# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1983881'
loop_
_audit_author_name
_audit_author_address
'Jakub Zakrzewski'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2020-02-13 deposited with the CCDC.	2020-10-30 downloaded from the CCDC.
;

_audit_creation_date             2019-08-23T12:28:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C26 H24 Co Ho N10 O6, 2(H2O)'
_chemical_formula_sum            'C26 H28 Co Ho N10 O8'
_chemical_formula_weight         832.44

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_Int_Tables_number      63
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   14.7754(11)
_cell_length_b                   14.9336(11)
_cell_length_c                   14.0276(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3095.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    14806
_cell_measurement_theta_min      3.091
_cell_measurement_theta_max      27.479
_cell_measurement_wavelength     0.71075

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.422
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.074
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1648

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.351
_exptl_absorpt_correction_T_max  0.801

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_radiation_type           MoK\a
_diffrn_measurement_method       ω
_diffrn_radiation_probe          x-ray
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_number            14806
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.091
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_reflns_Friedel_coverage         0
_reflns_number_total             1920
_reflns_number_gt                1902
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+31.6492P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1920
_refine_ls_number_parameters     195
_refine_ls_number_restraints     26
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.058
_refine_ls_wR_factor_gt          0.0578
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_restrained_S_all      1.288
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.971
_refine_diff_density_min         -2.103
_refine_diff_density_rms         0.131

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Ho1 Ho 0.5 0.44775(2) 0.25 0.00483(8) Uani 1 4 d S T P . .
Co1 Co 0.5 0.81667(5) 0.25 0.00631(17) Uani 1 4 d S T P . .
N2 N 0.5 1.0212(3) 0.25 0.0112(11) Uani 1 4 d S T P . .
N1 N 0.5 0.6125(3) 0.25 0.0045(9) Uani 1 4 d S TU P . .
O3 O 0.4058(2) 0.3179(2) 0.25 0.0390(12) Uani 1 2 d S TU P . .
H3A H 0.34871 0.326919 0.280472 0.059 Uiso 0.5 1 d R U P . .
H3B H 0.429245 0.269743 0.287362 0.059 Uiso 0.5 1 d R U P . .
C1 C 0.5 0.6917(4) 0.25 0.0052(11) Uani 1 4 d S TU P . .
C3 C 0.5 0.8173(3) 0.1144(3) 0.0098(8) Uani 1 2 d S T P . .
C2 C 0.5 0.9441(5) 0.25 0.0122(12) Uani 1 4 d S T P . .
N3 N 0.5 0.8185(3) 0.0326(3) 0.0157(8) Uani 1 2 d S T P . .
C4 C 0.6285(3) 0.8157(3) 0.25 0.0251(13) Uani 1 2 d S TU P . .
O1S O 0.4315(3) 0.1742(3) 0.1507(3) 0.0115(9) Uani 0.5 1 d G . P . .
H1SA H 0.448521 0.124868 0.178231 0.017 Uiso 0.5 1 d G U P . .
H1SB H 0.460782 0.180794 0.097349 0.017 Uiso 0.5 1 d G U P . .
N4 N 0.7052(4) 0.8139(4) 0.25 0.075(2) Uani 1 2 d S TU P . .
C5 C 0.6832(4) 0.5416(4) 0.1380(4) 0.0112(12) Uani 0.5 1 d . . P A 1
O1 O 0.6372(3) 0.4922(3) 0.1941(3) 0.0128(9) Uani 0.5 1 d . . P A 1
C9 C 0.7785(5) 0.5487(5) 0.1480(6) 0.0213(15) Uani 0.5 1 d . . P A 1
H9 H 0.807956 0.520486 0.200187 0.026 Uiso 0.5 1 calc R U P A 1
C7 C 0.6979(6) 0.6358(5) -0.0016(5) 0.0261(18) Uani 0.5 1 d . . P A 1
H7 H 0.671152 0.666348 -0.053887 0.031 Uiso 0.5 1 calc R U P A 1
C8 C 0.8276(6) 0.5955(6) 0.0834(7) 0.035(2) Uani 0.5 1 d . . P A 1
H8 H 0.891549 0.598416 0.089846 0.042 Uiso 0.5 1 calc R U P A 1
N5 N 0.7870(8) 0.6382(8) 0.0100(8) 0.028(3) Uani 0.5 1 d . . P A 1
H5N H 0.820349 0.668181 -0.030994 0.10(5) Uiso 0.5 1 calc R . P A 1
C6 C 0.6446(6) 0.5899(5) 0.0605(5) 0.0185(15) Uani 0.5 1 d . . P A 1
H6 H 0.580836 0.59019 0.052177 0.022 Uiso 0.5 1 calc R U P A 1
C10 C 0.3807(4) 0.4079(4) 0.4456(4) 0.0100(12) Uani 0.5 1 d . . P A 2
C11 C 0.2932(5) 0.4180(4) 0.4065(5) 0.0135(13) Uani 0.5 1 d . . P A 2
H11 H 0.286557 0.441338 0.343939 0.016 Uiso 0.5 1 calc R U P A 2
C13 C 0.3088(5) 0.3504(4) 0.5874(5) 0.0184(15) Uani 0.5 1 d . . P A 2
H13 H 0.313415 0.326779 0.650051 0.022 Uiso 0.5 1 calc R U P A 2
C12 C 0.2186(5) 0.3947(5) 0.4571(6) 0.0157(14) Uani 0.5 1 d . . P A 2
H12 H 0.160499 0.400859 0.42884 0.019 Uiso 0.5 1 calc R U P A 2
N6 N 0.2256(7) 0.3626(7) 0.5477(6) 0.0179(19) Uani 0.5 1 d . . P A 2
H6N H 0.176527 0.349766 0.580444 0.022 Uiso 0.5 1 calc R U P A 2
C14 C 0.3852(5) 0.3715(5) 0.5385(5) 0.0157(14) Uani 0.5 1 d . . P A 2
H14 H 0.442543 0.361676 0.567273 0.019 Uiso 0.5 1 calc R U P A 2
O2 O 0.4529(3) 0.4313(3) 0.4001(3) 0.0116(9) Uani 0.5 1 d . . P A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Ho1 O2 2.231(4) . ?
Ho1 O2 2.231(4) 10_556 ?
Ho1 O2 2.231(4) 12_655 ?
Ho1 O2 2.231(4) 3_655 ?
Ho1 O1 2.272(4) . ?
Ho1 O1 2.272(4) 10_556 ?
Ho1 O1 2.272(4) 12_655 ?
Ho1 O1 2.272(4) 3_655 ?
Ho1 O3 2.388(4) . ?
Ho1 O3 2.388(4) 3_655 ?
Ho1 N1 2.460(5) . ?
Co1 C1 1.867(6) . ?
Co1 C4 1.899(5) 3_655 ?
Co1 C4 1.899(5) . ?
Co1 C3 1.902(5) . ?
Co1 C3 1.902(5) 10_556 ?
Co1 C2 1.902(7) . ?
N2 C2 1.152(9) . ?
N1 C1 1.182(8) . ?
C3 N3 1.148(6) . ?
C4 N4 1.134(8) . ?
C5 O1 1.276(7) . ?
C5 C9 1.419(9) . ?
C5 C6 1.423(10) . ?
O1 O1 1.568(9) 10_556 ?
C9 C8 1.355(11) . ?
C7 N5 1.326(14) . ?
C7 C6 1.360(11) . ?
C8 N5 1.352(15) . ?
C10 O2 1.291(8) . ?
C10 C11 1.412(9) . ?
C10 C14 1.414(9) . ?
C11 C12 1.356(10) . ?
C13 C14 1.357(10) . ?
C13 N6 1.361(13) . ?
C12 N6 1.362(9) . ?
O2 O2 1.392(9) 12_655 ?

