# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_CrphenNbox-1
_database_code_depnum_ccdc_archive 'CCDC 1580889'
_audit_update_record             
;
2018-02-01 deposited with the CCDC.
2018-02-06 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT094_CrphenNbox-1        
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.68 Report
RESPONSE: Residual electron density peaks are located in the vicinity of
Nb atom. This is a result of absorption, and since we used Cu radiation,
absorption correction could only partially address this problem.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H36 Cr2 N8 Nb2 O22'
_chemical_formula_weight         1462.73

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'
Nb Nb -0.1121 2.4826 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_H-M_alt        'P 42 21 2'
_space_group_name_Hall           'P 4n 2n'

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

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

_cell_length_a                   14.770(5)
_cell_length_b                   14.770(5)
_cell_length_c                   12.583(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     2745(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4421
_cell_measurement_theta_min      3.545
_cell_measurement_theta_max      74.946
_cell_measurement_temperature    293(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.055
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_exptl_absorpt_coefficient_mu    7.31
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_T_max  0.99

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54179
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4323
_diffrn_reflns_number            15115
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_theta_min         4.233
_diffrn_reflns_theta_max         75.642
_diffrn_reflns_theta_full        67.68
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15

_reflns_number_total             2846
_reflns_number_gt                2032
_reflns_threshold_expression     'I > 2σ(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0658
_refine_ls_wR_factor_ref         0.1891
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_refine_ls_number_reflns         2846
_refine_ls_number_parameters     209
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0872P)²+4.3880P] where P=(Fo²+2Fc²)/3'
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_extinction_method     none
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(5)
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'


loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
C1 0.1765(9) 0.6251(12) 0.9236(12) 0.079(4) Uani d 1 . . C
H1 0.199553 0.625145 0.854848 0.094 Uiso calc 1 . . H
C2 0.0803(9) 0.6217(14) 0.9401(14) 0.093(5) Uani d 1 . . C
H2 0.041149 0.619186 0.882309 0.111 Uiso calc 1 . . H
C3 0.0472(10) 0.6223(15) 1.0403(13) 0.097(5) Uani d 1 . . C
H3 -0.015053 0.620791 1.051152 0.116 Uiso calc 1 . . H
C4 0.1050(8) 0.6251(10) 1.1267(12) 0.075(3) Uani d 1 . . C
C5 0.0758(8) 0.6268(10) 1.2319(12) 0.085(4) Uani d 1 . . C
H5 0.014048 0.627981 1.246349 0.103 Uiso calc 1 . . H
C6 0.1373(10) 0.6267(10) 1.3162(10) 0.078(3) Uani d 1 . . C
H6 0.117125 0.62933 1.386165 0.094 Uiso calc 1 . . H
C7 0.2317(9) 0.6223(9) 1.2930(10) 0.073(3) Uani d 1 . . C
C8 0.2963(10) 0.6144(11) 1.3733(11) 0.087(4) Uani d 1 . . C
H8 0.278529 0.610598 1.444067 0.105 Uiso calc 1 . . H
C9 0.3883(12) 0.6123(12) 1.3459(10) 0.088(3) Uani d 1 . . C
H9 0.432894 0.608533 1.397944 0.105 Uiso calc 1 . . H
C10 0.4110(8) 0.6160(9) 1.2381(13) 0.086(4) Uani d 1 . . C
H10 0.472006 0.612857 1.220187 0.103 Uiso calc 1 . . H
C11 0.2617(7) 0.6237(8) 1.1898(10) 0.063(3) Uani d 1 . . C
C12 0.1973(8) 0.6256(9) 1.1040(11) 0.066(3) Uani d 1 . . C
C13 0.3017(9) 0.3555(10) 1.2125(13) 0.080(4) Uani d 1 . . C
C14 0.2199(8) 0.3591(10) 1.1352(11) 0.078(4) Uani d 1 . . C
N1 0.2317(5) 0.6280(5) 1.0044(9) 0.0599(19) Uani d 1 . . N
N2 0.3522(6) 0.6236(6) 1.1607(7) 0.061(3) Uani d 1 . . N
O1 0.3684(5) 0.5010(3) 0.9924(7) 0.0643(17) Uani d 1 . . O
O2 0.3768(5) 0.3632(6) 1.1616(6) 0.070(2) Uani d 1 . . O
O3 0.2412(5) 0.3633(7) 1.0375(7) 0.082(3) Uani d 1 . . O
O4 0.2939(6) 0.3501(8) 1.3085(9) 0.107(3) Uani d 1 . . O
O5 0.1428(6) 0.3519(12) 1.1718(8) 0.127(5) Uani d 1 . . O
O6 0.3974(10) 0.3974(10) 0.5 0.176(9) Uani d 1 . . O
H6A 0.38(4) 0.35(2) 0.47(4) 0.5 Uiso d 1 . . H
Cr1 0.37172(9) 0.62828(9) 1 0.0536(5) Uani d 1 . . Cr
Nb1 0.38110(5) 0.38110(5) 1 0.0576(4) Uani d 1 . . Nb


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 . 1.304(16) ?
C1 C2 . 1.436(17) ?
C1 H1 . 0.93 ?
C2 C3 . 1.35(2) ?
C2 H2 . 0.93 ?
C3 C4 . 1.384(18) ?
C3 H3 . 0.93 ?
C4 C5 . 1.392(18) ?
C4 C12 . 1.393(16) ?
C5 C6 . 1.397(19) ?
C5 H5 . 0.93 ?
C6 C7 . 1.425(18) ?
C6 H6 . 0.93 ?
C7 C11 . 1.372(14) ?
C7 C8 . 1.394(19) ?
C8 C9 . 1.40(2) ?
C8 H8 . 0.93 ?
C9 C10 . 1.398(19) ?
C9 H9 . 0.93 ?
C10 N2 . 1.310(16) ?
C10 H10 . 0.93 ?
C11 N2 . 1.386(13) ?
C11 C12 . 1.440(17) ?
C12 N1 . 1.352(15) ?
C13 O4 . 1.215(16) ?
C13 O2 . 1.286(16) ?
C13 C14 . 1.552(17) ?
C14 O5 . 1.233(15) ?
C14 O3 . 1.271(14) ?
N1 Cr1 . 2.069(7) ?
N2 Cr1 . 2.043(9) ?
O1 Nb1 . 1.783(5) ?
O1 Cr1 . 1.883(5) ?
O2 Nb1 . 2.051(8) ?
O3 Nb1 . 2.135(8) ?
O6 H6A . 0.820(14) ?


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 120.5(14) . . ?
N1 C1 H1 119.8 . . ?
C2 C1 H1 119.8 . . ?
C3 C2 C1 119.5(15) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 120.7(13) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C3 C4 C5 123.8(13) . . ?
C3 C4 C12 116.3(14) . . ?
C5 C4 C12 119.9(13) . . ?
C4 C5 C6 121.4(12) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C7 118.7(11) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
C11 C7 C8 117.7(12) . . ?
C11 C7 C6 120.6(11) . . ?
C8 C7 C6 121.6(13) . . ?
C7 C8 C9 119.2(13) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C10 C9 C8 118.0(13) . . ?
C10 C9 H9 121 . . ?
C8 C9 H9 121 . . ?
N2 C10 C9 124.5(12) . . ?
N2 C10 H10 117.8 . . ?
C9 C10 H10 117.8 . . ?
C7 C11 N2 124.2(10) . . ?
C7 C11 C12 119.8(10) . . ?
N2 C11 C12 116.0(10) . . ?
N1 C12 C4 123.9(13) . . ?
N1 C12 C11 116.6(10) . . ?
C4 C12 C11 119.5(12) . . ?
O4 C13 O2 125.7(13) . . ?
O4 C13 C14 123.4(13) . . ?
O2 C13 C14 110.8(13) . . ?
O5 C14 O3 126.5(12) . . ?
O5 C14 C13 118.8(13) . . ?
O3 C14 C13 114.6(11) . . ?
C1 N1 C12 119.1(10) . . ?
C1 N1 Cr1 127.2(9) . . ?
C12 N1 Cr1 113.6(8) . . ?
C10 N2 C11 116.2(10) . . ?
C10 N2 Cr1 130.2(8) . . ?
C11 N2 Cr1 113.5(7) . . ?
Nb1 O1 Cr1 170.4(5) . . ?
C13 O2 Nb1 122.2(8) . . ?
C14 O3 Nb1 117.3(7) . . ?
O1 Cr1 N2 90.8(4) . . ?
O1 Cr1 N1 88.5(3) . . ?
N2 Cr1 N1 80.3(4) . . ?
O1 Nb1 O1 102.2(5) 6_557 . ?
O1 Nb1 O2 100.3(4) 6_557 6_557 ?
O1 Nb1 O2 87.9(3) . 6_557 ?
O1 Nb1 O2 87.9(3) 6_557 . ?
O1 Nb1 O2 100.3(4) . . ?
O2 Nb1 O2 167.0(4) 6_557 . ?
O1 Nb1 O3 91.9(4) 6_557 6_557 ?
O1 Nb1 O3 159.4(4) . 6_557 ?
O2 Nb1 O3 74.6(3) 6_557 6_557 ?
O2 Nb1 O3 95.2(3) . 6_557 ?
O1 Nb1 O3 159.4(4) 6_557 . ?
O1 Nb1 O3 91.9(4) . . ?
O2 Nb1 O3 95.2(3) 6_557 . ?
O2 Nb1 O3 74.6(3) . . ?
O3 Nb1 O3 79.1(6) 6_557 . ?

