# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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. 
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data_1
_database_code_depnum_ccdc_archive 'CCDC 2059754'
_audit_update_record             
;
2021-01-29 deposited with the CCDC.	2021-03-03 downloaded from the CCDC.
;
_audit_creation_date             2020-10-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        'Ho(tppo)2(H2O)5Cl3 H2O'
_chemical_formula_moiety         'C24 H60 Cl3 Ho N6 O8 P2'
_chemical_formula_sum            'C24 H60 Cl3 Ho N6 O8 P2'
_chemical_formula_weight         894.00
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'C H O Dy'
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'
Cl Cl 0.1484 0.1585 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   9.9663(3)
_cell_length_b                   26.9370(9)
_cell_length_c                   30.2924(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8132.4(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9137
_cell_measurement_temperature    293
_cell_measurement_theta_max      24.9670
_cell_measurement_theta_min      2.2730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.267
_exptl_absorpt_correction_T_max  0.69235
_exptl_absorpt_correction_T_min  0.62499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3664
_exptl_crystal_preparation       NONE
_exptl_crystal_recrystallization_method NONE
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            43248
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.655
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     32.00 109.00   0.50   12.00    --   20.00  54.00-180.00  154
  2  ω    -55.00 -29.00   0.50   12.00    --   20.00  54.00  30.00   52
  3  ω    -27.00   0.00   0.50   12.00    --   20.00  54.00  30.00   54
  4  ω     69.00 100.00   0.50   12.00    --   20.00  54.00  30.00   62
  5  ω    -72.00 106.00   0.50   12.00    --   20.00  54.00   0.00  356
  6  ω    -67.00 -42.00   0.50   12.00    --   20.00  54.00  90.00   50
  7  ω     12.00  55.00   0.50   12.00    --   20.00  54.00  90.00   86
  8  ω      1.00  26.00   0.50   12.00    --   20.00  54.00-180.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0095712000
_diffrn_orient_matrix_UB_12      -0.0258824000
_diffrn_orient_matrix_UB_13      0.0030054000
_diffrn_orient_matrix_UB_21      -0.0222672000
_diffrn_orient_matrix_UB_22      0.0043354000
_diffrn_orient_matrix_UB_23      0.0219047000
_diffrn_orient_matrix_UB_31      -0.0668983000
_diffrn_orient_matrix_UB_32      0.0022385000
_diffrn_orient_matrix_UB_33      -0.0077072000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4953
_reflns_number_total             7173
_reflns_odcompleteness_completeness 86.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.627
_refine_diff_density_min         -1.467
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7173
_refine_ls_number_restraints     171
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0546
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0601P)²+39.5145P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1461
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O5-H5b \\sim O1-H1a
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C0AA \\sim C18 \\sim C20: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5.a Free rotating group:
 O8(H8c,H8d)
5.b Rotating group:
 O1(H1a), O2(H2a), O3(H3a), O5(H5a)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1c,H1d), C2(H2c,H2d), C3(H3c,H3d), C4(H4c,H4d), C5(H5c,H5d), C6(H6a,H6b),
 C7(H7a,H7b), C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C11(H11a,H11b),
 C12(H12a,H12b), C13(H13a,H13b), C14(H14a,H14b), C15(H15a,H15b), C16(H16a,H16b),
  C17(H17a,H17b), C18(H18a,H18b), C20(H20a,H20b), C21(H21a,H21b), C22(H22a,
 H22b), C23(H23a,H23b), C24(H24a,H24b), C0AA(H0Aa,H0Ab)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.39352(3) 0.74492(2) 0.62579(2) 0.03226(13) Uani 1 1 d . U . . .
P1 P 0.2528(2) 0.87152(7) 0.62899(7) 0.0436(4) Uani 1 1 d . U . . .
P2 P 0.5347(2) 0.61845(7) 0.62576(7) 0.0457(5) Uani 1 1 d . U . . .
O1 O 0.3927(7) 0.7459(2) 0.54769(17) 0.0537(12) Uani 1 1 d D U . . .
H1A H 0.320533 0.731413 0.537167 0.081 Uiso 1 1 d DGR . . . .
O2 O 0.5937(6) 0.7815(2) 0.60158(17) 0.0508(11) Uani 1 1 d . U . . .
H2A H 0.589979 0.786617 0.573736 0.076 Uiso 1 1 d GR . . . .
O3 O 0.5150(6) 0.7686(2) 0.68858(18) 0.0502(12) Uani 1 1 d . U . . .
H3A H 0.575305 0.790375 0.681781 0.075 Uiso 1 1 d GR . . . .
O4 O 0.2726(7) 0.7190(2) 0.68852(19) 0.0495(12) Uani 1 1 d . U . . .
O5 O 0.1902(6) 0.7098(2) 0.60137(18) 0.0511(11) Uani 1 1 d D U . . .