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
O2 Ho1 O2 36.3(2) . 12_655 ?
O2 Ho1 O2 167.3(2) 10_556 12_655 ?
O1 Ho1 O1 40.4(2) . 10_556 ?
O1 Ho1 O1 126.3(2) . 12_655 ?
O1 Ho1 O1 146.0(2) 10_556 12_655 ?
O1 Ho1 O1 146.1(2) . 3_655 ?
O1 Ho1 O1 126.3(2) 10_556 3_655 ?
O1 Ho1 O1 40.4(2) 12_655 3_655 ?
O2 Ho1 O3 74.25(11) . . ?
O2 Ho1 O3 74.25(11) 10_556 . ?
O2 Ho1 O3 95.29(11) 12_655 . ?
O2 Ho1 O3 95.29(11) 3_655 . ?
O1 Ho1 O3 139.23(13) . . ?
O1 Ho1 O3 139.23(13) 10_556 . ?
O1 Ho1 O3 73.57(14) 12_655 . ?
O1 Ho1 O3 73.57(14) 3_655 . ?
O1 Ho1 O3 73.56(14) . 3_655 ?
O1 Ho1 O3 73.57(14) 10_556 3_655 ?
O1 Ho1 O3 139.23(13) 12_655 3_655 ?
O1 Ho1 O3 139.23(13) 3_655 3_655 ?
O3 Ho1 O3 71.33(18) . 3_655 ?
O2 Ho1 N1 96.33(11) . . ?
O2 Ho1 N1 96.33(11) 10_556 . ?
O2 Ho1 N1 96.33(11) 12_655 . ?
O2 Ho1 N1 96.33(11) 3_655 . ?
O1 Ho1 N1 73.03(11) . . ?
O1 Ho1 N1 73.02(11) 10_556 . ?
O1 Ho1 N1 73.02(11) 12_655 . ?
O1 Ho1 N1 73.02(11) 3_655 . ?
O3 Ho1 N1 144.33(9) . . ?
O3 Ho1 N1 144.33(9) 3_655 . ?
C1 Co1 C4 89.55(15) . 3_655 ?
C1 Co1 C4 89.55(15) . . ?
C4 Co1 C4 179.1(3) 3_655 . ?
C1 Co1 C3 90.30(13) . . ?
C4 Co1 C3 90.002(2) 3_655 . ?
C4 Co1 C3 90.002(2) . . ?
C1 Co1 C3 90.30(13) . 10_556 ?
C4 Co1 C3 90.002(2) 3_655 10_556 ?
C4 Co1 C3 90.002(2) . 10_556 ?
C3 Co1 C3 179.4(3) . 10_556 ?
C1 Co1 C2 180 . . ?
C4 Co1 C2 90.45(15) 3_655 . ?
C4 Co1 C2 90.45(15) . . ?
C3 Co1 C2 89.70(13) . . ?
C3 Co1 C2 89.70(13) 10_556 . ?
C1 N1 Ho1 180 . . ?
N1 C1 Co1 180 . . ?
N3 C3 Co1 179.4(4) . . ?
N2 C2 Co1 180 . . ?
N4 C4 Co1 179.1(5) . . ?
O1 C5 C9 120.7(6) . . ?
O1 C5 C6 123.4(6) . . ?
C9 C5 C6 115.8(6) . . ?
C5 O1 O1 128.1(3) . 10_556 ?
C5 O1 Ho1 149.0(4) . . ?
O1 O1 Ho1 69.82(12) 10_556 . ?
C8 C9 C5 120.2(7) . . ?
N5 C7 C6 120.6(8) . . ?
N5 C8 C9 121.0(9) . . ?
C7 N5 C8 121.4(9) . . ?
C7 C6 C5 120.8(8) . . ?
O2 C10 C11 122.4(5) . . ?
O2 C10 C14 121.4(6) . . ?
C11 C10 C14 116.2(6) . . ?
C12 C11 C10 120.9(6) . . ?
C14 C13 N6 120.9(7) . . ?
C11 C12 N6 121.1(8) . . ?
C13 N6 C12 119.8(9) . . ?
C13 C14 C10 121.1(7) . . ?
C10 O2 O2 145.7(3) . 12_655 ?
C10 O2 Ho1 138.9(4) . . ?
O2 O2 Ho1 71.83(11) 12_655 . ?