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(3) . . . . ?
C1 C2 C3 C4 -1(4) . . . . ?
C2 C3 C4 C5 179.4(19) . . . . ?
C2 C3 C4 C12 -1(3) . . . . ?
C3 C4 C5 C6 177.9(18) . . . . ?
C12 C4 C5 C6 -2(2) . . . . ?
C4 C5 C6 C7 -2(2) . . . . ?
C5 C6 C7 C11 4(2) . . . . ?
C5 C6 C7 C8 -174.6(15) . . . . ?
C11 C7 C8 C9 3(2) . . . . ?
C6 C7 C8 C9 -178.7(15) . . . . ?
C7 C8 C9 C10 -2(3) . . . . ?
C8 C9 C10 N2 2(3) . . . . ?
C8 C7 C11 N2 -4(2) . . . . ?
C6 C7 C11 N2 177.1(12) . . . . ?
C8 C7 C11 C12 175.8(12) . . . . ?
C6 C7 C11 C12 -3(2) . . . . ?
C3 C4 C12 N1 3(2) . . . . ?
C5 C4 C12 N1 -177.1(13) . . . . ?
C3 C4 C12 C11 -176.8(16) . . . . ?
C5 C4 C12 C11 3(2) . . . . ?
C7 C11 C12 N1 179.2(11) . . . . ?
N2 C11 C12 N1 -0.7(16) . . . . ?
C7 C11 C12 C4 -1(2) . . . . ?
N2 C11 C12 C4 179.6(12) . . . . ?
O4 C13 C14 O5 -3(2) . . . . ?
O2 C13 C14 O5 179.5(16) . . . . ?
O4 C13 C14 O3 -178.9(15) . . . . ?
O2 C13 C14 O3 3.9(19) . . . . ?
C2 C1 N1 C12 2(2) . . . . ?
C2 C1 N1 Cr1 177.6(13) . . . . ?
C4 C12 N1 C1 -3.7(17) . . . . ?
C11 C12 N1 C1 176.5(14) . . . . ?
C4 C12 N1 Cr1 179.8(11) . . . . ?
C11 C12 N1 Cr1 0.1(14) . . . . ?
C9 C10 N2 C11 -3(2) . . . . ?
C9 C10 N2 Cr1 -179.0(12) . . . . ?
C7 C11 N2 C10 4.4(18) . . . . ?
C12 C11 N2 C10 -175.7(11) . . . . ?
C7 C11 N2 Cr1 -178.9(10) . . . . ?
C12 C11 N2 Cr1 0.9(13) . . . . ?
O4 C13 O2 Nb1 -175.5(12) . . . . ?
C14 C13 O2 Nb1 1.6(16) . . . . ?
O5 C14 O3 Nb1 177.5(15) . . . . ?
C13 C14 O3 Nb1 -7.3(16) . . . . ?

_refine_diff_density_max         2.014
_refine_diff_density_min         -0.43
_refine_diff_density_rms         0.098


####################################################################### 
# 
# 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_CrtrpyNbox-2
_database_code_depnum_ccdc_archive 'CCDC 1580890'
_audit_update_record             
;
2018-02-01 deposited with the CCDC.
2018-02-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H34 Cr2 N6 Nb2 O26'
_chemical_formula_weight         1280.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   11.0343(9)
_cell_length_b                   17.4862(14)
_cell_length_c                   11.9713(7)
_cell_angle_alpha                90
_cell_angle_beta                 90.766(3)
_cell_angle_gamma                90
_cell_volume                     2309.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9891
_cell_measurement_theta_min      4.664
_cell_measurement_theta_max      54.91