H5A H 0.146404 0.697627 0.623518 0.077 Uiso 1 1 d GR . . . .
O6 O 0.2965(6) 0.81845(18) 0.62745(16) 0.0529(11) Uani 1 1 d . U . . .
O7 O 0.4935(6) 0.67151(18) 0.62658(17) 0.0538(11) Uani 1 1 d . U . . .
N1 N 0.1359(7) 0.8779(3) 0.5930(3) 0.0691(18) Uani 1 1 d . U . . .
N2 N 0.3660(7) 0.9130(2) 0.6164(2) 0.0474(13) Uani 1 1 d . U . . .
N3 N 0.2109(8) 0.8847(2) 0.6799(2) 0.0610(17) Uani 1 1 d . U . . .
N4 N 0.4202(7) 0.5782(2) 0.6120(2) 0.0548(14) Uani 1 1 d . U . . .
N5 N 0.6520(8) 0.6133(3) 0.5894(3) 0.075(2) Uani 1 1 d . U . . .
N6 N 0.5759(8) 0.6017(3) 0.6757(2) 0.0667(18) Uani 1 1 d . U . . .
C1 C 0.4811(10) 0.9221(4) 0.6464(3) 0.077(3) Uani 1 1 d . U . . .
H1C H 0.458084 0.946825 0.668405 0.092 Uiso 1 1 calc R . . . .
H1D H 0.507167 0.891741 0.661302 0.092 Uiso 1 1 calc R . . . .
C2 C 0.5910(12) 0.9402(6) 0.6176(4) 0.121(5) Uani 1 1 d . U . . .
H2C H 0.603873 0.975594 0.621792 0.145 Uiso 1 1 calc R . . . .
H2D H 0.674204 0.923388 0.624925 0.145 Uiso 1 1 calc R . . . .
C3 C 0.5548(14) 0.9302(6) 0.5735(5) 0.129(4) Uani 1 1 d . U . . .
H3C H 0.608869 0.902995 0.562348 0.155 Uiso 1 1 calc R . . . .
H3D H 0.572614 0.959177 0.555471 0.155 Uiso 1 1 calc R . . . .
C4 C 0.4141(11) 0.9172(4) 0.5702(3) 0.079(3) Uani 1 1 d . U . . .
H4C H 0.402945 0.886005 0.554734 0.095 Uiso 1 1 calc R . . . .
H4D H 0.364815 0.942826 0.554600 0.095 Uiso 1 1 calc R . . . .
C5 C 0.0576(13) 0.9243(4) 0.5874(5) 0.117(4) Uani 1 1 d . U . . .
H5C H 0.023816 0.935544 0.615713 0.140 Uiso 1 1 calc R . . . .
H5D H 0.113818 0.950177 0.575024 0.140 Uiso 1 1 calc R . . . .
C6 C -0.0492(13) 0.9137(5) 0.5588(4) 0.117(4) Uani 1 1 d . U . . .
H6A H -0.039059 0.932577 0.531750 0.141 Uiso 1 1 calc R . . . .
H6B H -0.133217 0.923339 0.572545 0.141 Uiso 1 1 calc R . . . .
C7 C -0.0512(13) 0.8612(5) 0.5489(5) 0.124(5) Uani 1 1 d . U . . .
H7A H -0.040874 0.855969 0.517420 0.149 Uiso 1 1 calc R . . . .
H7B H -0.135886 0.846760 0.558113 0.149 Uiso 1 1 calc R . . . .
C8 C 0.0605(10) 0.8378(4) 0.5730(3) 0.076(3) Uani 1 1 d . U . . .
H8A H 0.026617 0.815451 0.595464 0.091 Uiso 1 1 calc R . . . .
H8B H 0.116879 0.819075 0.552866 0.091 Uiso 1 1 calc R . . . .
C9 C 0.1862(15) 0.9352(4) 0.6962(4) 0.116(5) Uani 1 1 d . U . . .
H9A H 0.269257 0.950717 0.705498 0.139 Uiso 1 1 calc R . . . .
H9B H 0.145035 0.955475 0.673464 0.139 Uiso 1 1 calc R . . . .
C10 C 0.0951(14) 0.9286(4) 0.7336(4) 0.120(4) Uani 1 1 d . U . . .
H10A H 0.138590 0.940117 0.760367 0.144 Uiso 1 1 calc R . . . .
H10B H 0.015190 0.948458 0.729047 0.144 Uiso 1 1 calc R . . . .
C11 C 0.0585(11) 0.8788(4) 0.7387(3) 0.084(3) Uani 1 1 d . U . . .
H11A H -0.035845 0.874446 0.731919 0.101 Uiso 1 1 calc R . . . .
H11B H 0.073618 0.868249 0.768958 0.101 Uiso 1 1 calc R . . . .
C12 C 0.1426(10) 0.8484(3) 0.7078(3) 0.063(2) Uani 1 1 d . U . . .
