso 1 1 d DR U . . .
O12 O 0.5706(3) -0.06109(15) 0.6457(3) 0.1296(16) Uani 1 1 d G . . . .
H12A H 0.583151 -0.073880 0.684027 0.194 Uiso 1 1 d G U . . .
H12B H 0.520461 -0.087191 0.633796 0.194 Uiso 1 1 d G U . . .
O13 O 0.4798(5) -0.0735(3) 0.7626(4) 0.173(2) Uani 1 1 d G . . . .
H13A H 0.428502 -0.045277 0.763116 0.260 Uiso 1 1 d G U . . .
H13B H 0.454337 -0.110449 0.778339 0.260 Uiso 1 1 d G 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 O8 1.9562(15) . ?
Cr1 O4 1.9609(16) . ?
Cr1 O1 1.9633(16) . ?
Cr1 O5 1.9678(15) . ?
Cr1 N1 2.0579(18) . ?
Cr1 N2 2.0704(17) . ?
C1 N1 1.336(3) . ?
C1 C2 1.383(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.379(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.385(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(3) . ?
C4 H4 0.9300 . ?
C5 N1 1.358(3) . ?
C5 C6 1.478(3) . ?
C6 N2 1.346(3) . ?
C6 C7 1.386(3) . ?
C7 C8 1.376(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.366(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.389(3) . ?
C9 H9 0.9300 . ?
C10 N2 1.340(3) . ?
C10 H10 0.9300 . ?
C11 O2 1.217(3) . ?
C11 O1 1.288(3) . ?
C11 C12 1.548(3) . ?
C12 O3 1.220(3) . ?
C12 O4 1.288(3) . ?
C13 O6 1.211(3) . ?
C13 O5 1.300(3) . ?
C13 C14 1.549(3) . ?
C14 O7 1.209(3) . ?
C14 O8 1.294(3) . ?
C15 N3 1.482(4) . ?
C15 C16 1.541(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 O9 1.418(3) . ?
C16 C22 1.535(3) . ?
C16 C17 1.537(3) . ?
C17 C18 1.526(4) . ?
C17 C21 1.529(3) . ?
C17 H17 0.9800 . ?
C18 C19 1.514(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 N3 1.482(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N3 1.494(4) . ?
C20 C21 1.529(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 O11 1.187(4) . ?
C22 O10 1.301(4) . ?
N3 H3N 0.81(4) . ?
O9 H9O 0.828(18) . ?
O10 H10O 0.855(10) . ?
O12 H12A 0.8400 . ?
O12 H12B 0.8400 . ?
O13 H13A 0.8400 . ?
O13 H13B 0.8400 . ?

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
O8 Cr1 O4 93.64(6) . . ?
O8 Cr1 O1 174.22(7) . . ?
O4 Cr1 O1 82.74(6) . . ?
O8 Cr1 O5 82.38(6) . . ?
O4 Cr1 O5 91.27(7) . . ?
O1 Cr1 O5 93.16(7) . . ?
O8 Cr1 N1 89.84(7) . . ?
O4 Cr1 N1 171.54(7) . . ?
O1 Cr1 N1 94.37(7) . . ?
O5 Cr1 N1 96.84(7) . . ?
O8 Cr1 N2 92.01(7) . . ?
O4 Cr1 N2 93.36(7) . . ?
O1 Cr1 N2 92.70(7) . . ?
O5 Cr1 N2 172.95(7) . . ?
N1 Cr1 N2 78.79(7) . . ?
N1 C1 C2 122.2(2) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C3 C2 C1 118.8(2) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C2 C3 C4 119.4(2) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 119.2(2) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N1 C5 C4 121.2(2) . . ?
N1 C5 C6 114.79(18) . . ?
C4 C5 C6 124.0(2) . . ?
N2 C6 C7 121.1(2) . . ?
N2 C6 C5 115.15(19) . . ?
C7 C6 C5 123.7(2) . . ?
C8 C7 C6 119.1(3) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C9 C8 C7 119.9(2) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 118.7(2) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
N2 C10 C9 121.7(2) . . ?