_exptl_crystal_description       stick
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_F_000             1284
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.069
_exptl_absorpt_coefficient_mu    1.043
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  
'D8 Venture Bruker with double microsource Ag-Mo'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51049
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_av_R_equivalents  0.1147
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.329
_diffrn_reflns_theta_max         27.547
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5310
_reflns_number_gt                4154
_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       'Bruker Instrument Service v4.2.2'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'Sir 92'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0239P)²+4.7729P] 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         5310
_refine_ls_number_parameters     352
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0851
_refine_ls_wR_factor_gt          0.0769
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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 0.6943(3) -0.08812(18) 0.7030(3) 0.0188(7) Uani 1 1 d . . . . .
H1 H 0.701667 -0.038165 0.677253 0.023 Uiso 1 1 calc R U . . .
C2 C 0.7139(3) -0.1026(2) 0.8154(3) 0.0256(8) Uani 1 1 d . . . . .
H2 H 0.731794 -0.062961 0.864737 0.031 Uiso 1 1 calc R U . . .
C3 C 0.7065(3) -0.1776(2) 0.8532(3) 0.0289(8) Uani 1 1 d . . . . .
H3 H 0.721113 -0.188926 0.928072 0.035 Uiso 1 1 calc R U . . .
C4 C 0.6771(3) -0.2351(2) 0.7786(3) 0.0256(8) Uani 1 1 d . . . . .
H4 H 0.672104 -0.285569 0.802522 0.031 Uiso 1 1 calc R U . . .
C5 C 0.6551(3) -0.21649(18) 0.6673(3) 0.0162(6) Uani 1 1 d . . . . .
C6 C 0.6167(3) -0.27258(18) 0.5810(3) 0.0176(7) Uani 1 1 d . . . . .
C7 C 0.6042(4) -0.3510(2) 0.5946(3) 0.0287(8) Uani 1 1 d . . . . .
H7 H 0.619934 -0.374140 0.663228 0.034 Uiso 1 1 calc R U . . .
C8 C 0.5677(4) -0.3938(2) 0.5030(3) 0.0336(9) Uani 1 1 d . . . . .
H8 H 0.559973 -0.446535 0.510378 0.040 Uiso 1 1 calc R U . . .
C9 C 0.5424(4) -0.36016(19) 0.4007(3) 0.0272(8) Uani 1 1 d . . . . .
H9 H 0.517387 -0.389364 0.339648 0.033 Uiso 1 1 calc R U . . .
C10 C 0.5554(3) -0.28141(18) 0.3921(3) 0.0180(7) Uani 1 1 d . . . . .
C11 C 0.5352(3) -0.23394(19) 0.2918(3) 0.0183(7) Uani 1 1 d . . . . .
C12 C 0.4855(3) -0.2607(2) 0.1926(3) 0.0255(8) Uani 1 1 d . . . . .
H12 H 0.460810 -0.311412 0.186068 0.031 Uiso 1 1 calc R U . . .
C13 C 0.4730(4) -0.2112(2) 0.1036(3) 0.0316(9) Uani 1 1 d . . . . .
H13 H 0.438719 -0.228223 0.036728 0.038 Uiso 1 1 calc R U . . .
C14 C 0.5111(4) -0.1363(2) 0.1136(3) 0.0294(8) Uani 1 1 d . . . . .
H14 H 0.505548 -0.102915 0.053236 0.035 Uiso 1 1 calc R U . . .
C15 C 0.5582(3) -0.1118(2) 0.2161(3) 0.0226(7) Uani 1 1 d . . . . .
H15 H 0.581912 -0.061080 0.224406 0.027 Uiso 1 1 calc R U . . .
C16 C 0.6790(3) 0.22485(18) 0.3104(3) 0.0158(6) Uani 1 1 d . . . . .
C17 C 0.6482(3) 0.15894(18) 0.2271(3) 0.0173(7) Uani 1 1 d . . . . .
C18 C 0.9481(3) 0.07902(17) 0.4521(3) 0.0151(6) Uani 1 1 d . . . . .
C19 C 0.9020(3) 0.09283(17) 0.5714(3) 0.0165(7) Uani 1 1 d . . . . .
N1 N 0.6652(2) -0.14316(14) 0.6298(2) 0.0137(5) Uani 1 1 d . . . . .
N2 N 0.5927(2) -0.24027(14) 0.4815(2) 0.0148(5) Uani 1 1 d . . . . .
N3 N 0.5702(2) -0.15953(15) 0.3028(2) 0.0167(6) Uani 1 1 d . . . . .
O1 O 0.5357(2) 0.10236(12) 0.50429(18) 0.0149(5) Uani 1 1 d . . . . .
O2 O 0.6690(2) -0.02450(12) 0.43725(18) 0.0151(4) Uani 1 1 d . . . . .
O3 O 0.7037(2) 0.20095(12) 0.40866(18) 0.0174(5) Uani 1 1 d . . . . .
O4 O 0.6776(2) 0.29136(13) 0.27812(19) 0.0225(5) Uani 1 1 d . . . . .
O5 O 0.6389(3) 0.16959(14) 0.12786(19) 0.0303(6) Uani 1 1 d . . . . .
O6 O 0.6341(2) 0.09264(12) 0.27569(18) 0.0171(5) Uani 1 1 d . . . . .
O7 O 0.86285(19) 0.07293(12) 0.37843(17) 0.0157(5) Uani 1 1 d . . . . .
O8 O 1.0575(2) 0.07632(13) 0.43533(19) 0.0200(5) Uani 1 1 d . . . . .
O9 O 0.9713(2) 0.10388(15) 0.6486(2) 0.0266(6) Uani 1 1 d . . . . .
O10 O 0.7833(2) 0.09369(12) 0.57947(18) 0.0157(5) Uani 1 1 d . . . . .
O11 O 0.7969(2) -0.15997(12) 0.43071(18) 0.0157(5) Uani 1 1 d D . . . .
H11A H 0.806(3) -0.1767(19) 0.3646(14) 0.024 Uiso 1 1 d D U . . .
H11B H 0.848(3) -0.1284(17) 0.456(3) 0.024 Uiso 1 1 d D U . . .
O12 O 0.6812(3) 0.01334(18) 0.0283(3) 0.0488(8) Uani 1 1 d D . . . .
H12A H 0.653(5) 0.0554(18) 0.054(4) 0.073 Uiso 1 1 d D U . . .
H12B H 0.732(4) -0.012(2) 0.070(3) 0.073 Uiso 1 1 d D U . . .
O13 O 0.8579(3) -0.03982(18) 0.1780(3) 0.0456(8) Uani 1 1 d D . . . .
H13A H 0.877(4) -0.0160(19) 0.238(2) 0.068 Uiso 1 1 d D U . . .
H13B H 0.854(5) -0.0885(7) 0.172(4) 0.068 Uiso 1 1 d D U . . .
Cr1 Cr 0.62702(5) -0.12933(3) 0.46060(4) 0.01045(11) Uani 1 1 d . . . . .
Nb1 Nb 0.67623(3) 0.07792(2) 0.44096(2) 0.01119(8) 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 1.338(4) . ?
C1 C2 1.384(5) . ?
C2 C3 1.390(5) . ?
C3 C4 1.380(5) . ?
C4 C5 1.390(5) . ?
C5 N1 1.363(4) . ?
C5 C6 1.482(5) . ?
C6 N2 1.341(4) . ?
C6 C7 1.389(5) . ?
C7 C8 1.382(5) . ?
C8 C9 1.384(5) . ?
C9 C10 1.389(5) . ?
C10 N2 1.350(4) . ?
C10 C11 1.474(5) . ?
C11 N3 1.363(4) . ?
C11 C12 1.383(4) . ?
C12 C13 1.379(5) . ?
C13 C14 1.380(5) . ?
C14 C15 1.394(5) . ?
C15 N3 1.337(4) . ?
C16 O4 1.226(4) . ?
C16 O3 1.275(4) . ?
C16 C17 1.558(4) . ?
C17 O5 1.206(4) . ?
C17 O6 1.307(4) . ?
C18 O8 1.228(4) . ?
C18 O7 1.285(4) . ?
C18 C19 1.541(4) . ?
C19 O9 1.208(4) . ?
C19 O10 1.315(4) . ?
N1 Cr1 2.077(3) . ?
N2 Cr1 1.993(3) . ?
N3 Cr1 2.052(3) . ?
O1 Nb1 1.787(2) . ?
O1 Cr1 1.909(2) 3_656 ?
O2 Nb1 1.793(2) . ?
O2 Cr1 1.912(2) . ?
O3 Nb1 2.207(2) . ?
O6 Nb1 2.043(2) . ?
O7 Nb1 2.202(2) . ?
O10 Nb1 2.042(2) . ?
O11 Cr1 1.987(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 122.6(3) . . ?
C1 C2 C3 118.7(3) . . ?
C4 C3 C2 119.4(3) . . ?
C3 C4 C5 119.1(3) . . ?
N1 C5 C4 121.4(3) . . ?
N1 C5 C6 114.7(3) . . ?
C4 C5 C6 123.9(3) . . ?
N2 C6 C7 120.1(3) . . ?
N2 C6 C5 113.0(3) . . ?
C7 C6 C5 126.9(3) . . ?
C8 C7 C6 118.1(3) . . ?
C7 C8 C9 121.7(3) . . ?
C8 C9 C10 117.9(3) . . ?
N2 C10 C9 120.0(3) . . ?
N2 C10 C11 112.8(3) . . ?
C9 C10 C11 127.2(3) . . ?
N3 C11 C12 121.0(3) . . ?
N3 C11 C10 114.8(3) . . ?
C12 C11 C10 124.2(3) . . ?
C13 C12 C11 119.0(3) . . ?
C12 C13 C14 120.2(3) . . ?
C13 C14 C15 118.5(3) . . ?
N3 C15 C14 121.6(3) . . ?
O4 C16 O3 127.1(3) . . ?
O4 C16 C17 119.9(3) . . ?
O3 C16 C17 113.0(3) . . ?
O5 C17 O6 124.5(3) . . ?
O5 C17 C16 122.1(3) . . ?
O6 C17 C16 113.5(3) . . ?
O8 C18 O7 126.7(3) . . ?
O8 C18 C19 119.6(3) . . ?
O7 C18 C19 113.7(3) . . ?
O9 C19 O10 124.2(3) . . ?
O9 C19 C18 121.5(3) . . ?
O10 C19 C18 114.3(3) . . ?
C1 N1 C5 118.8(3) . . ?
C1 N1 Cr1 126.8(2) . . ?
C5 N1 Cr1 114.4(2) . . ?
C6 N2 C10 122.3(3) . . ?
C6 N2 Cr1 119.1(2) . . ?
C10 N2 Cr1 118.4(2) . . ?
C15 N3 C11 119.7(3) . . ?
C15 N3 Cr1 125.5(2) . . ?
C11 N3 Cr1 114.7(2) . . ?
Nb1 O1 Cr1 167.61(13) . 3_656 ?
Nb1 O2 Cr1 164.72(14) . . ?
C16 O3 Nb1 116.93(19) . . ?
C17 O6 Nb1 121.0(2) . . ?
C18 O7 Nb1 116.28(19) . . ?
C19 O10 Nb1 120.31(19) . . ?
O1 Cr1 O2 91.47(9) 3_656 . ?
O1 Cr1 O11 177.36(10) 3_656 . ?
O2 Cr1 O11 90.08(9) . . ?
O1 Cr1 N2 91.83(10) 3_656 . ?
O2 Cr1 N2 176.67(10) . . ?
O11 Cr1 N2 86.64(10) . . ?
O1 Cr1 N3 89.39(10) 3_656 . ?
O2 Cr1 N3 100.59(10) . . ?
O11 Cr1 N3 92.43(10) . . ?
N2 Cr1 N3 78.99(11) . . ?
O1 Cr1 N1 89.60(10) 3_656 . ?
O2 Cr1 N1 101.99(10) . . ?
O11 Cr1 N1 87.99(10) . . ?
N2 Cr1 N1 78.49(10) . . ?
N3 Cr1 N1 157.41(11) . . ?
O1 Nb1 O2 102.16(10) . . ?
O1 Nb1 O10 96.84(9) . . ?
O2 Nb1 O10 100.38(9) . . ?
O1 Nb1 O6 101.14(9) . . ?
O2 Nb1 O6 95.30(9) . . ?
O10 Nb1 O6 153.04(9) . . ?
O1 Nb1 O7 166.99(9) . . ?
O2 Nb1 O7 89.64(9) . . ?
O10 Nb1 O7 75.39(8) . . ?
O6 Nb1 O7 82.96(9) . . ?
O1 Nb1 O3 87.90(9) . . ?
O2 Nb1 O3 167.20(9) . . ?
O10 Nb1 O3 86.06(8) . . ?
O6 Nb1 O3 74.79(8) . . ?
O7 Nb1 O3 81.24(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 1.9(5) . . . . ?
C1 C2 C3 C4 -1.5(6) . . . . ?
C2 C3 C4 C5 -0.3(6) . . . . ?
C3 C4 C5 N1 1.8(5) . . . . ?
C3 C4 C5 C6 -176.7(3) . . . . ?
N1 C5 C6 N2 -3.1(4) . . . . ?
C4 C5 C6 N2 175.5(3) . . . . ?
N1 C5 C6 C7 177.1(3) . . . . ?
C4 C5 C6 C7 -4.3(6) . . . . ?
N2 C6 C7 C8 0.5(5) . . . . ?
C5 C6 C7 C8 -179.7(3) . . . . ?
C6 C7 C8 C9 -0.9(6) . . . . ?
C7 C8 C9 C10 0.4(6) . . . . ?
C8 C9 C10 N2 0.5(5) . . . . ?
C8 C9 C10 C11 179.1(3) . . . . ?
N2 C10 C11 N3 7.0(4) . . . . ?
C9 C10 C11 N3 -171.6(3) . . . . ?
N2 C10 C11 C12 -173.3(3) . . . . ?
C9 C10 C11 C12 8.1(6) . . . . ?
N3 C11 C12 C13 0.9(5) . . . . ?
C10 C11 C12 C13 -178.8(3) . . . . ?
C11 C12 C13 C14 0.8(6) . . . . ?
C12 C13 C14 C15 -2.2(6) . . . . ?
C13 C14 C15 N3 1.9(6) . . . . ?
O4 C16 C17 O5 10.5(5) . . . . ?
O3 C16 C17 O5 -169.6(3) . . . . ?
O4 C16 C17 O6 -169.7(3) . . . . ?
O3 C16 C17 O6 10.2(4) . . . . ?
O8 C18 C19 O9 2.7(5) . . . . ?
O7 C18 C19 O9 -175.9(3) . . . . ?
O8 C18 C19 O10 -179.2(3) . . . . ?
O7 C18 C19 O10 2.1(4) . . . . ?
C2 C1 N1 C5 -0.4(5) . . . . ?
C2 C1 N1 Cr1 177.6(3) . . . . ?
C4 C5 N1 C1 -1.5(5) . . . . ?
C6 C5 N1 C1 177.2(3) . . . . ?
C4 C5 N1 Cr1 -179.7(3) . . . . ?
C6 C5 N1 Cr1 -1.1(3) . . . . ?
C7 C6 N2 C10 0.4(5) . . . . ?
C5 C6 N2 C10 -179.4(3) . . . . ?
C7 C6 N2 Cr1 -174.0(3) . . . . ?
C5 C6 N2 Cr1 6.1(4) . . . . ?
C9 C10 N2 C6 -0.9(5) . . . . ?
C11 C10 N2 C6 -179.7(3) . . . . ?
C9 C10 N2 Cr1 173.5(3) . . . . ?
C11 C10 N2 Cr1 -5.2(4) . . . . ?
C14 C15 N3 C11 -0.3(5) . . . . ?
C14 C15 N3 Cr1 -175.6(3) . . . . ?
C12 C11 N3 C15 -1.1(5) . . . . ?
C10 C11 N3 C15 178.6(3) . . . . ?
C12 C11 N3 Cr1 174.7(3) . . . . ?
C10 C11 N3 Cr1 -5.6(4) . . . . ?
O4 C16 O3 Nb1 173.0(3) . . . . ?
C17 C16 O3 Nb1 -7.0(3) . . . . ?
O5 C17 O6 Nb1 170.9(3) . . . . ?
C16 C17 O6 Nb1 -9.0(4) . . . . ?
O8 C18 O7 Nb1 178.6(3) . . . . ?
C19 C18 O7 Nb1 -2.9(3) . . . . ?
O9 C19 O10 Nb1 177.8(2) . . . . ?
C18 C19 O10 Nb1 -0.2(3) . . . . ?
Cr1 O1 Nb1 O2 -91.3(6) 3_656 . . . ?
Cr1 O1 Nb1 O10 166.5(6) 3_656 . . . ?
Cr1 O1 Nb1 O6 6.7(6) 3_656 . . . ?
Cr1 O1 Nb1 O7 114.0(6) 3_656 . . . ?
Cr1 O1 Nb1 O3 80.8(6) 3_656 . . . ?
Cr1 O2 Nb1 O1 -14.8(5) . . . . ?
Cr1 O2 Nb1 O10 84.6(5) . . . . ?
Cr1 O2 Nb1 O6 -117.4(5) . . . . ?
Cr1 O2 Nb1 O7 159.7(5) . . . . ?
Cr1 O2 Nb1 O3 -156.0(4) . . . . ?