H12A H 0.207004 0.828544 0.724073 0.076 Uiso 1 1 calc R . . . .
H12B H 0.086785 0.826546 0.690229 0.076 Uiso 1 1 calc R . . . .
C13 C 0.7269(11) 0.6547(4) 0.5704(4) 0.086(3) Uani 1 1 d . U . . .
H13A H 0.761067 0.676220 0.593515 0.103 Uiso 1 1 calc R . . . .
H13B H 0.670265 0.674070 0.550908 0.103 Uiso 1 1 calc R . . . .
C14 C 0.8378(14) 0.6318(6) 0.5458(5) 0.137(5) Uani 1 1 d . U . . .
H14A H 0.830530 0.639941 0.514664 0.165 Uiso 1 1 calc R . . . .
H14B H 0.923075 0.644210 0.556564 0.165 Uiso 1 1 calc R . . . .
C15 C 0.8308(15) 0.5787(6) 0.5517(5) 0.141(6) Uani 1 1 d . U . . .
H15A H 0.812920 0.562643 0.523646 0.170 Uiso 1 1 calc R . . . .
H15B H 0.915776 0.566348 0.562875 0.170 Uiso 1 1 calc R . . . .
C16 C 0.7278(14) 0.5677(4) 0.5818(5) 0.127(4) Uani 1 1 d . U . . .
H16A H 0.765467 0.555745 0.609305 0.152 Uiso 1 1 calc R . . . .
H16B H 0.669530 0.542215 0.569818 0.152 Uiso 1 1 calc R . . . .
C17 C 0.6427(11) 0.6365(3) 0.7062(3) 0.071(2) Uani 1 1 d . U . . .
H17A H 0.576836 0.655698 0.722461 0.086 Uiso 1 1 calc R . . . .
H17B H 0.700422 0.659116 0.690112 0.086 Uiso 1 1 calc R . . . .
C18 C 0.7242(14) 0.6046(4) 0.7373(4) 0.113(3) Uani 1 1 d . U . . .
H18A H 0.819488 0.608944 0.731942 0.136 Uiso 1 1 calc R . . . .
H18B H 0.705105 0.613034 0.767767 0.136 Uiso 1 1 calc R . . . .
C20 C 0.6002(15) 0.5506(4) 0.6903(4) 0.117(3) Uani 1 1 d . U . . .
H20A H 0.516651 0.534325 0.698095 0.141 Uiso 1 1 calc R . . . .
H20B H 0.644405 0.531520 0.667400 0.141 Uiso 1 1 calc R . . . .
C21 C 0.3000(9) 0.5722(4) 0.6406(4) 0.071(2) Uani 1 1 d . U . . .
H21A H 0.317801 0.548702 0.664143 0.085 Uiso 1 1 calc R . . . .
H21B H 0.274632 0.603761 0.653640 0.085 Uiso 1 1 calc R . . . .
C22 C 0.1923(12) 0.5536(5) 0.6114(5) 0.107(4) Uani 1 1 d . U . . .
H22A H 0.186320 0.517731 0.613066 0.129 Uiso 1 1 calc R . . . .
H22B H 0.106437 0.567686 0.619761 0.129 Uiso 1 1 calc R . . . .
C23 C 0.2288(14) 0.5691(5) 0.5674(5) 0.127(5) Uani 1 1 d . U . . .
H23A H 0.186774 0.600610 0.560512 0.153 Uiso 1 1 calc R . . . .
H23B H 0.198366 0.544688 0.546039 0.153 Uiso 1 1 calc R . . . .
C24 C 0.3771(12) 0.5740(4) 0.5652(3) 0.097(3) Uani 1 1 d . U . . .
H24A H 0.416988 0.545053 0.551381 0.116 Uiso 1 1 calc R . . . .
H24B H 0.402511 0.603315 0.548644 0.116 Uiso 1 1 calc R . . . .
Cl1 Cl 0.6377(2) 0.79191(11) 0.50012(7) 0.0725(7) Uani 1 1 d . U . . .
Cl2 Cl 0.7777(2) 0.82497(10) 0.67044(8) 0.0743(7) Uani 1 1 d . U . . .
Cl3 Cl 0.0110(2) 0.66237(10) 0.67044(8) 0.0726(7) Uani 1 1 d . U . . .
O8 O 0.3957(8) 0.7438(3) 0.76621(18) 0.0655(18) Uani 1 1 d . U . . .
H8C H 0.369667 0.763494 0.786404 0.098 Uiso 1 1 d G . . . .
H8D H 0.413527 0.716932 0.779681 0.098 Uiso 1 1 d G . . . .
C0AA C 0.6847(16) 0.5557(4) 0.7280(4) 0.132(3) Uani 1 1 d . U . . .
H0AA H 0.637873 0.542507 0.753538 0.159 Uiso 1 1 calc R . . . .
