# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1041434'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H26 Ho N5 O17'
_chemical_formula_weight         941.53

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'
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 0.0060 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   p21/m

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

_cell_length_a                   7.6609(15)
_cell_length_b                   21.518(4)
_cell_length_c                   12.258(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.82(3)
_cell_angle_gamma                90.00
_cell_volume                     1996.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5808
_cell_measurement_theta_min      1.68
_cell_measurement_theta_max      25.01

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    2.059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16521
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3622
_reflns_number_gt                3388
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. The atom O8 was restrained with the ?°ISOR?+- command due to their unreasonable anisotropic Ueq parameters and obvious ADP problems. Furthermore, some constraints (SIMU, DFIX, and DANG) were applied to the H2O molecule. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1157P)²+48.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3622
_refine_ls_number_parameters     272
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0734
_refine_ls_wR_factor_ref         0.2019
_refine_ls_wR_factor_gt          0.1947
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O8 O 0.708(2) 0.6866(7) 1.1536(10) 0.102(4) Uani 1 1 d U . .
O9 O 0.7384(8) 0.6657(3) 1.3254(5) 0.0177(14) Uani 1 1 d . . .
C12 C 0.6700(19) 0.6547(6) 1.2287(10) 0.047(4) Uani 1 1 d . . .
C13 C 0.5680(14) 0.5462(5) 1.2688(8) 0.025(2) Uani 1 1 d . . .
H13 H 0.6368 0.5483 1.3381 0.030 Uiso 1 1 calc R . .
Ho1 Ho 0.08415(7) 0.2500 0.73279(4) 0.0125(2) Uani 1 2 d SD . .
O3 O -0.2951(10) 0.3670(3) 0.5570(5) 0.0229(15) Uani 1 1 d . . .
O6 O 0.4266(10) 0.3868(4) 1.2844(6) 0.0300(18) Uani 1 1 d . . .
O5 O -0.0216(10) 0.6484(3) 0.6029(6) 0.0287(17) Uani 1 1 d . . .
O2 O -0.1234(9) 0.3243(3) 0.6976(6) 0.0233(15) Uani 1 1 d . . .
O1 O 0.0299(13) 0.2500 0.5356(7) 0.0177(19) Uani 1 2 d SD . .
H1 H 0.052(14) 0.2178(5) 0.500(5) 0.027 Uiso 1 1 d D . .
O4 O -0.2131(11) 0.5890(3) 0.4932(6) 0.0284(17) Uani 1 1 d . . .
H4 H -0.2019 0.6149 0.4456 0.043 Uiso 1 1 calc R . .
O7 O 0.5935(13) 0.4483(4) 1.4026(6) 0.040(2) Uani 1 1 d . . .
H7 H 0.5925 0.4186 1.4443 0.059 Uiso 1 1 calc R . .
N3 N 0.6162(15) 0.2500 0.4651(10) 0.019(2) Uani 1 2 d S . .
H3A H 0.6657 0.2838 0.5003 0.023 Uiso 0.50 1 calc PR . .