_refine_diff_density_max         0.564
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.107

####################################################################### 
# 
# 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_CrtrpyNbox-3
_database_code_depnum_ccdc_archive 'CCDC 1580891'
_audit_update_record             
;
2018-02-01 deposited with the CCDC.
2018-02-06 downloaded from the CCDC.
;
# start Validation Reply Form

_vrf_PLAT306_CrtrpyNbox-3        
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......      O26 Check   
RESPONSE:  Hydrogen atoms on water molecule O26 have not been determined.
;
_vrf_PLAT430_CrtrpyNbox-3        
;
PROBLEM: Short Inter D...A Contact O3     ..O25     .       2.82 Ang.      
RESPONSE:  This alert is due to missing (not determined) hydrogen
atoms on water molecules O24, O25 and O26.
;
# end Validation Reply Form 

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C55 H35 Cr3 N9 Nb O25.19'
_chemical_formula_weight         1473.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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                   14.206(5)
_cell_length_b                   14.903(5)
_cell_length_c                   15.710(5)
_cell_angle_alpha                71.440(5)
_cell_angle_beta                 88.232(5)
_cell_angle_gamma                68.059(5)
_cell_volume                     2909.9(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1017
_cell_measurement_theta_min      4.098
_cell_measurement_theta_max      49.98