H0AB H 0.764448 0.535669 0.723558 0.159 Uiso 1 1 calc R . . . .
H1B H 0.454(8) 0.755(2) 0.528(3) 0.04(2) Uiso 1 1 d . . . . .
H4A H 0.194(11) 0.702(4) 0.690(3) 0.10(4) Uiso 1 1 d . . . . .
H2B H 0.683(13) 0.789(5) 0.612(4) 0.14(5) Uiso 1 1 d . . . . .
H3B H 0.510(11) 0.761(4) 0.715(4) 0.10(4) Uiso 1 1 d . . . . .
H4B H 0.288(10) 0.732(4) 0.710(3) 0.08(4) Uiso 1 1 d . . . . .
H5B H 0.157(12) 0.712(5) 0.5748(18) 0.16(5) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O1 2.366(5) . ?
Ho1 O2 2.344(5) . ?
Ho1 O3 2.343(5) . ?
Ho1 O4 2.356(5) . ?
Ho1 O5 2.355(5) . ?
Ho1 O6 2.205(5) . ?
Ho1 O7 2.215(5) . ?
P1 O6 1.495(5) . ?
P1 N1 1.605(7) . ?
P1 N2 1.632(7) . ?
P1 N3 1.636(7) . ?
P2 O7 1.487(5) . ?
P2 N4 1.628(7) . ?
P2 N5 1.613(8) . ?
P2 N6 1.630(7) . ?
O1 H1A 0.8784 . ?
O1 H1B 0.88(8) . ?
O2 H2A 0.8552 . ?
O2 H2B 0.96(13) . ?
O3 H3A 0.8646 . ?
O3 H3B 0.83(11) . ?
O4 H4A 0.90(11) . ?
O4 H4B 0.75(10) . ?
O5 H5A 0.8653 . ?
O5 H5B 0.87(2) . ?
N1 C5 1.483(12) . ?
N1 C8 1.449(11) . ?
N2 C1 1.484(11) . ?
N2 C4 1.482(10) . ?
N3 C9 1.466(11) . ?
N3 C12 1.462(10) . ?
N4 C21 1.488(11) . ?
N4 C24 1.485(12) . ?
N5 C13 1.460(11) . ?
N5 C16 1.459(12) . ?
N6 C17 1.475(11) . ?
N6 C20 1.466(11) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.482(14) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.411(16) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C3 C4 1.448(15) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C5 C6 1.401(14) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.447(16) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.472(14) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.464(14) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.399(13) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.498(12) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.470(15) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.444(17) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.404(16) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.511(13) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C0AA 1.404(14) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C0AA 1.425(14) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.478(14) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.443(17) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.485(17) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
O8 H8C 0.8500 . ?
O8 H8D 0.8501 . ?
C0AA H0AA 0.9700 . ?
C0AA H0AB 0.9700 . ?

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 O1 71.7(2) . . ?
O2 Ho1 O4 144.3(2) . . ?
O2 Ho1 O5 143.44(19) . . ?
O3 Ho1 O1 144.1(2) . . ?
O3 Ho1 O2 72.52(19) . . ?
O3 Ho1 O4 71.9(2) . . ?
O3 Ho1 O5 144.0(2) . . ?
O4 Ho1 O1 143.9(2) . . ?
O5 Ho1 O1 71.8(2) . . ?
O5 Ho1 O4 72.2(2) . . ?
O6 Ho1 O1 90.6(2) . . ?
O6 Ho1 O2 90.1(2) . . ?
O6 Ho1 O3 87.9(2) . . ?
O6 Ho1 O4 91.3(2) . . ?
O6 Ho1 O5 89.4(2) . . ?
O6 Ho1 O7 177.94(19) . . ?
O7 Ho1 O1 91.3(2) . . ?
O7 Ho1 O2 89.8(2) . . ?
O7 Ho1 O3 90.1(2) . . ?
O7 Ho1 O4 87.5(2) . . ?
O7 Ho1 O5 91.9(2) . . ?
O6 P1 N1 107.0(4) . . ?
O6 P1 N2 116.5(4) . . ?
O6 P1 N3 108.1(3) . . ?
N1 P1 N2 105.6(4) . . ?
N1 P1 N3 115.6(4) . . ?
N2 P1 N3 104.4(4) . . ?
O7 P2 N4 116.8(4) . . ?
O7 P2 N5 107.1(4) . . ?
O7 P2 N6 108.7(4) . . ?
N4 P2 N6 103.3(4) . . ?
N5 P2 N4 106.0(4) . . ?
N5 P2 N6 115.3(4) . . ?
Ho1 O1 H1A 111.1 . . ?
Ho1 O1 H1B 132(5) . . ?
H1A O1 H1B 116.9 . . ?
Ho1 O2 H2A 109.8 . . ?
Ho1 O2 H2B 140(7) . . ?
H2A O2 H2B 109.6 . . ?