H3B H 0.6657 0.2162 0.5003 0.023 Uiso 0.50 1 calc PR . .
C1 C -0.1837(12) 0.3707(4) 0.6413(8) 0.0151(19) Uani 1 1 d . . .
N1 N 0.1654(13) 0.4935(5) 0.9302(8) 0.033(2) Uani 1 1 d . . .
C3 C -0.1409(13) 0.4865(4) 0.6174(8) 0.0177(19) Uani 1 1 d . . .
H3 H -0.2104 0.4840 0.5484 0.021 Uiso 1 1 calc R . .
C2 C -0.1123(12) 0.4334(4) 0.6826(8) 0.0159(19) Uani 1 1 d . . .
C5 C -0.0955(13) 0.5996(4) 0.5815(8) 0.019(2) Uani 1 1 d . . .
C6 C 0.0369(14) 0.5478(5) 0.7574(8) 0.021(2) Uani 1 1 d . . .
H6 H 0.0892 0.5854 0.7814 0.026 Uiso 1 1 calc R . .
N2 N 0.2504(14) 0.5430(5) 0.9569(7) 0.037(2) Uani 1 1 d . . .
C16 C 0.4948(14) 0.4363(5) 1.3092(8) 0.023(2) Uani 1 1 d . . .
C17 C 0.421(2) 0.2500 0.4696(14) 0.031(4) Uani 1 2 d S . .
H17A H 0.4015 0.2563 0.5443 0.047 Uiso 0.50 1 calc PR A -1
H17B H 0.3710 0.2108 0.4434 0.047 Uiso 0.50 1 calc PR A -1
H17C H 0.3651 0.2828 0.4238 0.047 Uiso 0.50 1 calc PR A -1
C7 C 0.0610(13) 0.4955(5) 0.8239(8) 0.024(2) Uani 1 1 d . . .
C4 C -0.0669(12) 0.5431(5) 0.6541(8) 0.0181(19) Uani 1 1 d . . .
C14 C 0.4760(14) 0.4918(5) 1.2349(8) 0.025(2) Uani 1 1 d . . .
C18 C 0.652(2) 0.2500 0.3508(13) 0.028(3) Uani 1 2 d S . .
H18A H 0.5757 0.2793 0.3080 0.042 Uiso 0.50 1 calc PR B -1
H18B H 0.6313 0.2092 0.3198 0.042 Uiso 0.50 1 calc PR B -1
H18C H 0.7730 0.2615 0.3499 0.042 Uiso 0.50 1 calc PR B -1
C8 C -0.0140(13) 0.4389(5) 0.7874(8) 0.022(2) Uani 1 1 d . . .
H8 H 0.0017 0.4044 0.8336 0.026 Uiso 1 1 calc R . .
C15 C 0.3700(14) 0.4890(5) 1.1324(8) 0.025(2) Uani 1 1 d . . .
H15 H 0.3093 0.4526 1.1100 0.030 Uiso 1 1 calc R . .
C9 C 0.3552(16) 0.5400(6) 1.0644(9) 0.035(3) Uani 1 1 d . . .
C10 C 0.454(2) 0.5943(7) 1.0949(10) 0.052(4) Uani 1 1 d . . .
H10 H 0.4504 0.6276 1.0462 0.063 Uiso 1 1 calc R . .
C11 C 0.5559(17) 0.5975(6) 1.1981(9) 0.037(3) 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
O8 C12 1.219(17) . ?
O8 Ho1 2.377(11) 3_667 ?
O9 C12 1.243(14) . ?
O9 Ho1 2.438(6) 3_667 ?
C12 C11 1.523(15) . ?
C12 Ho1 2.775(12) 3_667 ?
C13 C14 1.397(15) . ?
C13 C11 1.397(15) . ?
Ho1 O2 2.249(7) 4_565 ?
Ho1 O2 2.249(7) . ?
Ho1 O8 2.377(11) 3_667 ?
Ho1 O8 2.377(11) 2_647 ?
Ho1 O1 2.389(9) . ?
Ho1 O9 2.438(6) 3_667 ?
Ho1 O9 2.438(6) 2_647 ?
Ho1 C12 2.775(12) 3_667 ?
Ho1 C12 2.775(12) 2_647 ?
O3 C1 1.237(11) . ?
O6 C16 1.204(13) . ?
O5 C5 1.202(12) . ?
O2 C1 1.262(12) . ?
O4 C5 1.318(12) . ?
O7 C16 1.298(13) . ?
N3 C18 1.469(19) . ?
N3 C17 1.507(19) . ?
C1 C2 1.512(13) . ?
N1 N2 1.265(13) . ?
N1 C7 1.421(13) . ?
C3 C4 1.390(14) . ?
C3 C2 1.392(13) . ?
C2 C8 1.391(13) . ?
C5 C4 1.503(13) . ?
C6 C7 1.385(14) . ?
C6 C4 1.392(13) . ?
N2 C9 1.435(13) . ?
C16 C14 1.497(15) . ?
C7 C8 1.391(15) . ?
C14 C15 1.388(14) . ?
C15 C9 1.373(16) . ?
C9 C10 1.411(17) . ?
C10 C11 1.383(16) . ?