# END of CIF
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1983883'
loop_
_audit_author_name
_audit_author_address
'Jakub Zakrzewski'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2020-02-13 deposited with the CCDC.	2020-10-30 downloaded from the CCDC.
;

_audit_creation_date             2019-08-23T13:11:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C26 H24 Ir Ho N10 O6, 2(H2O)'
_chemical_formula_sum            'C26 H28 Ho Ir N10 O8'
_chemical_formula_weight         965.71

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_Int_Tables_number      63
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   14.8720(3)
_cell_length_b                   15.2339(3)
_cell_length_c                   14.1487(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3205.51(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11862
_cell_measurement_theta_min      2.395
_cell_measurement_theta_max      27.095
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1848

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    6.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.478
_exptl_absorpt_correction_T_max  0.691
_exptl_absorpt_process_details   'SADABS-2016/2 (Krause, 2015)'

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'D8Quest Eco Photon50'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_time  0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_number            11862
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.395
_diffrn_reflns_theta_max         27.095
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             1918
_reflns_number_gt                1735
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0244P)²+8.0040P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1918
_refine_ls_number_parameters     195
_refine_ls_number_restraints     7
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0187
_refine_ls_wR_factor_ref         0.0462
_refine_ls_wR_factor_gt          0.0448
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.194
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.813
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.11