Ho1 O3 H3A 110.5 . . ?
Ho1 O3 H3B 133(8) . . ?
H3A O3 H3B 116.1 . . ?
Ho1 O4 H4A 129(6) . . ?
Ho1 O4 H4B 117(8) . . ?
H4A O4 H4B 111(9) . . ?
Ho1 O5 H5A 110.0 . . ?
Ho1 O5 H5B 126(9) . . ?
H5A O5 H5B 123.2 . . ?
P1 O6 Ho1 170.9(4) . . ?
P2 O7 Ho1 169.2(4) . . ?
C5 N1 P1 123.3(7) . . ?
C8 N1 P1 125.5(6) . . ?
C8 N1 C5 107.9(8) . . ?
C1 N2 P1 120.3(5) . . ?
C4 N2 P1 119.8(6) . . ?
C4 N2 C1 108.3(7) . . ?
C9 N3 P1 124.1(6) . . ?
C12 N3 P1 121.3(6) . . ?
C12 N3 C9 110.3(7) . . ?
C21 N4 P2 119.2(6) . . ?
C24 N4 P2 119.9(6) . . ?
C24 N4 C21 108.4(8) . . ?
C13 N5 P2 125.0(7) . . ?
C16 N5 P2 123.8(7) . . ?
C16 N5 C13 108.4(8) . . ?
C17 N6 P2 121.3(6) . . ?
C20 N6 P2 125.6(7) . . ?
C20 N6 C17 109.4(7) . . ?
N2 C1 H1C 110.6 . . ?
N2 C1 H1D 110.6 . . ?
H1C C1 H1D 108.8 . . ?
C2 C1 N2 105.5(8) . . ?
C2 C1 H1C 110.6 . . ?
C2 C1 H1D 110.6 . . ?
C1 C2 H2C 110.2 . . ?
C1 C2 H2D 110.2 . . ?
H2C C2 H2D 108.5 . . ?
C3 C2 C1 107.7(11) . . ?
C3 C2 H2C 110.2 . . ?
C3 C2 H2D 110.2 . . ?
C2 C3 H3C 109.4 . . ?
C2 C3 H3D 109.4 . . ?
C2 C3 C4 111.0(11) . . ?
H3C C3 H3D 108.0 . . ?
C4 C3 H3C 109.4 . . ?
C4 C3 H3D 109.4 . . ?
N2 C4 H4C 110.6 . . ?
N2 C4 H4D 110.6 . . ?
C3 C4 N2 105.5(9) . . ?
C3 C4 H4C 110.6 . . ?
C3 C4 H4D 110.6 . . ?
H4C C4 H4D 108.8 . . ?
N1 C5 H5C 110.2 . . ?
N1 C5 H5D 110.2 . . ?
H5C C5 H5D 108.5 . . ?
C6 C5 N1 107.4(10) . . ?
C6 C5 H5C 110.2 . . ?
C6 C5 H5D 110.2 . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
C5 C6 C7 109.7(10) . . ?
H6A C6 H6B 108.2 . . ?
C7 C6 H6A 109.7 . . ?
C7 C6 H6B 109.7 . . ?
C6 C7 H7A 110.2 . . ?
C6 C7 H7B 110.2 . . ?
C6 C7 C8 107.8(10) . . ?
H7A C7 H7B 108.5 . . ?
C8 C7 H7A 110.2 . . ?
C8 C7 H7B 110.2 . . ?
N1 C8 C7 106.3(9) . . ?
N1 C8 H8A 110.5 . . ?
N1 C8 H8B 110.5 . . ?
C7 C8 H8A 110.5 . . ?
C7 C8 H8B 110.5 . . ?
H8A C8 H8B 108.7 . . ?
N3 C9 H9A 110.8 . . ?
N3 C9 H9B 110.8 . . ?
H9A C9 H9B 108.9 . . ?
C10 C9 N3 104.6(8) . . ?
C10 C9 H9A 110.8 . . ?
C10 C9 H9B 110.8 . . ?
C9 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C11 C10 C9 111.3(9) . . ?
C11 C10 H10A 109.4 . . ?
C11 C10 H10B 109.4 . . ?
C10 C11 H11A 110.1 . . ?
C10 C11 H11B 110.1 . . ?
C10 C11 C12 108.0(8) . . ?
H11A C11 H11B 108.4 . . ?
C12 C11 H11A 110.1 . . ?
C12 C11 H11B 110.1 . . ?
N3 C12 C11 104.9(7) . . ?
N3 C12 H12A 110.8 . . ?
N3 C12 H12B 110.8 . . ?
C11 C12 H12A 110.8 . . ?
C11 C12 H12B 110.8 . . ?
H12A C12 H12B 108.8 . . ?
N5 C13 H13A 110.7 . . ?
N5 C13 H13B 110.7 . . ?
N5 C13 C14 105.3(10) . . ?