_exptl_crystal_description       stick
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_F_000             1498
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.059
_exptl_absorpt_coefficient_mu    0.835
_shelx_estimated_absorpt_T_min   0.814
_shelx_estimated_absorpt_T_max   0.952
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  
'D8 Venture Bruker with double microsource Ag-Mo'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            131815
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_av_R_equivalents  0.1039
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.971
_diffrn_reflns_theta_max         26.639
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11695
_reflns_number_gt                8959
_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       'Bruker Instrument Service v4.2.2'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    
;SIR92: Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
 Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
;
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0330P)²+2.8349P] 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         11695
_refine_ls_number_parameters     855
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.0941
_refine_ls_wR_factor_gt          0.0856
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 -0.0675(3) -0.0345(3) 0.4119(3) 0.0546(10) Uani 1 1 d . . . . .
H1 H -0.099301 0.032855 0.411081 0.066 Uiso 1 1 calc R U . . .
C2 C -0.0596(3) -0.1130(4) 0.4916(3) 0.0720(13) Uani 1 1 d . . . . .
H2 H -0.084430 -0.098605 0.543212 0.086 Uiso 1 1 calc R U . . .
C3 C -0.0150(3) -0.2105(4) 0.4923(3) 0.0728(13) Uani 1 1 d . . . . .
H3 H -0.008114 -0.264738 0.544806 0.087 Uiso 1 1 calc R U . . .
C4 C 0.0205(3) -0.2291(3) 0.4141(3) 0.0573(10) Uani 1 1 d . . . . .
H4 H 0.049346 -0.296157 0.413807 0.069 Uiso 1 1 calc R U . . .
C5 C 0.0137(2) -0.1488(2) 0.3361(2) 0.0394(8) Uani 1 1 d . . . . .
C6 C 0.0583(2) -0.1585(2) 0.2515(2) 0.0375(7) Uani 1 1 d . . . . .
C7 C 0.1075(3) -0.2476(3) 0.2325(3) 0.0504(9) Uani 1 1 d . . . . .
H7 H 0.110212 -0.310058 0.272450 0.061 Uiso 1 1 calc R U . . .
C8 C 0.1532(3) -0.2427(3) 0.1526(3) 0.0565(11) Uani 1 1 d . . . . .
H8 H 0.186977 -0.303091 0.139991 0.068 Uiso 1 1 calc R U . . .
C9 C 0.1505(3) -0.1517(3) 0.0913(3) 0.0493(9) Uani 1 1 d . . . . .
H9 H 0.182915 -0.149863 0.038750 0.059 Uiso 1 1 calc R U . . .
C10 C 0.0973(2) -0.0633(2) 0.1114(2) 0.0367(7) Uani 1 1 d . . . . .
C11 C 0.0833(2) 0.0408(2) 0.0548(2) 0.0377(7) Uani 1 1 d . . . . .
C12 C 0.1212(3) 0.0669(3) -0.0293(2) 0.0502(9) Uani 1 1 d . . . . .
H12 H 0.159595 0.016218 -0.052982 0.060 Uiso 1 1 calc R U . . .
C13 C 0.1011(3) 0.1682(4) -0.0762(3) 0.0629(11) Uani 1 1 d . . . . .
H13 H 0.124737 0.187171 -0.132367 0.075 Uiso 1 1 calc R U . . .
C14 C 0.0458(3) 0.2406(3) -0.0391(3) 0.0649(11) Uani 1 1 d . . . . .
H14 H 0.031246 0.309685 -0.069588 0.078 Uiso 1 1 calc R U . . .
C15 C 0.0112(3) 0.2097(3) 0.0452(3) 0.0526(9) Uani 1 1 d . . . . .
H15 H -0.025401 0.259701 0.070260 0.063 Uiso 1 1 calc R U . . .
C16 C 0.2781(3) 0.2492(3) 0.0584(2) 0.0493(9) Uani 1 1 d . . . . .
H16 H 0.209278 0.287642 0.058404 0.059 Uiso 1 1 calc R U . . .
C17 C 0.3117(4) 0.2288(4) -0.0202(3) 0.0670(12) Uani 1 1 d . . . . .
H17 H 0.266405 0.253541 -0.071469 0.080 Uiso 1 1 calc R U . . .
C18 C 0.4117(4) 0.1723(4) -0.0206(4) 0.0803(14) Uani 1 1 d . . . . .
H18 H 0.435955 0.158305 -0.072477 0.096 Uiso 1 1 calc R U . . .
C19 C 0.4772(4) 0.1358(4) 0.0563(4) 0.0747(14) Uani 1 1 d . . . . .
H19 H 0.545776 0.096314 0.056803 0.090 Uiso 1 1 calc R U . . .
C20 C 0.4399(3) 0.1583(3) 0.1344(3) 0.0496(9) Uani 1 1 d . . . . .
C21 C 0.5001(3) 0.1226(3) 0.2213(3) 0.0548(10) Uani 1 1 d . . . . .
C22 C 0.6041(3) 0.0634(3) 0.2404(4) 0.0779(15) Uani 1 1 d . . . . .
H22 H 0.642388 0.041637 0.196462 0.093 Uiso 1 1 calc R U . . .
C23 C 0.6480(4) 0.0385(4) 0.3233(5) 0.0916(18) Uani 1 1 d . . . . .
H23 H 0.717648 -0.000437 0.335642 0.110 Uiso 1 1 calc R U . . .
C24 C 0.5948(4) 0.0679(3) 0.3918(4) 0.0829(17) Uani 1 1 d . . . . .
H24 H 0.627193 0.048772 0.449017 0.099 Uiso 1 1 calc R U . . .
C25 C 0.4881(3) 0.1288(3) 0.3709(3) 0.0574(11) Uani 1 1 d . . . . .
C26 C 0.4156(4) 0.1698(3) 0.4306(3) 0.0601(12) Uani 1 1 d . . . . .
C27 C 0.4386(5) 0.1564(4) 0.5202(3) 0.0865(18) Uani 1 1 d . . . . .
H27 H 0.505632 0.120175 0.546328 0.104 Uiso 1 1 calc R U . . .
C28 C 0.3649(6) 0.1953(4) 0.5701(3) 0.095(2) Uani 1 1 d . . . . .
H28 H 0.381264 0.185505 0.630150 0.114 Uiso 1 1 calc R U . . .
C29 C 0.2646(5) 0.2501(4) 0.5314(3) 0.0859(17) Uani 1 1 d . . . . .
H29 H 0.212848 0.276523 0.564941 0.103 Uiso 1 1 calc R U . . .
C30 C 0.2437(4) 0.2643(3) 0.4395(3) 0.0622(11) Uani 1 1 d . . . . .
H30 H 0.177284 0.301811 0.412233 0.075 Uiso 1 1 calc R U . . .
C31 C 0.7416(4) 0.5078(3) 0.5218(3) 0.0727(13) Uani 1 1 d . . . . .
H31 H 0.812182 0.475824 0.533882 0.087 Uiso 1 1 calc R U . . .
C32 C 0.6827(7) 0.5303(5) 0.5916(4) 0.110(2) Uani 1 1 d . . . . .
H32 H 0.713693 0.512511 0.649138 0.133 Uiso 1 1 calc R U . . .
C33 C 0.5795(8) 0.5785(5) 0.5734(6) 0.128(3) Uani 1 1 d . . . . .
H33 H 0.539114 0.595378 0.618094 0.153 Uiso 1 1 calc R U . . .
C34 C 0.5357(5) 0.6022(4) 0.4879(5) 0.099(2) Uani 1 1 d . . . . .
H34 H 0.465227 0.634371 0.474754 0.119 Uiso 1 1 calc R U . . .
C35 C 0.5975(3) 0.5775(3) 0.4212(3) 0.0647(12) Uani 1 1 d . . . . .
C36 C 0.5588(3) 0.5974(3) 0.3276(4) 0.0643(12) Uani 1 1 d . . . . .
C37 C 0.4566(4) 0.6447(4) 0.2888(6) 0.108(2) Uani 1 1 d . . . . .
H37 H 0.403087 0.669809 0.321352 0.130 Uiso 1 1 calc R U . . .
C38 C 0.4396(5) 0.6520(5) 0.1990(6) 0.117(3) Uani 1 1 d . . . . .
H38 H 0.373024 0.684022 0.171685 0.141 Uiso 1 1 calc R U . . .
C39 C 0.5169(5) 0.6139(4) 0.1493(5) 0.108(2) Uani 1 1 d . . . . .
H39 H 0.502605 0.619387 0.090022 0.130 Uiso 1 1 calc R U . . .
C40 C 0.6156(4) 0.5678(3) 0.1893(3) 0.0681(13) Uani 1 1 d . . . . .
C41 C 0.7098(4) 0.5222(3) 0.1499(3) 0.0625(11) Uani 1 1 d . . . . .
C42 C 0.7121(6) 0.5102(4) 0.0625(4) 0.0987(19) Uani 1 1 d . . . . .
H42 H 0.652470 0.529809 0.026351 0.118 Uiso 1 1 calc R U . . .
C43 C 0.8063(7) 0.4685(4) 0.0349(4) 0.107(2) Uani 1 1 d . . . . .
H43 H 0.810383 0.457375 -0.020331 0.128 Uiso 1 1 calc R U . . .
C44 C 0.8947(6) 0.4429(4) 0.0862(4) 0.101(2) Uani 1 1 d . . . . .
H44 H 0.957905 0.419720 0.064571 0.122 Uiso 1 1 calc R U . . .
C45 C 0.8870(4) 0.4524(3) 0.1708(3) 0.0731(13) Uani 1 1 d . . . . .
H45 H 0.946474 0.431493 0.207581 0.088 Uiso 1 1 calc R U . . .
C46 C -0.2220(2) 0.1711(3) 0.1543(2) 0.0412(8) Uani 1 1 d . . . . .
C47 C -0.1929(2) 0.2222(2) 0.2164(2) 0.0347(7) Uani 1 1 d . . . . .
C48 C 0.2595(2) -0.1994(2) 0.4202(2) 0.0353(7) Uani 1 1 d . . . . .
C49 C 0.2558(3) -0.1360(2) 0.4818(2) 0.0397(8) Uani 1 1 d . . . . .
C50 C 0.4374(2) -0.0923(3) 0.2295(2) 0.0432(8) Uani 1 1 d . . . . .
C51 C 0.3522(3) -0.0538(3) 0.1504(2) 0.0425(8) Uani 1 1 d . . . . .
C52 C 0.2626(3) 0.4448(3) 0.1948(2) 0.0532(10) Uani 1 1 d . . . . .