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Ho1 Ho 0.5 0.44467(2) 0.25 0.01370(8) Uani 1 4 d S T P . .
Ir1 Ir 0.5 0.81398(2) 0.25 0.01422(7) Uani 1 4 d S T P . .
N2 N 0.5 1.0218(4) 0.25 0.0381(15) Uani 1 4 d S T P . .
N1 N 0.5 0.6056(3) 0.25 0.0231(11) Uani 1 4 d S T P . .
O3 O 0.4072(3) 0.3170(2) 0.25 0.0589(15) Uani 1 2 d S T P . .
H3A H 0.345586 0.328878 0.267308 0.088 Uiso 0.5 1 d R U P . .
H3B H 0.423015 0.273858 0.29793 0.088 Uiso 0.5 1 d R U P . .
C1 C 0.5 0.6820(4) 0.25 0.0163(11) Uani 1 4 d S T P . .
C3 C 0.5 0.8154(3) 0.1065(3) 0.0201(9) Uani 1 2 d S T P . .
C2 C 0.5 0.9482(4) 0.25 0.0257(15) Uani 1 4 d S T P . .
N3 N 0.5 0.8169(3) 0.0259(3) 0.0361(10) Uani 1 2 d S T P . .
C4 C 0.6364(3) 0.8128(3) 0.25 0.0385(14) Uani 1 2 d S TU P . .
O1S O 0.4286(3) 0.1735(3) 0.1531(3) 0.0260(10) Uani 0.5 1 d G . P . .
H1SA H 0.442823 0.122988 0.179956 0.039 Uiso 0.5 1 d G U P . .
H1SB H 0.46147 0.181129 0.102295 0.039 Uiso 0.5 1 d G U P . .
N4 N 0.7121(4) 0.8108(4) 0.25 0.090(2) Uani 1 2 d S TU P . .
C5 C 0.6810(5) 0.5381(4) 0.1389(5) 0.0234(13) Uani 0.5 1 d . . P A 1
O1 O 0.6359(3) 0.4882(3) 0.1923(3) 0.0268(10) Uani 0.5 1 d . . P A 1
C9 C 0.7756(6) 0.5467(6) 0.1490(7) 0.048(2) Uani 0.5 1 d . . P A 1
H9 H 0.805187 0.518305 0.200066 0.057 Uiso 0.5 1 calc R U P A 1
C7 C 0.6972(10) 0.6340(5) 0.0036(6) 0.060(3) Uani 0.5 1 d . . P A 1
H7 H 0.670531 0.665502 -0.047094 0.072 Uiso 0.5 1 calc R U P A 1
C8 C 0.8241(8) 0.5947(8) 0.0869(10) 0.072(3) Uani 0.5 1 d . . P A 1
H8 H 0.887467 0.59848 0.094626 0.087 Uiso 0.5 1 calc R U P A 1
N5 N 0.7848(12) 0.6373(11) 0.0142(11) 0.059(5) Uani 0.5 1 d . . P A 1
H5N H 0.817901 0.667248 -0.026054 0.10(4) Uiso 0.5 1 calc R . P A 1
C6 C 0.6425(6) 0.5866(6) 0.0634(6) 0.0371(17) Uani 0.5 1 d . . P A 1
H6 H 0.579207 0.586379 0.054071 0.044 Uiso 0.5 1 calc R U P A 1
C10 C 0.3792(4) 0.4075(4) 0.4441(4) 0.0223(12) Uani 0.5 1 d . . P A 2
C11 C 0.2920(5) 0.4169(5) 0.4062(5) 0.0307(15) Uani 0.5 1 d . . P A 2
H11 H 0.284715 0.439269 0.34396 0.037 Uiso 0.5 1 calc R U P A 2
C13 C 0.3084(6) 0.3518(5) 0.5843(6) 0.0376(18) Uani 0.5 1 d . . P A 2
H13 H 0.313617 0.328523 0.646329 0.045 Uiso 0.5 1 calc R U P A 2
C12 C 0.2184(6) 0.3944(6) 0.4572(7) 0.0376(19) Uani 0.5 1 d . . P A 2
H12 H 0.160276 0.400549 0.430098 0.045 Uiso 0.5 1 calc R U P A 2
N6 N 0.2271(8) 0.3629(10) 0.5478(7) 0.035(3) Uani 0.5 1 d . . P A 2
H6N H 0.179046 0.350152 0.581347 0.042 Uiso 0.5 1 calc R U P A 2
C14 C 0.3844(5) 0.3725(5) 0.5361(5) 0.0308(15) Uani 0.5 1 d . . P A 2
H14 H 0.441513 0.363292 0.564555 0.037 Uiso 0.5 1 calc R U P A 2
O2 O 0.4501(3) 0.4299(3) 0.3981(3) 0.0270(10) Uani 0.5 1 d . . P A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Ho1 O2 2.235(4) 10_556 ?
Ho1 O2 2.235(4) 12_655 ?
Ho1 O2 2.235(4) 3_655 ?
Ho1 O2 2.235(4) . ?
Ho1 O1 2.278(4) 10_556 ?
Ho1 O1 2.278(4) 12_655 ?
Ho1 O1 2.278(4) 3_655 ?
Ho1 O1 2.278(4) . ?
Ho1 O3 2.385(3) . ?
Ho1 O3 2.385(3) 3_655 ?
Ho1 N1 2.452(5) . ?
Ir1 C1 2.011(6) . ?
Ir1 C4 2.029(5) 3_655 ?
Ir1 C4 2.029(5) . ?
Ir1 C3 2.030(4) 10_556 ?
Ir1 C3 2.030(4) . ?
Ir1 C2 2.045(6) . ?
N2 C2 1.121(8) . ?
N1 C1 1.163(8) . ?
O3 H3A 0.9659 . ?
O3 H3B 0.9729 . ?
C3 N3 1.141(6) . ?
C4 N4 1.126(8) . ?
O1S H1SA 0.884 . ?
O1S H1SB 0.877 . ?
C5 O1 1.265(8) . ?
C5 C6 1.419(11) . ?
C5 C9 1.420(10) . ?
O1 O1 1.634(10) 10_556 ?
C9 C8 1.351(13) . ?
C9 H9 0.95 . ?
C7 N5 1.31(2) . ?
C7 C6 1.378(14) . ?
C7 H7 0.95 . ?
C8 N5 1.35(2) . ?
C8 H8 0.95 . ?
N5 H5N 0.88 . ?
C6 H6 0.95 . ?
C10 O2 1.284(8) . ?
C10 C14 1.409(9) . ?
C10 C11 1.411(9) . ?
C11 C12 1.354(10) . ?
C11 H11 0.95 . ?
C13 N6 1.325(15) . ?
C13 C14 1.358(11) . ?
C13 H13 0.95 . ?
C12 N6 1.376(13) . ?
C12 H12 0.95 . ?
N6 H6N 0.88 . ?
C14 H14 0.95 . ?
O2 O2 1.485(9) 12_655 ?