H13A C13 H13B 108.8 . . ?
C14 C13 H13A 110.7 . . ?
C14 C13 H13B 110.7 . . ?
C13 C14 H14A 110.0 . . ?
C13 C14 H14B 110.0 . . ?
H14A C14 H14B 108.4 . . ?
C15 C14 C13 108.4(11) . . ?
C15 C14 H14A 110.0 . . ?
C15 C14 H14B 110.0 . . ?
C14 C15 H15A 109.9 . . ?
C14 C15 H15B 109.9 . . ?
H15A C15 H15B 108.3 . . ?
C16 C15 C14 108.9(11) . . ?
C16 C15 H15A 109.9 . . ?
C16 C15 H15B 109.9 . . ?
N5 C16 H16A 110.2 . . ?
N5 C16 H16B 110.2 . . ?
C15 C16 N5 107.7(11) . . ?
C15 C16 H16A 110.2 . . ?
C15 C16 H16B 110.2 . . ?
H16A C16 H16B 108.5 . . ?
N6 C17 H17A 110.6 . . ?
N6 C17 H17B 110.6 . . ?
N6 C17 C18 105.8(8) . . ?
H17A C17 H17B 108.7 . . ?
C18 C17 H17A 110.6 . . ?
C18 C17 H17B 110.6 . . ?
C17 C18 H18A 110.8 . . ?
C17 C18 H18B 110.8 . . ?
H18A C18 H18B 108.8 . . ?
C0AA C18 C17 105.0(9) . . ?
C0AA C18 H18A 110.8 . . ?
C0AA C18 H18B 110.8 . . ?
N6 C20 H20A 110.9 . . ?
N6 C20 H20B 110.9 . . ?
H20A C20 H20B 108.9 . . ?
C0AA C20 N6 104.5(9) . . ?
C0AA C20 H20A 110.9 . . ?
C0AA C20 H20B 110.9 . . ?
N4 C21 H21A 110.6 . . ?
N4 C21 H21B 110.6 . . ?
H21A C21 H21B 108.7 . . ?
C22 C21 N4 105.8(9) . . ?
C22 C21 H21A 110.6 . . ?
C22 C21 H21B 110.6 . . ?
C21 C22 H22A 110.6 . . ?
C21 C22 H22B 110.6 . . ?
H22A C22 H22B 108.7 . . ?
C23 C22 C21 105.8(10) . . ?
C23 C22 H22A 110.6 . . ?
C23 C22 H22B 110.6 . . ?
C22 C23 H23A 110.0 . . ?
C22 C23 H23B 110.0 . . ?
C22 C23 C24 108.5(11) . . ?
H23A C23 H23B 108.4 . . ?
C24 C23 H23A 110.0 . . ?
C24 C23 H23B 110.0 . . ?
N4 C24 C23 104.6(10) . . ?
N4 C24 H24A 110.8 . . ?
N4 C24 H24B 110.8 . . ?
C23 C24 H24A 110.8 . . ?
C23 C24 H24B 110.8 . . ?
H24A C24 H24B 108.9 . . ?
H8C O8 H8D 104.4 . . ?
C18 C0AA C20 114.6(10) . . ?
C18 C0AA H0AA 108.6 . . ?
C18 C0AA H0AB 108.6 . . ?
C20 C0AA H0AA 108.6 . . ?
C20 C0AA H0AB 108.6 . . ?
H0AA C0AA H0AB 107.6 . . ?

_olex2_exptl_crystal_mounting_method 293
_olex2_submission_original_sample_id Ho-Cl
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.524
_oxdiff_exptl_absorpt_empirical_full_min 0.786
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 2059755'
_audit_update_record             
;
2021-01-29 deposited with the CCDC.	2021-03-03 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         'C24 H60 Br3 Ho N6 O8 P2'
_chemical_formula_sum            'C24 H60 Br3 Ho N6 O8 P2'
_chemical_formula_weight         1027.38

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'
Br Br -0.2901 2.4595 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.0871(3)
_cell_length_b                   26.8701(8)
_cell_length_c                   30.9089(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8377.6(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8028
_cell_measurement_theta_min      2.2400
_cell_measurement_theta_max      23.2320

_exptl_crystal_description       block
_exptl_crystal_colour            pinkish
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_F_000             4096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    4.871
_shelx_estimated_absorpt_T_min   0.246
_shelx_estimated_absorpt_T_max   0.909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.56647
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34768
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.009
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7375
_reflns_number_gt                4866
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0378P)²+9.3087P] 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         7375
_refine_ls_number_parameters     412
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.0929
_refine_ls_wR_factor_gt          0.0816
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.60396(3) 0.73829(2) 0.37349(2) 0.03611(9) Uani 1 1 d . . . . .
P1 P 0.73833(17) 0.86562(6) 0.36946(5) 0.0451(4) Uani 1 1 d . . . . .