C53 C 0.1571(3) 0.4363(3) 0.1909(2) 0.0549(10) Uani 1 1 d . . . . .
C54 C 0.9610(3) 0.5170(4) 0.3657(3) 0.0630(11) Uani 1 1 d . . . . .
C55 C 0.8859(3) 0.6252(3) 0.3124(3) 0.0538(10) Uani 1 1 d . . . . .
N1 N -0.03140(19) -0.05124(19) 0.33586(19) 0.0377(6) Uani 1 1 d . . . . .
N2 N 0.05255(18) -0.06952(18) 0.18981(17) 0.0331(6) Uani 1 1 d . . . . .
N3 N 0.02805(19) 0.11278(19) 0.09130(18) 0.0371(6) Uani 1 1 d . . . . .
N4 N 0.3400(2) 0.21613(19) 0.13411(19) 0.0390(6) Uani 1 1 d . . . . .
N5 N 0.4462(2) 0.1524(2) 0.2871(2) 0.0452(7) Uani 1 1 d . . . . .
N6 N 0.3167(2) 0.2255(2) 0.39125(18) 0.0458(7) Uani 1 1 d . . . . .
N7 N 0.6996(3) 0.5308(2) 0.4386(2) 0.0500(8) Uani 1 1 d . . . . .
N8 N 0.6333(2) 0.5628(2) 0.2762(2) 0.0500(8) Uani 1 1 d . . . . .
N9 N 0.7964(3) 0.4908(2) 0.2021(2) 0.0536(8) Uani 1 1 d . . . . .
O1 O -0.15190(16) 0.08496(16) 0.15894(16) 0.0425(5) Uani 1 1 d . . . . .
O2 O -0.3024(2) 0.2113(2) 0.1062(2) 0.0710(8) Uani 1 1 d . . . . .
O3 O -0.25691(17) 0.29397(16) 0.23281(16) 0.0461(6) Uani 1 1 d . . . . .
O4 O -0.09791(16) 0.18098(15) 0.24724(15) 0.0391(5) Uani 1 1 d . . . . .
O5 O 0.10491(15) 0.04788(15) 0.27521(14) 0.0330(5) Uani 1 1 d . . . . .
O6 O 0.25399(17) -0.15135(15) 0.33576(14) 0.0372(5) Uani 1 1 d . . . . .
O7 O 0.2668(2) -0.28860(16) 0.45535(16) 0.0504(6) Uani 1 1 d . . . . .
O8 O 0.2529(3) -0.1678(2) 0.56320(17) 0.0733(9) Uani 1 1 d . . . . .
O9 O 0.25652(17) -0.04582(15) 0.43703(13) 0.0370(5) Uani 1 1 d . . . . .
O10 O 0.40306(15) -0.06664(17) 0.29885(15) 0.0412(5) Uani 1 1 d . . . . .
O11 O 0.52529(19) -0.1403(2) 0.2216(2) 0.0759(9) Uani 1 1 d . . . . .
O12 O 0.3670(2) -0.0731(3) 0.0816(2) 0.0822(10) Uani 1 1 d . . . . .
O13 O 0.26342(15) 0.00119(16) 0.16982(14) 0.0367(5) Uani 1 1 d . . . . .
O14 O 0.25508(16) 0.12688(15) 0.28825(14) 0.0363(5) Uani 1 1 d . . . . .
O15 O 0.33672(19) 0.35948(17) 0.22252(17) 0.0498(6) Uani 1 1 d . . . . .
O16 O 0.2715(3) 0.5273(2) 0.1729(2) 0.0943(12) Uani 1 1 d . . . . .
O17 O 0.0802(2) 0.5111(2) 0.1605(3) 0.0972(12) Uani 1 1 d . . . . .
O18 O 0.16041(17) 0.34283(17) 0.21858(16) 0.0468(6) Uani 1 1 d . . . . .
O19 O 0.7712(2) 0.36279(18) 0.36963(17) 0.0556(7) Uani 1 1 d D . . . .
O20 O 0.9187(2) 0.4491(2) 0.37988(19) 0.0615(7) Uani 1 1 d . . . . .
O21 O 1.0476(2) 0.5002(3) 0.3912(3) 0.0975(12) Uani 1 1 d . . . . .
O22 O 0.9110(3) 0.6975(2) 0.2945(2) 0.0810(10) Uani 1 1 d . . . . .
O23 O 0.79604(19) 0.62854(17) 0.29103(18) 0.0521(6) Uani 1 1 d . . . . .
O24 O 0.7278(8) -0.1388(8) 0.2116(8) 0.178(7) Uani 0.527(14) 1 d . . . . .
O25 O -0.4632(5) 0.3602(7) 0.2682(6) 0.166(5) Uani 0.661(13) 1 d . . . . .
O26 O 0.4878(4) 0.6143(4) -0.0782(4) 0.176(2) Uani 1 1 d . . . . .
Cr1 Cr -0.01896(3) 0.05790(3) 0.21903(3) 0.03011(12) Uani 1 1 d . . . . .
Cr2 Cr 0.29792(4) 0.24043(3) 0.25608(3) 0.03112(12) Uani 1 1 d . . . . .
Cr3 Cr 0.77742(4) 0.50007(4) 0.32981(4) 0.03834(13) Uani 1 1 d . . . . .
Nb1 Nb 0.24089(2) 0.00979(2) 0.29716(2) 0.02577(7) Uani 1 1 d . . . . .
H19A H 0.760(3) 0.342(2) 0.3289(16) 0.039 Uiso 1 1 d D U . . .
H19B H 0.754(2) 0.335(2) 0.4206(14) 0.039 Uiso 1 1 d 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 1.345(4) . ?
C1 C2 1.387(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.348(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.383(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(5) . ?
C4 H4 0.9300 . ?
C5 N1 1.351(4) . ?
C5 C6 1.480(5) . ?
C6 N2 1.345(4) . ?
C6 C7 1.374(4) . ?
C7 C8 1.390(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.378(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.384(4) . ?
C9 H9 0.9300 . ?
C10 N2 1.361(4) . ?
C10 C11 1.462(5) . ?
C11 N3 1.353(4) . ?
C11 C12 1.406(5) . ?
C12 C13 1.373(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.364(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.395(6) . ?
C14 H14 0.9300 . ?
C15 N3 1.325(4) . ?
C15 H15 0.9300 . ?
C16 N4 1.341(4) . ?
C16 C17 1.393(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.355(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.376(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.409(6) . ?
C19 H19 0.9300 . ?
C20 N4 1.357(4) . ?
C20 C21 1.466(6) . ?
C21 N5 1.357(5) . ?
C21 C22 1.392(5) . ?
C22 C23 1.339(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.387(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.429(6) . ?
C24 H24 0.9300 . ?
C25 N5 1.345(5) . ?
C25 C26 1.465(6) . ?
C26 N6 1.378(5) . ?
C26 C27 1.390(6) . ?
C27 C28 1.354(8) . ?
C27 H27 0.9300 . ?
C28 C29 1.391(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.415(6) . ?
C29 H29 0.9300 . ?
C30 N6 1.330(5) . ?
C30 H30 0.9300 . ?
C31 N7 1.339(5) . ?
C31 C32 1.409(7) . ?
C31 H31 0.9300 . ?
C32 C33 1.362(10) . ?
C32 H32 0.9300 . ?
C33 C34 1.379(10) . ?
C33 H33 0.9300 . ?
C34 C35 1.398(6) . ?
C34 H34 0.9300 . ?
C35 N7 1.345(5) . ?
C35 C36 1.484(7) . ?
C36 N8 1.358(5) . ?
C36 C37 1.411(7) . ?
C37 C38 1.402(9) . ?
C37 H37 0.9300 . ?
C38 C39 1.379(9) . ?
C38 H38 0.9300 . ?
C39 C40 1.376(7) . ?
C39 H39 0.9300 . ?
C40 N8 1.369(6) . ?
C40 C41 1.474(6) . ?
C41 N9 1.340(5) . ?
C41 C42 1.437(7) . ?
C42 C43 1.371(8) . ?
C42 H42 0.9300 . ?
C43 C44 1.371(9) . ?
C43 H43 0.9300 . ?
C44 C45 1.377(7) . ?
C44 H44 0.9300 . ?
C45 N9 1.348(5) . ?
C45 H45 0.9300 . ?
C46 O2 1.220(4) . ?
C46 O1 1.279(4) . ?
C46 C47 1.560(4) . ?
C47 O3 1.213(4) . ?
C47 O4 1.291(4) . ?
C48 O7 1.230(4) . ?
C48 O6 1.281(4) . ?
C48 C49 1.542(4) . ?
C49 O8 1.219(4) . ?
C49 O9 1.307(4) . ?
C50 O11 1.211(4) . ?
C50 O10 1.290(4) . ?
C50 C51 1.567(5) . ?
C51 O12 1.196(4) . ?
C51 O13 1.311(4) . ?
C52 O16 1.221(4) . ?
C52 O15 1.261(4) . ?
C52 C53 1.555(6) . ?
C53 O17 1.203(4) . ?
C53 O18 1.303(4) . ?
C54 O21 1.214(5) . ?
C54 O20 1.317(5) . ?
C54 C55 1.533(6) . ?
C55 O22 1.208(4) . ?
C55 O23 1.308(4) . ?
N1 Cr1 2.083(3) . ?
N2 Cr1 1.983(2) . ?
N3 Cr1 2.103(3) . ?
N4 Cr2 2.090(3) . ?
N5 Cr2 1.996(3) . ?
N6 Cr2 2.078(3) . ?
N7 Cr3 2.087(3) . ?
N8 Cr3 1.988(3) . ?
N9 Cr3 2.057(3) . ?
O1 Cr1 1.980(2) . ?
O4 Cr1 1.941(2) . ?
O5 Nb1 1.808(2) . ?
O5 Cr1 1.927(2) . ?
O6 Nb1 2.217(2) . ?
O9 Nb1 2.073(2) . ?
O10 Nb1 2.151(2) . ?
O13 Nb1 2.053(2) . ?
O14 Nb1 1.792(2) . ?
O14 Cr2 1.922(2) . ?
O15 Cr2 1.961(2) . ?
O18 Cr2 1.940(2) . ?
O19 Cr3 1.975(2) . ?
O19 H19A 0.834(17) . ?
O19 H19B 0.852(17) . ?
O20 Cr3 1.950(3) . ?
O23 Cr3 1.932(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 123.1(4) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C3 C2 C1 118.4(4) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 119.3(4) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C5 120.9(4) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
N1 C5 C4 119.4(3) . . ?
N1 C5 C6 114.3(3) . . ?
C4 C5 C6 126.2(3) . . ?
N2 C6 C7 118.4(3) . . ?
N2 C6 C5 114.7(3) . . ?
C7 C6 C5 126.9(3) . . ?
C6 C7 C8 118.8(3) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C9 C8 C7 122.5(3) . . ?
C9 C8 H8 118.7 . . ?
C7 C8 H8 118.7 . . ?
C8 C9 C10 116.9(4) . . ?
C8 C9 H9 121.5 . . ?