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
O2 Ho1 O2 168.5(2) 10_556 12_655 ?
O2 Ho1 O2 139.4(2) 10_556 . ?
O2 Ho1 O2 38.8(2) 12_655 . ?
O2 Ho1 O2 168.5(2) 3_655 . ?
O1 Ho1 O1 146.2(2) 10_556 12_655 ?
O1 Ho1 O1 125.0(2) 10_556 3_655 ?
O1 Ho1 O1 42.0(2) 12_655 3_655 ?
O1 Ho1 O1 42.0(2) 10_556 . ?
O1 Ho1 O1 125.0(2) 12_655 . ?
O1 Ho1 O1 146.2(2) 3_655 . ?
O2 Ho1 O3 74.08(12) 10_556 . ?
O2 Ho1 O3 96.33(13) 12_655 . ?
O2 Ho1 O3 96.33(13) 3_655 . ?
O2 Ho1 O3 74.08(12) . . ?
O1 Ho1 O3 138.63(14) 10_556 . ?
O1 Ho1 O3 73.98(14) 12_655 . ?
O1 Ho1 O3 73.98(14) 3_655 . ?
O1 Ho1 O3 138.63(14) . . ?
O1 Ho1 O3 73.98(14) 10_556 3_655 ?
O1 Ho1 O3 138.63(14) 12_655 3_655 ?
O1 Ho1 O3 138.63(14) 3_655 3_655 ?
O1 Ho1 O3 73.99(14) . 3_655 ?
O3 Ho1 O3 70.70(18) . 3_655 ?
O2 Ho1 N1 95.77(12) 10_556 . ?
O2 Ho1 N1 95.77(12) 12_655 . ?
O2 Ho1 N1 95.77(12) 3_655 . ?
O2 Ho1 N1 95.77(12) . . ?
O1 Ho1 N1 73.09(11) 10_556 . ?
O1 Ho1 N1 73.09(11) 12_655 . ?
O1 Ho1 N1 73.09(11) 3_655 . ?
O1 Ho1 N1 73.09(11) . . ?
O3 Ho1 N1 144.65(9) . . ?
O3 Ho1 N1 144.65(9) 3_655 . ?
C1 Ir1 C4 89.48(13) . 3_655 ?
C1 Ir1 C4 89.48(13) . . ?
C4 Ir1 C4 179.0(3) 3_655 . ?
C1 Ir1 C3 90.61(12) . 10_556 ?
C4 Ir1 C3 90.005(2) 3_655 10_556 ?
C4 Ir1 C3 90.005(2) . 10_556 ?
C1 Ir1 C3 90.61(12) . . ?
C4 Ir1 C3 90.005(2) 3_655 . ?
C4 Ir1 C3 90.005(2) . . ?
C3 Ir1 C3 178.8(2) 10_556 . ?
C1 Ir1 C2 180 . . ?
C4 Ir1 C2 90.52(13) 3_655 . ?
C4 Ir1 C2 90.52(13) . . ?
C3 Ir1 C2 89.39(12) 10_556 . ?
C3 Ir1 C2 89.39(12) . . ?
C1 N1 Ho1 180 . . ?
Ho1 O3 H3A 113.3 . . ?
Ho1 O3 H3B 114.3 . . ?
H3A O3 H3B 100.3 . . ?
N1 C1 Ir1 180 . . ?
N3 C3 Ir1 179.4(4) . . ?
N2 C2 Ir1 180 . . ?
N4 C4 Ir1 179.0(5) . . ?
H1SA O1S H1SB 109.5 . . ?
O1 C5 C6 123.2(7) . . ?
O1 C5 C9 121.4(7) . . ?
C6 C5 C9 115.3(7) . . ?
C5 O1 O1 126.7(4) . 10_556 ?
C5 O1 Ho1 149.3(4) . . ?
O1 O1 Ho1 68.98(12) 10_556 . ?
C8 C9 C5 120.9(10) . . ?
C8 C9 H9 119.6 . . ?
C5 C9 H9 119.6 . . ?
N5 C7 C6 122.5(11) . . ?
N5 C7 H7 118.8 . . ?
C6 C7 H7 118.8 . . ?
N5 C8 C9 121.6(11) . . ?
N5 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C7 N5 C8 119.9(10) . . ?
C7 N5 H5N 120.1 . . ?
C8 N5 H5N 120.1 . . ?
C7 C6 C5 119.7(9) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
O2 C10 C14 121.5(6) . . ?
O2 C10 C11 122.4(6) . . ?
C14 C10 C11 116.1(6) . . ?
C12 C11 C10 121.0(7) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
N6 C13 C14 122.3(8) . . ?
N6 C13 H13 118.8 . . ?
C14 C13 H13 118.8 . . ?
C11 C12 N6 120.6(9) . . ?
C11 C12 H12 119.7 . . ?
N6 C12 H12 119.7 . . ?
C13 N6 C12 119.6(9) . . ?
C13 N6 H6N 120.2 . . ?
C12 N6 H6N 120.2 . . ?
C13 C14 C10 120.4(7) . . ?
C13 C14 H14 119.8 . . ?
C10 C14 H14 119.8 . . ?
C10 O2 O2 145.2(4) . 12_655 ?
C10 O2 Ho1 140.7(4) . . ?
O2 O2 Ho1 70.59(12) 12_655 . ?