P2 P 0.46873(18) 0.61132(6) 0.37751(6) 0.0514(4) Uani 1 1 d . . . . .
O1 O 0.6959(4) 0.81222(14) 0.37118(12) 0.0503(11) Uani 1 1 d . . . . .
O2 O 0.5091(4) 0.66466(14) 0.37469(12) 0.0526(11) Uani 1 1 d . . . . .
O3 O 0.4061(5) 0.7738(2) 0.39781(18) 0.0633(15) Uani 1 1 d . . . . .
O4 O 0.4792(4) 0.75945(15) 0.31203(12) 0.0562(12) Uani 1 1 d . . . . .
H4A H 0.529026 0.776340 0.293514 0.084 Uiso 1 1 d R U . . .
H4B H 0.415234 0.781287 0.318143 0.084 Uiso 1 1 d R U . . .
O5 O 0.7214(4) 0.71070(16) 0.31222(11) 0.0557(12) Uani 1 1 d . . . . .
H5A H 0.805162 0.716523 0.315478 0.084 Uiso 1 1 d R U . . .
H5B H 0.699897 0.728709 0.290079 0.084 Uiso 1 1 d R U . . .
O6 O 0.8052(4) 0.70366(16) 0.39746(12) 0.0584(12) Uani 1 1 d . . . . .
H6A H 0.836773 0.721251 0.417917 0.088 Uiso 1 1 d R U . . .
H6B H 0.862610 0.706097 0.377252 0.088 Uiso 1 1 d R U . . .
O7 O 0.6077(4) 0.74186(16) 0.45016(12) 0.0603(12) Uani 1 1 d . . . . .
H7A H 0.673423 0.725201 0.459577 0.090 Uiso 1 1 d R U . . .
H7B H 0.540073 0.726608 0.460027 0.090 Uiso 1 1 d R U . . .
N1 N 0.8547(6) 0.8725(2) 0.40476(19) 0.0676(17) Uani 1 1 d . . . . .
N2 N 0.6273(5) 0.90712(18) 0.38228(15) 0.0490(14) Uani 1 1 d . . . . .
N3 N 0.7787(6) 0.87895(18) 0.31972(16) 0.0583(15) Uani 1 1 d . . . . .
N4 N 0.3529(6) 0.6079(2) 0.4133(2) 0.083(2) Uani 1 1 d . . . . .
N5 N 0.4278(7) 0.5926(2) 0.3295(2) 0.089(2) Uani 1 1 d . U . . .
N6 N 0.5826(6) 0.57198(19) 0.39287(19) 0.0608(15) Uani 1 1 d . . . . .
C1 C 0.3717(8) 0.6253(3) 0.2969(2) 0.081(2) Uani 1 1 d . . . . .
H1A H 0.441383 0.642508 0.281302 0.097 Uiso 1 1 calc R U . . .
H1B H 0.313954 0.649826 0.310178 0.097 Uiso 1 1 calc R U . . .
C2 C 0.2945(10) 0.5919(3) 0.2670(3) 0.109(3) Uani 1 1 d . U . . .
H2A H 0.199918 0.596381 0.271211 0.130 Uiso 1 1 calc R U . . .
H2B H 0.315914 0.599014 0.237076 0.130 Uiso 1 1 calc R U . . .
C3 C 0.3322(12) 0.5436(4) 0.2779(3) 0.149(3) Uani 1 1 d . U . . .
H3C H 0.387840 0.530313 0.255016 0.178 Uiso 1 1 calc R U . . .
H3D H 0.253584 0.522870 0.279704 0.178 Uiso 1 1 calc R U . . .
C4 C 0.4020(11) 0.5409(3) 0.3177(3) 0.137(3) Uani 1 1 d . U . . .
H4C H 0.484415 0.522705 0.314235 0.164 Uiso 1 1 calc R U . . .
H4D H 0.348829 0.524519 0.339643 0.164 Uiso 1 1 calc R U . . .
C5 C 0.6985(8) 0.5641(3) 0.3648(3) 0.090(3) Uani 1 1 d . . . . .
H5C H 0.680306 0.538611 0.343407 0.108 Uiso 1 1 calc R U . . .
H5D H 0.722532 0.594623 0.350072 0.108 Uiso 1 1 calc R U . . .
C6 C 0.8046(10) 0.5482(4) 0.3941(4) 0.136(4) Uani 1 1 d . U . . .
H6C H 0.816688 0.512455 0.392134 0.163 Uiso 1 1 calc R U . . .
H6D H 0.887274 0.564194 0.386077 0.163 Uiso 1 1 calc R U . . .
C7 C 0.7694(13) 0.5615(5) 0.4366(4) 0.161(5) Uani 1 1 d . U . . .
H7C H 0.816257 0.591548 0.444978 0.193 Uiso 1 1 calc R U . . .