C10 C9 H9 121.5 . . ?
N2 C10 C9 119.7(3) . . ?
N2 C10 C11 114.6(3) . . ?
C9 C10 C11 125.7(3) . . ?
N3 C11 C12 121.7(3) . . ?
N3 C11 C10 113.1(3) . . ?
C12 C11 C10 125.2(3) . . ?
C13 C12 C11 119.2(4) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C14 C13 C12 118.9(4) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 119.1(4) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
N3 C15 C14 123.3(4) . . ?
N3 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
N4 C16 C17 123.2(4) . . ?
N4 C16 H16 118.4 . . ?
C17 C16 H16 118.4 . . ?
C18 C17 C16 118.7(4) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C17 C18 C19 119.6(4) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C18 C19 C20 119.8(4) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
N4 C20 C19 120.5(4) . . ?
N4 C20 C21 113.9(3) . . ?
C19 C20 C21 125.7(4) . . ?
N5 C21 C22 119.3(4) . . ?
N5 C21 C20 114.6(3) . . ?
C22 C21 C20 126.1(4) . . ?
C23 C22 C21 118.6(5) . . ?
C23 C22 H22 120.7 . . ?
C21 C22 H22 120.7 . . ?
C22 C23 C24 123.3(5) . . ?
C22 C23 H23 118.3 . . ?
C24 C23 H23 118.3 . . ?
C23 C24 C25 117.3(5) . . ?
C23 C24 H24 121.4 . . ?
C25 C24 H24 121.4 . . ?
N5 C25 C24 118.1(5) . . ?
N5 C25 C26 114.0(3) . . ?
C24 C25 C26 127.9(4) . . ?
N6 C26 C27 119.6(5) . . ?
N6 C26 C25 114.6(3) . . ?
C27 C26 C25 125.8(5) . . ?
C28 C27 C26 120.9(5) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C27 C28 C29 119.9(4) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C28 C29 C30 118.0(5) . . ?
C28 C29 H29 121.0 . . ?
C30 C29 H29 121.0 . . ?
N6 C30 C29 121.6(5) . . ?
N6 C30 H30 119.2 . . ?
C29 C30 H30 119.2 . . ?
N7 C31 C32 122.3(6) . . ?
N7 C31 H31 118.9 . . ?
C32 C31 H31 118.9 . . ?
C33 C32 C31 118.8(7) . . ?
C33 C32 H32 120.6 . . ?
C31 C32 H32 120.6 . . ?
C32 C33 C34 119.3(6) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 H33 120.4 . . ?
C33 C34 C35 119.7(6) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
N7 C35 C34 121.3(5) . . ?
N7 C35 C36 114.3(3) . . ?
C34 C35 C36 124.4(5) . . ?
N8 C36 C37 118.5(5) . . ?
N8 C36 C35 113.6(4) . . ?
C37 C36 C35 127.9(5) . . ?
C38 C37 C36 116.9(6) . . ?
C38 C37 H37 121.6 . . ?
C36 C37 H37 121.6 . . ?
C39 C38 C37 123.2(6) . . ?
C39 C38 H38 118.4 . . ?
C37 C38 H38 118.4 . . ?
C40 C39 C38 118.4(6) . . ?
C40 C39 H39 120.8 . . ?
C38 C39 H39 120.8 . . ?
N8 C40 C39 118.8(5) . . ?
N8 C40 C41 113.0(4) . . ?
C39 C40 C41 128.1(5) . . ?
N9 C41 C42 120.8(5) . . ?
N9 C41 C40 115.0(4) . . ?
C42 C41 C40 124.3(5) . . ?
C43 C42 C41 116.9(6) . . ?
C43 C42 H42 121.5 . . ?
C41 C42 H42 121.5 . . ?
C44 C43 C42 122.0(6) . . ?
C44 C43 H43 119.0 . . ?
C42 C43 H43 119.0 . . ?
C43 C44 C45 117.9(6) . . ?
C43 C44 H44 121.0 . . ?
C45 C44 H44 121.0 . . ?
N9 C45 C44 122.4(6) . . ?
N9 C45 H45 118.8 . . ?
C44 C45 H45 118.8 . . ?
O2 C46 O1 125.0(3) . . ?
O2 C46 C47 122.6(3) . . ?
O1 C46 C47 112.4(3) . . ?
O3 C47 O4 125.0(3) . . ?
O3 C47 C46 120.8(3) . . ?
O4 C47 C46 114.2(3) . . ?
O7 C48 O6 126.8(3) . . ?
O7 C48 C49 118.6(3) . . ?
O6 C48 C49 114.6(3) . . ?
O8 C49 O9 124.6(3) . . ?
O8 C49 C48 122.9(3) . . ?
O9 C49 C48 112.5(3) . . ?
O11 C50 O10 126.4(3) . . ?
O11 C50 C51 120.4(3) . . ?
O10 C50 C51 113.2(3) . . ?
O12 C51 O13 124.8(3) . . ?
O12 C51 C50 124.0(3) . . ?
O13 C51 C50 111.2(3) . . ?
O16 C52 O15 123.8(4) . . ?
O16 C52 C53 122.3(4) . . ?
O15 C52 C53 113.9(3) . . ?
O17 C53 O18 123.8(4) . . ?
O17 C53 C52 121.4(4) . . ?
O18 C53 C52 114.7(3) . . ?
O21 C54 O20 126.5(5) . . ?
O21 C54 C55 121.9(4) . . ?
O20 C54 C55 111.6(3) . . ?
O22 C55 O23 125.9(4) . . ?
O22 C55 C54 120.8(4) . . ?
O23 C55 C54 113.3(3) . . ?
C1 N1 C5 118.9(3) . . ?
C1 N1 Cr1 126.5(2) . . ?
C5 N1 Cr1 114.1(2) . . ?
C6 N2 C10 123.6(3) . . ?
C6 N2 Cr1 117.5(2) . . ?
C10 N2 Cr1 118.8(2) . . ?
C15 N3 C11 117.7(3) . . ?
C15 N3 Cr1 126.4(2) . . ?
C11 N3 Cr1 115.9(2) . . ?
C16 N4 C20 118.2(3) . . ?
C16 N4 Cr2 126.6(2) . . ?
C20 N4 Cr2 115.2(2) . . ?
C25 N5 C21 123.4(3) . . ?
C25 N5 Cr2 118.5(3) . . ?
C21 N5 Cr2 118.0(2) . . ?
C30 N6 C26 120.0(3) . . ?
C30 N6 Cr2 126.0(3) . . ?
C26 N6 Cr2 114.0(3) . . ?
C31 N7 C35 118.7(4) . . ?
C31 N7 Cr3 126.2(3) . . ?
C35 N7 Cr3 115.1(3) . . ?
C36 N8 C40 124.2(4) . . ?
C36 N8 Cr3 118.4(3) . . ?
C40 N8 Cr3 117.5(3) . . ?
C41 N9 C45 119.7(4) . . ?
C41 N9 Cr3 115.1(3) . . ?
C45 N9 Cr3 125.1(3) . . ?
C46 O1 Cr1 114.5(2) . . ?
C47 O4 Cr1 114.65(18) . . ?
Nb1 O5 Cr1 156.80(12) . . ?
C48 O6 Nb1 116.72(18) . . ?
C49 O9 Nb1 121.82(19) . . ?
C50 O10 Nb1 118.11(19) . . ?
C51 O13 Nb1 121.7(2) . . ?
Nb1 O14 Cr2 163.84(13) . . ?
C52 O15 Cr2 114.3(2) . . ?
C53 O18 Cr2 112.9(2) . . ?
Cr3 O19 H19A 116(2) . . ?
Cr3 O19 H19B 125(2) . . ?
H19A O19 H19B 114(3) . . ?
C54 O20 Cr3 116.8(3) . . ?
C55 O23 Cr3 116.8(2) . . ?
O5 Cr1 O4 91.53(9) . . ?
O5 Cr1 O1 173.55(9) . . ?
O4 Cr1 O1 82.70(9) . . ?
O5 Cr1 N2 92.22(9) . . ?
O4 Cr1 N2 175.91(10) . . ?
O1 Cr1 N2 93.64(9) . . ?
O5 Cr1 N1 89.39(9) . . ?
O4 Cr1 N1 99.03(10) . . ?
O1 Cr1 N1 94.33(10) . . ?
N2 Cr1 N1 79.36(11) . . ?
O5 Cr1 N3 89.75(10) . . ?
O4 Cr1 N3 104.19(10) . . ?
O1 Cr1 N3 88.90(10) . . ?
N2 Cr1 N3 77.48(10) . . ?
N1 Cr1 N3 156.78(10) . . ?
O14 Cr2 O18 93.99(10) . . ?
O14 Cr2 O15 178.04(10) . . ?
O18 Cr2 O15 84.06(11) . . ?
O14 Cr2 N5 94.47(10) . . ?
O18 Cr2 N5 171.45(10) . . ?
O15 Cr2 N5 87.48(10) . . ?
O14 Cr2 N6 90.65(10) . . ?
O18 Cr2 N6 102.28(12) . . ?
O15 Cr2 N6 89.56(10) . . ?
N5 Cr2 N6 78.81(13) . . ?
O14 Cr2 N4 89.94(9) . . ?
O18 Cr2 N4 100.58(11) . . ?
O15 Cr2 N4 90.63(10) . . ?
N5 Cr2 N4 78.27(12) . . ?
N6 Cr2 N4 157.04(12) . . ?
O23 Cr3 O20 81.54(11) . . ?
O23 Cr3 O19 175.06(12) . . ?
O20 Cr3 O19 93.98(12) . . ?
O23 Cr3 N8 94.10(11) . . ?
O20 Cr3 N8 175.62(11) . . ?
O19 Cr3 N8 90.40(12) . . ?
O23 Cr3 N9 90.13(11) . . ?
O20 Cr3 N9 101.22(13) . . ?
O19 Cr3 N9 88.70(11) . . ?
N8 Cr3 N9 79.16(14) . . ?
O23 Cr3 N7 93.06(11) . . ?
O20 Cr3 N7 101.12(13) . . ?
O19 Cr3 N7 89.84(11) . . ?
N8 Cr3 N7 78.56(14) . . ?
N9 Cr3 N7 157.66(14) . . ?
O14 Nb1 O5 103.89(9) . . ?
O14 Nb1 O13 102.56(9) . . ?
O5 Nb1 O13 91.12(9) . . ?
O14 Nb1 O9 95.51(9) . . ?
O5 Nb1 O9 100.09(9) . . ?
O13 Nb1 O9 155.82(8) . . ?
O14 Nb1 O10 90.82(9) . . ?
O5 Nb1 O10 161.60(8) . . ?
O13 Nb1 O10 74.70(8) . . ?
O9 Nb1 O10 89.25(9) . . ?
O14 Nb1 O6 165.76(9) . . ?
O5 Nb1 O6 87.48(8) . . ?
O13 Nb1 O6 85.50(8) . . ?
O9 Nb1 O6 73.77(8) . . ?
O10 Nb1 O6 79.90(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 -1.1(7) . . . . ?
C1 C2 C3 C4 -0.4(7) . . . . ?
C2 C3 C4 C5 2.1(6) . . . . ?
C3 C4 C5 N1 -2.3(5) . . . . ?
C3 C4 C5 C6 173.0(3) . . . . ?
N1 C5 C6 N2 3.8(4) . . . . ?
C4 C5 C6 N2 -171.7(3) . . . . ?
N1 C5 C6 C7 -179.3(3) . . . . ?
C4 C5 C6 C7 5.2(5) . . . . ?
N2 C6 C7 C8 2.9(5) . . . . ?
C5 C6 C7 C8 -173.9(3) . . . . ?
C6 C7 C8 C9 -0.5(5) . . . . ?
C7 C8 C9 C10 -1.6(5) . . . . ?
C8 C9 C10 N2 1.3(5) . . . . ?
C8 C9 C10 C11 -178.7(3) . . . . ?
N2 C10 C11 N3 0.2(4) . . . . ?
C9 C10 C11 N3 -179.8(3) . . . . ?
N2 C10 C11 C12 -179.4(3) . . . . ?
C9 C10 C11 C12 0.6(5) . . . . ?
N3 C11 C12 C13 -0.6(5) . . . . ?
C10 C11 C12 C13 179.0(3) . . . . ?