# END of CIF
####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1983882'
loop_
_audit_author_name
_audit_author_address
'Jakub Zakrzewski'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2020-02-13 deposited with the CCDC.	2020-10-30 downloaded from the CCDC.
;

_audit_creation_date             2019-08-23T13:05:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C26 H24 Rh Ho N10 O6, 2(H2O)'
_chemical_formula_sum            'C26 H28 Ho N10 O8 Rh'
_chemical_formula_weight         876.42

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_Int_Tables_number      63
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, z'
'x, -y, z+1/2'
'-x, -y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'x, -y, -z'
'-x, y, -z-1/2'
'x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z-1/2'
'x+1/2, y+1/2, -z-1/2'

_cell_length_a                   14.8236(6)
_cell_length_b                   15.1198(8)
_cell_length_c                   14.0660(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3152.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    14551
_cell_measurement_theta_min      3.059
_cell_measurement_theta_max      27.461
_cell_measurement_wavelength     0.71075

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.089
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1720

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_T_max  0.771

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_radiation_type           MoK\a
_diffrn_measurement_method       ω
_diffrn_radiation_probe          x-ray
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_number            14551
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.059
_diffrn_reflns_theta_max         27.461
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_reflns_Friedel_coverage         0
_reflns_number_total             1947
_reflns_number_gt                1762
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0222P)²+61.1278P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1947
_refine_ls_number_parameters     195
_refine_ls_number_restraints     15
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0574
_refine_ls_wR_factor_ref         0.0969
_refine_ls_wR_factor_gt          0.0935
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_restrained_S_all      1.196
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.513
_refine_diff_density_min         -3.974
_refine_diff_density_rms         0.202