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
C12 O8 Ho1 95.6(8) . 3_667 ?
C12 O9 Ho1 92.0(7) . 3_667 ?
O8 C12 O9 119.9(11) . . ?
O8 C12 C11 117.7(12) . . ?
O9 C12 C11 122.0(10) . . ?
O8 C12 Ho1 58.5(7) . 3_667 ?
O9 C12 Ho1 61.4(6) . 3_667 ?
C11 C12 Ho1 171.1(12) . 3_667 ?
C14 C13 C11 119.6(9) . . ?
O2 Ho1 O2 90.6(4) 4_565 . ?
O2 Ho1 O8 155.5(4) 4_565 3_667 ?
O2 Ho1 O8 95.4(5) . 3_667 ?
O2 Ho1 O8 95.4(5) 4_565 2_647 ?
O2 Ho1 O8 155.5(4) . 2_647 ?
O8 Ho1 O8 70.1(7) 3_667 2_647 ?
O2 Ho1 O1 78.3(3) 4_565 . ?
O2 Ho1 O1 78.3(3) . . ?
O8 Ho1 O1 126.1(3) 3_667 . ?
O8 Ho1 O1 126.1(3) 2_647 . ?
O2 Ho1 O9 151.9(2) 4_565 3_667 ?
O2 Ho1 O9 79.9(2) . 3_667 ?
O8 Ho1 O9 52.5(3) 3_667 3_667 ?
O8 Ho1 O9 104.2(5) 2_647 3_667 ?
O1 Ho1 O9 73.9(2) . 3_667 ?
O2 Ho1 O9 79.9(2) 4_565 2_647 ?
O2 Ho1 O9 151.9(2) . 2_647 ?
O8 Ho1 O9 104.2(5) 3_667 2_647 ?
O8 Ho1 O9 52.5(3) 2_647 2_647 ?
O1 Ho1 O9 73.9(2) . 2_647 ?
O9 Ho1 O9 96.1(3) 3_667 2_647 ?
O2 Ho1 C12 177.5(3) 4_565 3_667 ?
O2 Ho1 C12 87.1(4) . 3_667 ?
O8 Ho1 C12 25.9(4) 3_667 3_667 ?
O8 Ho1 C12 87.1(5) 2_647 3_667 ?
O1 Ho1 C12 100.4(3) . 3_667 ?
O9 Ho1 C12 26.6(3) 3_667 3_667 ?
O9 Ho1 C12 101.8(4) 2_647 3_667 ?
O2 Ho1 C12 87.1(4) 4_565 2_647 ?
O2 Ho1 C12 177.5(3) . 2_647 ?
O8 Ho1 C12 87.1(5) 3_667 2_647 ?
O8 Ho1 C12 25.9(4) 2_647 2_647 ?
O1 Ho1 C12 100.4(3) . 2_647 ?
O9 Ho1 C12 101.8(4) 3_667 2_647 ?
O9 Ho1 C12 26.6(3) 2_647 2_647 ?
C12 Ho1 C12 95.3(6) 3_667 2_647 ?
C1 O2 Ho1 149.0(6) . . ?
C18 N3 C17 111.6(11) . . ?
O3 C1 O2 123.5(9) . . ?
O3 C1 C2 120.4(8) . . ?
O2 C1 C2 116.1(8) . . ?
N2 N1 C7 114.1(9) . . ?
C4 C3 C2 120.9(8) . . ?
C8 C2 C3 118.4(9) . . ?
C8 C2 C1 120.1(8) . . ?
C3 C2 C1 121.5(8) . . ?
O5 C5 O4 124.8(9) . . ?
O5 C5 C4 123.8(9) . . ?
O4 C5 C4 111.4(8) . . ?
C7 C6 C4 118.8(9) . . ?
N1 N2 C9 113.1(9) . . ?
O6 C16 O7 124.9(10) . . ?
O6 C16 C14 123.7(9) . . ?
O7 C16 C14 111.5(9) . . ?
C6 C7 C8 120.8(9) . . ?
C6 C7 N1 124.6(9) . . ?
C8 C7 N1 114.6(9) . . ?
C3 C4 C6 120.4(9) . . ?
C3 C4 C5 120.2(8) . . ?
C6 C4 C5 119.4(9) . . ?
C15 C14 C13 120.3(10) . . ?
C15 C14 C16 120.3(9) . . ?
C13 C14 C16 119.4(9) . . ?
C7 C8 C2 120.6(9) . . ?
C9 C15 C14 119.8(10) . . ?
C15 C9 C10 120.7(10) . . ?
C15 C9 N2 125.2(10) . . ?
C10 C9 N2 114.0(10) . . ?
C11 C10 C9 119.2(11) . . ?
C10 C11 C13 120.2(10) . . ?
C10 C11 C12 119.2(10) . . ?
C13 C11 C12 120.3(9) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         6.516
_refine_diff_density_min         -2.347
_refine_diff_density_rms         0.332
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.034 0.250 0.067 199.3 57.5
2 0.010 0.750 -0.067 199.3 55.8
_platon_squeeze_details          
; ?
;