C11 C12 C13 C14 0.9(5) . . . . ?
C12 C13 C14 C15 -0.1(6) . . . . ?
C13 C14 C15 N3 -1.1(6) . . . . ?
N4 C16 C17 C18 0.4(6) . . . . ?
C16 C17 C18 C19 0.6(7) . . . . ?
C17 C18 C19 C20 -0.7(7) . . . . ?
C18 C19 C20 N4 -0.2(6) . . . . ?
C18 C19 C20 C21 178.5(4) . . . . ?
N4 C20 C21 N5 0.5(4) . . . . ?
C19 C20 C21 N5 -178.3(3) . . . . ?
N4 C20 C21 C22 -179.2(3) . . . . ?
C19 C20 C21 C22 2.1(6) . . . . ?
N5 C21 C22 C23 -0.6(6) . . . . ?
C20 C21 C22 C23 179.0(4) . . . . ?
C21 C22 C23 C24 0.6(7) . . . . ?
C22 C23 C24 C25 -0.8(7) . . . . ?
C23 C24 C25 N5 0.8(5) . . . . ?
C23 C24 C25 C26 -179.6(4) . . . . ?
N5 C25 C26 N6 0.1(4) . . . . ?
C24 C25 C26 N6 -179.4(3) . . . . ?
N5 C25 C26 C27 179.7(3) . . . . ?
C24 C25 C26 C27 0.1(6) . . . . ?
N6 C26 C27 C28 1.5(6) . . . . ?
C25 C26 C27 C28 -178.1(4) . . . . ?
C26 C27 C28 C29 -0.3(7) . . . . ?
C27 C28 C29 C30 -0.9(7) . . . . ?
C28 C29 C30 N6 1.1(6) . . . . ?
N7 C31 C32 C33 -1.0(7) . . . . ?
C31 C32 C33 C34 1.2(9) . . . . ?
C32 C33 C34 C35 -0.8(8) . . . . ?
C33 C34 C35 N7 0.1(7) . . . . ?
C33 C34 C35 C36 178.8(4) . . . . ?
N7 C35 C36 N8 1.5(5) . . . . ?
C34 C35 C36 N8 -177.4(4) . . . . ?
N7 C35 C36 C37 180.0(4) . . . . ?
C34 C35 C36 C37 1.1(6) . . . . ?
N8 C36 C37 C38 0.2(7) . . . . ?
C35 C36 C37 C38 -178.2(5) . . . . ?
C36 C37 C38 C39 1.2(9) . . . . ?
C37 C38 C39 C40 -0.9(10) . . . . ?
C38 C39 C40 N8 -1.0(7) . . . . ?
C38 C39 C40 C41 -179.8(5) . . . . ?
N8 C40 C41 N9 -4.7(5) . . . . ?
C39 C40 C41 N9 174.2(4) . . . . ?
N8 C40 C41 C42 174.9(4) . . . . ?
C39 C40 C41 C42 -6.2(7) . . . . ?
N9 C41 C42 C43 -1.9(7) . . . . ?
C40 C41 C42 C43 178.4(4) . . . . ?
C41 C42 C43 C44 -2.4(8) . . . . ?
C42 C43 C44 C45 5.1(8) . . . . ?
C43 C44 C45 N9 -3.6(7) . . . . ?
O2 C46 C47 O3 14.6(5) . . . . ?
O1 C46 C47 O3 -166.4(3) . . . . ?
O2 C46 C47 O4 -165.8(3) . . . . ?
O1 C46 C47 O4 13.2(4) . . . . ?
O7 C48 C49 O8 -5.1(5) . . . . ?
O6 C48 C49 O8 174.7(3) . . . . ?
O7 C48 C49 O9 174.6(3) . . . . ?
O6 C48 C49 O9 -5.5(4) . . . . ?
O11 C50 C51 O12 3.8(6) . . . . ?
O10 C50 C51 O12 -176.6(4) . . . . ?
O11 C50 C51 O13 -176.6(3) . . . . ?
O10 C50 C51 O13 3.0(4) . . . . ?
O16 C52 C53 O17 4.7(6) . . . . ?
O15 C52 C53 O17 -175.3(4) . . . . ?
O16 C52 C53 O18 -178.4(4) . . . . ?
O15 C52 C53 O18 1.6(5) . . . . ?
O21 C54 C55 O22 -0.3(6) . . . . ?
O20 C54 C55 O22 178.8(4) . . . . ?
O21 C54 C55 O23 -179.8(4) . . . . ?
O20 C54 C55 O23 -0.6(5) . . . . ?
C2 C1 N1 C5 0.9(5) . . . . ?
C2 C1 N1 Cr1 -170.1(3) . . . . ?
C4 C5 N1 C1 0.8(4) . . . . ?
C6 C5 N1 C1 -175.0(3) . . . . ?
C4 C5 N1 Cr1 172.8(2) . . . . ?
C6 C5 N1 Cr1 -3.0(3) . . . . ?
C7 C6 N2 C10 -3.4(4) . . . . ?
C5 C6 N2 C10 173.8(3) . . . . ?
C7 C6 N2 Cr1 180.0(2) . . . . ?
C5 C6 N2 Cr1 -2.8(3) . . . . ?
C9 C10 N2 C6 1.3(4) . . . . ?
C11 C10 N2 C6 -178.8(3) . . . . ?
C9 C10 N2 Cr1 177.8(2) . . . . ?
C11 C10 N2 Cr1 -2.2(3) . . . . ?
C14 C15 N3 C11 1.3(5) . . . . ?
C14 C15 N3 Cr1 179.3(3) . . . . ?
C12 C11 N3 C15 -0.5(4) . . . . ?
C10 C11 N3 C15 179.9(3) . . . . ?
C12 C11 N3 Cr1 -178.6(2) . . . . ?
C10 C11 N3 Cr1 1.7(3) . . . . ?
C17 C16 N4 C20 -1.3(5) . . . . ?
C17 C16 N4 Cr2 -179.2(3) . . . . ?
C19 C20 N4 C16 1.2(5) . . . . ?
C21 C20 N4 C16 -177.6(3) . . . . ?
C19 C20 N4 Cr2 179.3(3) . . . . ?
C21 C20 N4 Cr2 0.5(4) . . . . ?
C24 C25 N5 C21 -0.9(5) . . . . ?
C26 C25 N5 C21 179.5(3) . . . . ?
C24 C25 N5 Cr2 -178.5(2) . . . . ?
C26 C25 N5 Cr2 1.9(4) . . . . ?
C22 C21 N5 C25 0.8(5) . . . . ?
C20 C21 N5 C25 -178.9(3) . . . . ?
C22 C21 N5 Cr2 178.4(3) . . . . ?
C20 C21 N5 Cr2 -1.3(4) . . . . ?
C29 C30 N6 C26 -0.1(5) . . . . ?
C29 C30 N6 Cr2 -179.7(3) . . . . ?
C27 C26 N6 C30 -1.2(5) . . . . ?
C25 C26 N6 C30 178.3(3) . . . . ?
C27 C26 N6 Cr2 178.5(3) . . . . ?
C25 C26 N6 Cr2 -2.0(3) . . . . ?
C32 C31 N7 C35 0.3(5) . . . . ?
C32 C31 N7 Cr3 -179.1(3) . . . . ?
C34 C35 N7 C31 0.2(5) . . . . ?
C36 C35 N7 C31 -178.7(3) . . . . ?
C34 C35 N7 Cr3 179.6(3) . . . . ?
C36 C35 N7 Cr3 0.7(4) . . . . ?
C37 C36 N8 C40 -2.1(5) . . . . ?
C35 C36 N8 C40 176.5(3) . . . . ?
C37 C36 N8 Cr3 178.2(3) . . . . ?
C35 C36 N8 Cr3 -3.2(4) . . . . ?
C39 C40 N8 C36 2.5(6) . . . . ?
C41 C40 N8 C36 -178.5(3) . . . . ?
C39 C40 N8 Cr3 -177.8(3) . . . . ?
C41 C40 N8 Cr3 1.2(4) . . . . ?
C42 C41 N9 C45 3.4(6) . . . . ?
C40 C41 N9 C45 -176.9(3) . . . . ?
C42 C41 N9 Cr3 -173.7(3) . . . . ?
C40 C41 N9 Cr3 5.9(4) . . . . ?
C44 C45 N9 C41 -0.6(6) . . . . ?
C44 C45 N9 Cr3 176.2(3) . . . . ?
O2 C46 O1 Cr1 165.6(3) . . . . ?
C47 C46 O1 Cr1 -13.4(3) . . . . ?
O3 C47 O4 Cr1 173.4(3) . . . . ?
C46 C47 O4 Cr1 -6.2(3) . . . . ?
O7 C48 O6 Nb1 179.9(3) . . . . ?
C49 C48 O6 Nb1 0.1(3) . . . . ?
O8 C49 O9 Nb1 -171.2(3) . . . . ?
C48 C49 O9 Nb1 9.1(4) . . . . ?
O11 C50 O10 Nb1 -175.7(3) . . . . ?
C51 C50 O10 Nb1 4.8(4) . . . . ?
O12 C51 O13 Nb1 169.5(3) . . . . ?
C50 C51 O13 Nb1 -10.1(4) . . . . ?
O16 C52 O15 Cr2 178.2(3) . . . . ?
C53 C52 O15 Cr2 -1.7(4) . . . . ?
O17 C53 O18 Cr2 176.2(3) . . . . ?
C52 C53 O18 Cr2 -0.6(4) . . . . ?
O21 C54 O20 Cr3 -179.8(4) . . . . ?
C55 C54 O20 Cr3 1.1(4) . . . . ?
O22 C55 O23 Cr3 -179.5(3) . . . . ?
C54 C55 O23 Cr3 -0.1(4) . . . . ?
Cr2 O14 Nb1 O5 -128.5(5) . . . . ?
Cr2 O14 Nb1 O13 -34.2(5) . . . . ?
Cr2 O14 Nb1 O9 129.6(5) . . . . ?
Cr2 O14 Nb1 O10 40.3(5) . . . . ?
Cr2 O14 Nb1 O6 89.3(6) . . . . ?
Cr1 O5 Nb1 O14 129.5(3) . . . . ?
Cr1 O5 Nb1 O13 26.3(3) . . . . ?
Cr1 O5 Nb1 O9 -132.2(3) . . . . ?
Cr1 O5 Nb1 O10 -12.7(5) . . . . ?
Cr1 O5 Nb1 O6 -59.2(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C1 H1 O8 0.93 2.48 3.306(5) 148.0 2_556 yes
C12 H12 O1 0.93 2.61 3.406(4) 144.6 2 yes
C14 H14 O17 0.93 2.50 3.362(5) 154.9 2_565 yes
C19 H19 O12 0.93 2.53 3.150(5) 124.7 2_655 yes
C22 H22 O24 0.93 2.44 3.039(11) 122.6 . yes
C24 H24 O9 0.93 2.45 3.327(5) 156.7 2_656 yes
C27 H27 O10 0.93 2.53 3.264(5) 135.6 2_656 yes
C31 H31 O21 0.93 2.53 3.276(6) 136.9 2_766 yes
C32 H32 O16 0.93 2.66 3.542(7) 157.8 2_666 yes
C34 H34 O7 0.93 2.60 3.527(7) 173.7 1_565 yes
C42 H42 O26 0.93 2.54 3.465(8) 170.3 . yes
C45 H45 O17 0.93 2.57 3.163(6) 122.1 1_655 yes
O19 H19A O3 0.834(17) 1.923(18) 2.756(4) 177(3) 1_655 yes
O19 H19B O7 0.852(17) 1.904(18) 2.738(4) 166(3) 2_656 yes
O19 H19B O8 0.852(17) 2.46(3) 2.907(4) 113(2) 2_656 yes
C1 H1 O8 0.93 2.48 3.306(5) 148.0 2_556 yes
C12 H12 O1 0.93 2.61 3.406(4) 144.6 2 yes
C14 H14 O17 0.93 2.50 3.362(5) 154.9 2_565 yes
C19 H19 O12 0.93 2.53 3.150(5) 124.7 2_655 yes
C22 H22 O24 0.93 2.44 3.039(11) 122.6 . yes
C24 H24 O9 0.93 2.45 3.327(5) 156.7 2_656 yes
C27 H27 O10 0.93 2.53 3.264(5) 135.6 2_656 yes
C31 H31 O21 0.93 2.53 3.276(6) 136.9 2_766 yes
C34 H34 O7 0.93 2.60 3.527(7) 173.7 1_565 yes
C42 H42 O26 0.93 2.54 3.465(8) 170.3 . yes
C45 H45 O17 0.93 2.57 3.163(6) 122.1 1_655 yes
O19 H19A O3 0.834(17) 1.923(18) 2.756(4) 177(3) 1_655 yes
O19 H19B O7 0.852(17) 1.904(18) 2.738(4) 166(3) 2_656 yes
O19 H19B O8 0.852(17) 2.46(3) 2.907(4) 113(2) 2_656 yes

_refine_diff_density_max         0.580
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.066