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Ho1 Ho 0.5 0.44336(4) 0.25 0.00921(16) Uani 1 4 d S T P . .
Rh1 Rh 0.5 0.81384(7) 0.25 0.0158(3) Uani 1 4 d S T P . .
N2 N 0.5 1.0249(7) 0.25 0.018(2) Uani 1 4 d S TU P . .
N1 N 0.5 0.6044(6) 0.25 0.009(2) Uani 1 4 d S TU P . .
O3 O 0.4077(5) 0.3152(5) 0.25 0.050(3) Uani 1 2 d S T P . .
H3A H 0.347906 0.326102 0.273291 0.076 Uiso 0.5 1 d R U P . .
H3B H 0.427143 0.269826 0.293459 0.076 Uiso 0.5 1 d R U P . .
C1 C 0.5 0.6897(10) 0.25 0.028(3) Uani 1 4 d S TU P . .
C3 C 0.5 0.8147(6) 0.1076(7) 0.020(2) Uani 1 2 d S T P . .
C2 C 0.5 0.9499(10) 0.25 0.018(3) Uani 1 4 d S TU P . .
N3 N 0.5 0.8161(6) 0.0261(6) 0.031(2) Uani 1 2 d S T P . .
C4 C 0.6344(7) 0.8126(7) 0.25 0.041(3) Uani 1 2 d S TU P . .
O1S O 0.4292(6) 0.1728(6) 0.1528(7) 0.022(2) Uani 0.5 1 d G . P . .
H1SA H 0.453156 0.132688 0.190297 0.033 Uiso 0.5 1 d G U P . .
H1SB H 0.461638 0.177581 0.101333 0.033 Uiso 0.5 1 d G U P . .
N4 N 0.7114(9) 0.8110(9) 0.25 0.080(4) Uani 1 2 d S TU P . .
C5 C 0.6812(10) 0.5382(8) 0.1390(10) 0.023(3) Uani 0.5 1 d . . P A 1
O1 O 0.6367(6) 0.4865(7) 0.1926(7) 0.023(2) Uani 0.5 1 d . . P A 1
C9 C 0.7767(9) 0.5462(11) 0.1496(13) 0.038(4) Uani 0.5 1 d . . P A 1
H9 H 0.80708 0.517771 0.200586 0.046 Uiso 0.5 1 calc R U P A 1
C7 C 0.6959(14) 0.6349(11) 0.0025(12) 0.044(5) Uani 0.5 1 d . . P A 1
H7 H 0.668867 0.667191 -0.047926 0.053 Uiso 0.5 1 calc R U P A 1
C8 C 0.8235(14) 0.5955(13) 0.0850(19) 0.061(6) Uani 0.5 1 d . . P A 1
H8 H 0.887045 0.600513 0.091579 0.073 Uiso 0.5 1 calc R U P A 1
N5 N 0.783(2) 0.637(3) 0.0127(19) 0.044(9) Uani 0.5 1 d . . P A 1
H5N H 0.815884 0.666246 -0.028759 0.04(5) Uiso 0.5 1 calc R . P A 1
C6 C 0.6424(13) 0.5873(12) 0.0626(12) 0.031(4) Uani 0.5 1 d . . P A 1
H6 H 0.578916 0.586903 0.05357 0.037 Uiso 0.5 1 calc R U P A 1
C10 C 0.3792(9) 0.4066(9) 0.4457(10) 0.021(3) Uani 0.5 1 d . . P A 2
C11 C 0.2921(9) 0.4175(9) 0.4071(11) 0.024(3) Uani 0.5 1 d . . P A 2
H11 H 0.285784 0.441294 0.344958 0.029 Uiso 0.5 1 calc R U P A 2
C13 C 0.3078(10) 0.3522(10) 0.5855(12) 0.029(4) Uani 0.5 1 d . . P A 2
H13 H 0.312787 0.329965 0.648425 0.035 Uiso 0.5 1 calc R U P A 2
C12 C 0.2182(11) 0.3950(12) 0.4560(13) 0.029(4) Uani 0.5 1 d . . P A 2
H12 H 0.160362 0.401204 0.427591 0.035 Uiso 0.5 1 calc R U P A 2
N6 N 0.225(2) 0.363(3) 0.5479(15) 0.033(7) Uani 0.5 1 d . . P A 2
H6N H 0.176949 0.349593 0.581032 0.039 Uiso 0.5 1 calc R U P A 2
C14 C 0.3833(11) 0.3718(13) 0.5377(12) 0.031(4) Uani 0.5 1 d . . P A 2
H14 H 0.440342 0.361991 0.566657 0.037 Uiso 0.5 1 calc R U P A 2
O2 O 0.4514(6) 0.4301(6) 0.3996(7) 0.025(2) Uani 0.5 1 d . . P A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Ho1 O2 2.233(9) 12_556 ?
Ho1 O2 2.233(9) 2_655 ?
Ho1 O2 2.233(9) 11_656 ?
Ho1 O2 2.233(9) . ?
Ho1 O1 2.276(9) . ?
Ho1 O1 2.276(9) 12_556 ?
Ho1 O1 2.276(9) 2_655 ?
Ho1 O1 2.276(9) 11_656 ?
Ho1 O3 2.372(7) . ?
Ho1 O3 2.372(7) 2_655 ?
Ho1 N1 2.434(10) . ?
Rh1 C1 1.877(15) . ?
Rh1 C4 1.992(11) 2_655 ?
Rh1 C4 1.992(11) . ?
Rh1 C3 2.003(10) 11_656 ?
Rh1 C3 2.003(10) . ?
Rh1 C2 2.057(15) . ?
N2 C2 1.134(18) . ?
N1 C1 1.290(18) . ?
O3 H3A 0.959 . ?
O3 H3B 0.9634 . ?
C3 N3 1.147(13) . ?
C4 N4 1.142(16) . ?
O1S H1SA 0.878 . ?
O1S H1SB 0.8724 . ?
C5 O1 1.271(16) . ?
C5 C9 1.43(2) . ?
C5 C6 1.43(2) . ?
O1 O1 1.614(19) 12_556 ?
C9 C8 1.36(2) . ?
C9 H9 0.95 . ?
C7 N5 1.30(4) . ?
C7 C6 1.36(2) . ?
C7 H7 0.95 . ?
C8 N5 1.34(4) . ?
C8 H8 0.95 . ?
N5 H5N 0.88 . ?
C6 H6 0.95 . ?
C10 O2 1.301(16) . ?
C10 C14 1.40(2) . ?
C10 C11 1.410(19) . ?
C11 C12 1.34(2) . ?
C11 H11 0.95 . ?
C13 C14 1.34(2) . ?
C13 N6 1.34(3) . ?
C13 H13 0.95 . ?
C12 N6 1.39(3) . ?
C12 H12 0.95 . ?
N6 H6N 0.88 . ?
C14 H14 0.95 . ?
O2 O2 1.440(18) 2_655 ?