N2 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C1 N1 C5 119.18(19) . . ?
C1 N1 Cr1 125.33(15) . . ?
C5 N1 Cr1 115.26(14) . . ?
C10 N2 C6 119.44(19) . . ?
C10 N2 Cr1 125.35(16) . . ?
C6 N2 Cr1 115.16(14) . . ?
O2 C11 O1 126.1(2) . . ?
O2 C11 C12 119.9(2) . . ?
O1 C11 C12 114.00(18) . . ?
O3 C12 O4 124.7(2) . . ?
O3 C12 C11 121.5(2) . . ?
O4 C12 C11 113.87(18) . . ?
O6 C13 O5 125.0(2) . . ?
O6 C13 C14 121.5(2) . . ?
O5 C13 C14 113.48(18) . . ?
O7 C14 O8 125.4(2) . . ?
O7 C14 C13 121.1(2) . . ?
O8 C14 C13 113.56(18) . . ?
C11 O1 Cr1 114.59(14) . . ?
C12 O4 Cr1 114.70(14) . . ?
C13 O5 Cr1 114.74(13) . . ?
C14 O8 Cr1 115.30(13) . . ?
N3 C15 C16 109.7(2) . . ?
N3 C15 H15A 109.7 . . ?
C16 C15 H15A 109.7 . . ?
N3 C15 H15B 109.7 . . ?
C16 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
O9 C16 C22 108.04(19) . . ?
O9 C16 C17 111.91(18) . . ?
C22 C16 C17 109.7(2) . . ?
O9 C16 C15 107.46(19) . . ?
C22 C16 C15 112.1(2) . . ?
C17 C16 C15 107.68(19) . . ?
C18 C17 C21 108.9(2) . . ?
C18 C17 C16 108.23(19) . . ?
C21 C17 C16 109.8(2) . . ?
C18 C17 H17 110.0 . . ?
C21 C17 H17 110.0 . . ?
C16 C17 H17 110.0 . . ?
C19 C18 C17 108.9(2) . . ?
C19 C18 H18A 109.9 . . ?
C17 C18 H18A 109.9 . . ?
C19 C18 H18B 109.9 . . ?
C17 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
N3 C19 C18 109.3(2) . . ?
N3 C19 H19A 109.8 . . ?
C18 C19 H19A 109.8 . . ?
N3 C19 H19B 109.8 . . ?
C18 C19 H19B 109.8 . . ?
H19A C19 H19B 108.3 . . ?
N3 C20 C21 108.7(2) . . ?
N3 C20 H20A 110.0 . . ?
C21 C20 H20A 110.0 . . ?
N3 C20 H20B 110.0 . . ?
C21 C20 H20B 110.0 . . ?
H20A C20 H20B 108.3 . . ?
C20 C21 C17 108.9(2) . . ?
C20 C21 H21A 109.9 . . ?
C17 C21 H21A 109.9 . . ?
C20 C21 H21B 109.9 . . ?
C17 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
O11 C22 O10 124.9(3) . . ?
O11 C22 C16 123.2(3) . . ?
O10 C22 C16 111.9(3) . . ?
C15 N3 C19 111.5(2) . . ?
C15 N3 C20 109.8(2) . . ?
C19 N3 C20 110.1(3) . . ?
C15 N3 H3N 105.2 . . ?
C19 N3 H3N 112.5 . . ?
C20 N3 H3N 107.7 . . ?
C16 O9 H9O 107.8 . . ?
C22 O10 H10O 93.9 . . ?
H12A O12 H12B 104.0 . . ?
H13A O13 H13B 104.0 . . ?

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
N1 C1 C2 C3 0.6(4) . . . . ?
C1 C2 C3 C4 -0.5(4) . . . . ?
C2 C3 C4 C5 0.0(4) . . . . ?
C3 C4 C5 N1 0.6(4) . . . . ?
C3 C4 C5 C6 -177.6(2) . . . . ?
N1 C5 C6 N2 1.1(3) . . . . ?
C4 C5 C6 N2 179.3(2) . . . . ?
N1 C5 C6 C7 -177.0(2) . . . . ?