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
O2 Ho1 O2 140.9(5) 12_556 . ?
O2 Ho1 O2 37.6(5) 2_655 . ?
O2 Ho1 O2 169.7(5) 11_656 . ?
O1 Ho1 O1 41.5(5) . 12_556 ?
O1 Ho1 O1 125.8(5) . 2_655 ?
O1 Ho1 O1 146.7(5) 12_556 2_655 ?
O1 Ho1 O1 146.7(5) . 11_656 ?
O1 Ho1 O1 125.8(5) 12_556 11_656 ?
O1 Ho1 O1 41.5(5) 2_655 11_656 ?
O2 Ho1 O3 75.0(2) 12_556 . ?
O2 Ho1 O3 96.5(3) 2_655 . ?
O2 Ho1 O3 96.5(3) 11_656 . ?
O2 Ho1 O3 75.0(2) . . ?
O1 Ho1 O3 138.4(3) . . ?
O1 Ho1 O3 138.4(3) 12_556 . ?
O1 Ho1 O3 73.8(3) 2_655 . ?
O1 Ho1 O3 73.8(3) 11_656 . ?
O1 Ho1 O3 73.8(3) . 2_655 ?
O1 Ho1 O3 73.8(3) 12_556 2_655 ?
O1 Ho1 O3 138.4(3) 2_655 2_655 ?
O1 Ho1 O3 138.4(3) 11_656 2_655 ?
O3 Ho1 O3 70.5(3) . 2_655 ?
O2 Ho1 N1 95.2(2) 12_556 . ?
O2 Ho1 N1 95.2(2) 2_655 . ?
O2 Ho1 N1 95.2(2) 11_656 . ?
O2 Ho1 N1 95.2(2) . . ?
O1 Ho1 N1 73.3(2) . . ?
O1 Ho1 N1 73.3(2) 12_556 . ?
O1 Ho1 N1 73.3(2) 2_655 . ?
O1 Ho1 N1 73.3(2) 11_656 . ?
O3 Ho1 N1 144.77(17) . . ?
O3 Ho1 N1 144.77(17) 2_655 . ?
C1 Rh1 C4 89.4(3) . 2_655 ?
C1 Rh1 C4 89.4(3) . . ?
C4 Rh1 C4 178.9(6) 2_655 . ?
C1 Rh1 C3 90.4(3) . 11_656 ?
C4 Rh1 C3 90.004(4) 2_655 11_656 ?
C4 Rh1 C3 90.004(4) . 11_656 ?
C1 Rh1 C3 90.4(3) . . ?
C4 Rh1 C3 90.004(4) 2_655 . ?
C4 Rh1 C3 90.004(5) . . ?
C3 Rh1 C3 179.2(5) 11_656 . ?
C1 Rh1 C2 180 . . ?
C4 Rh1 C2 90.6(3) 2_655 . ?
C4 Rh1 C2 90.6(3) . . ?
C3 Rh1 C2 89.6(3) 11_656 . ?
C3 Rh1 C2 89.6(3) . . ?
C1 N1 Ho1 180 . . ?
Ho1 O3 H3A 113.2 . . ?
Ho1 O3 H3B 114.2 . . ?
H3A O3 H3B 100.5 . . ?
N1 C1 Rh1 180 . . ?
N3 C3 Rh1 179.4(9) . . ?
N2 C2 Rh1 180 . . ?
N4 C4 Rh1 179.4(12) . . ?
H1SA O1S H1SB 109.5 . . ?
O1 C5 C9 120.4(14) . . ?
O1 C5 C6 123.9(14) . . ?
C9 C5 C6 115.7(14) . . ?
C5 O1 O1 126.4(8) . 12_556 ?
C5 O1 Ho1 148.1(9) . . ?
O1 O1 Ho1 69.2(2) 12_556 . ?
C8 C9 C5 118.7(17) . . ?
C8 C9 H9 120.6 . . ?
C5 C9 H9 120.6 . . ?
N5 C7 C6 121(2) . . ?
N5 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
N5 C8 C9 122(2) . . ?
N5 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C7 N5 C8 121(2) . . ?
C7 N5 H5N 119.4 . . ?
C8 N5 H5N 119.4 . . ?
C7 C6 C5 120.5(17) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
O2 C10 C14 121.9(13) . . ?
O2 C10 C11 122.0(13) . . ?
C14 C10 C11 116.1(13) . . ?
C12 C11 C10 121.5(15) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C14 C13 N6 122.5(18) . . ?
C14 C13 H13 118.7 . . ?
N6 C13 H13 118.7 . . ?
C11 C12 N6 120(2) . . ?
C11 C12 H12 119.8 . . ?
N6 C12 H12 119.8 . . ?
C13 N6 C12 119(2) . . ?
C13 N6 H6N 120.6 . . ?
C12 N6 H6N 120.6 . . ?
C13 C14 C10 120.7(15) . . ?
C13 C14 H14 119.6 . . ?
C10 C14 H14 119.6 . . ?
C10 O2 Ho1 139.4(8) . . ?
O2 O2 Ho1 71.2(2) 2_655 . ?

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
C9 C5 O1 O1 54.5(16) . . . 12_556 ?
C6 C5 O1 O1 -129.2(12) . . . 12_556 ?
C9 C5 O1 Ho1 165.0(13) . . . . ?
C6 C5 O1 Ho1 -19(3) . . . . ?
O1 C5 C9 C8 173.6(16) . . . . ?
C6 C5 C9 C8 -3(2) . . . . ?
C5 C9 C8 N5 0(4) . . . . ?
C6 C7 N5 C8 -3(5) . . . . ?
C9 C8 N5 C7 3(5) . . . . ?
N5 C7 C6 C5 0(3) . . . . ?
O1 C5 C6 C7 -173.7(15) . . . . ?
C9 C5 C6 C7 3(2) . . . . ?
O2 C10 C11 C12 -178.4(14) . . . . ?
C14 C10 C11 C12 0(2) . . . . ?
C10 C11 C12 N6 2(3) . . . . ?
C14 C13 N6 C12 0(5) . . . . ?
C11 C12 N6 C13 -2(5) . . . . ?
N6 C13 C14 C10 1(3) . . . . ?
O2 C10 C14 C13 176.7(15) . . . . ?
C11 C10 C14 C13 -1(3) . . . . ?
C14 C10 O2 O2 8(2) . . . 2_655 ?
C11 C10 O2 O2 -174.4(8) . . . 2_655 ?
C14 C10 O2 Ho1 152.7(13) . . . . ?
C11 C10 O2 Ho1 -29(2) . . . . ?


# END of CIF