C4 C5 C6 C7 1.3(4) . . . . ?
N2 C6 C7 C8 -0.7(4) . . . . ?
C5 C6 C7 C8 177.2(3) . . . . ?
C6 C7 C8 C9 -1.3(5) . . . . ?
C7 C8 C9 C10 2.2(5) . . . . ?
C8 C9 C10 N2 -1.2(4) . . . . ?
C2 C1 N1 C5 0.0(3) . . . . ?
C2 C1 N1 Cr1 -174.15(18) . . . . ?
C4 C5 N1 C1 -0.5(3) . . . . ?
C6 C5 N1 C1 177.8(2) . . . . ?
C4 C5 N1 Cr1 174.16(19) . . . . ?
C6 C5 N1 Cr1 -7.5(2) . . . . ?
C9 C10 N2 C6 -0.8(3) . . . . ?
C9 C10 N2 Cr1 176.76(18) . . . . ?
C7 C6 N2 C10 1.8(4) . . . . ?
C5 C6 N2 C10 -176.3(2) . . . . ?
C7 C6 N2 Cr1 -176.0(2) . . . . ?
C5 C6 N2 Cr1 5.9(3) . . . . ?
O2 C11 C12 O3 4.4(4) . . . . ?
O1 C11 C12 O3 -177.1(2) . . . . ?
O2 C11 C12 O4 -175.0(3) . . . . ?
O1 C11 C12 O4 3.4(3) . . . . ?
O6 C13 C14 O7 0.5(3) . . . . ?
O5 C13 C14 O7 179.2(2) . . . . ?
O6 C13 C14 O8 -178.8(2) . . . . ?
O5 C13 C14 O8 -0.1(3) . . . . ?
O2 C11 O1 Cr1 176.7(3) . . . . ?
C12 C11 O1 Cr1 -1.7(2) . . . . ?
O3 C12 O4 Cr1 177.13(18) . . . . ?
C11 C12 O4 Cr1 -3.4(2) . . . . ?
O6 C13 O5 Cr1 173.50(19) . . . . ?
C14 C13 O5 Cr1 -5.2(2) . . . . ?
O7 C14 O8 Cr1 -173.87(19) . . . . ?
C13 C14 O8 Cr1 5.4(2) . . . . ?
N3 C15 C16 O9 127.6(2) . . . . ?
N3 C15 C16 C22 -113.8(2) . . . . ?
N3 C15 C16 C17 6.9(3) . . . . ?
O9 C16 C17 C18 -62.3(2) . . . . ?
C22 C16 C17 C18 177.8(2) . . . . ?
C15 C16 C17 C18 55.6(2) . . . . ?
O9 C16 C17 C21 179.0(2) . . . . ?
C22 C16 C17 C21 59.1(3) . . . . ?
C15 C16 C17 C21 -63.2(3) . . . . ?
C21 C17 C18 C19 52.8(3) . . . . ?
C16 C17 C18 C19 -66.6(3) . . . . ?
C17 C18 C19 N3 10.8(4) . . . . ?
N3 C20 C21 C17 9.8(4) . . . . ?
C18 C17 C21 C20 -64.8(3) . . . . ?
C16 C17 C21 C20 53.6(3) . . . . ?
O9 C16 C22 O11 129.1(4) . . . . ?
C17 C16 C22 O11 -108.7(4) . . . . ?
C15 C16 C22 O11 10.9(5) . . . . ?
O9 C16 C22 O10 -52.6(3) . . . . ?
C17 C16 C22 O10 69.6(3) . . . . ?
C15 C16 C22 O10 -170.8(2) . . . . ?
C16 C15 N3 C19 -64.6(3) . . . . ?
C16 C15 N3 C20 57.7(3) . . . . ?
C18 C19 N3 C15 54.1(4) . . . . ?
C18 C19 N3 C20 -68.0(4) . . . . ?
C21 C20 N3 C15 -67.8(3) . . . . ?
C21 C20 N3 C19 55.2(3) . . . . ?

_refine_diff_density_max         0.544
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.070