H7D H 0.793961 0.535149 0.456404 0.193 Uiso 1 1 calc R U . . .
C8 C 0.6247(11) 0.5702(4) 0.4386(3) 0.121(4) Uani 1 1 d . . . . .
H8A H 0.580571 0.543246 0.453760 0.145 Uiso 1 1 calc R U . . .
H8B H 0.604962 0.601270 0.453121 0.145 Uiso 1 1 calc R U . . .
C9 C 0.2816(12) 0.5619(4) 0.4238(4) 0.165(5) Uani 1 1 d . U . . .
H9A H 0.251539 0.545863 0.397474 0.198 Uiso 1 1 calc R U . . .
H9B H 0.340117 0.539126 0.438940 0.198 Uiso 1 1 calc R U . . .
C10 C 0.1739(12) 0.5736(5) 0.4498(4) 0.150(5) Uani 1 1 d . . . . .
H10A H 0.182460 0.557178 0.477554 0.179 Uiso 1 1 calc R U . . .
H10B H 0.092774 0.562194 0.436187 0.179 Uiso 1 1 calc R U . . .
C11 C 0.1687(11) 0.6266(5) 0.4558(4) 0.138(4) Uani 1 1 d . . . . .
H11A H 0.180749 0.634633 0.486162 0.165 Uiso 1 1 calc R U . . .
H11B H 0.083159 0.639257 0.446647 0.165 Uiso 1 1 calc R U . . .
C12 C 0.2774(8) 0.6497(3) 0.4293(3) 0.093(3) Uani 1 1 d . . . . .
H12A H 0.240852 0.668946 0.405566 0.112 Uiso 1 1 calc R U . . .
H12B H 0.332292 0.671243 0.446955 0.112 Uiso 1 1 calc R U . . .
C13 C 0.9247(8) 0.8324(3) 0.4266(2) 0.082(2) Uani 1 1 d . . . . .
H13A H 0.960281 0.808795 0.405883 0.098 Uiso 1 1 calc R U . . .
H13B H 0.866181 0.814839 0.446334 0.098 Uiso 1 1 calc R U . . .
C14 C 1.0339(9) 0.8577(4) 0.4508(3) 0.118(4) Uani 1 1 d . . . . .
H14A H 1.018833 0.855032 0.481749 0.141 Uiso 1 1 calc R U . . .
H14B H 1.118285 0.842114 0.444159 0.141 Uiso 1 1 calc R U . . .
C15 C 1.0358(10) 0.9087(4) 0.4381(3) 0.122(4) Uani 1 1 d . . . . .
H15A H 1.025008 0.929762 0.463352 0.146 Uiso 1 1 calc R U . . .
H15B H 1.120395 0.916558 0.424834 0.146 Uiso 1 1 calc R U . . .
C16 C 0.9321(10) 0.9180(4) 0.4084(3) 0.131(4) Uani 1 1 d . U . . .
H16A H 0.968304 0.927134 0.380379 0.157 Uiso 1 1 calc R U . . .
H16B H 0.876769 0.945074 0.418587 0.157 Uiso 1 1 calc R U . . .
C17 C 0.8021(11) 0.9291(3) 0.3029(3) 0.125(4) Uani 1 1 d . . . . .
H17A H 0.719353 0.944794 0.294565 0.150 Uiso 1 1 calc R U . . .
H17B H 0.845407 0.949745 0.324482 0.150 Uiso 1 1 calc R U . . .
C18 C 0.8858(12) 0.9222(4) 0.2662(3) 0.143(4) Uani 1 1 d . U . . .
H18A H 0.838781 0.932688 0.240419 0.172 Uiso 1 1 calc R U . . .
H18B H 0.963579 0.943182 0.269241 0.172 Uiso 1 1 calc R U . . .
C19 C 0.9261(9) 0.8729(3) 0.2612(2) 0.088(3) Uani 1 1 d . . . . .
H19A H 1.019535 0.869448 0.268034 0.106 Uiso 1 1 calc R U . . .
H19B H 0.911759 0.861925 0.231697 0.106 Uiso 1 1 calc R U . . .
C20 C 0.8435(7) 0.8429(3) 0.2920(2) 0.067(2) Uani 1 1 d . . . . .
H20A H 0.778507 0.823204 0.276430 0.080 Uiso 1 1 calc R U . . .
H20B H 0.898858 0.820653 0.308931 0.080 Uiso 1 1 calc R U . . .
C21 C 0.5806(8) 0.9115(3) 0.4272(2) 0.080(2) Uani 1 1 d . . . . .
H21A H 0.586210 0.879733 0.441951 0.096 Uiso 1 1 calc R U . . .
H21B H 0.633181 0.935721 0.442985 0.096 Uiso 1 1 calc R U . . .
C22 C 0.4423(12) 0.9280(5) 0.4238(4) 0.157(5) Uani 1 1 d . . . . .
H22A H 0.384285 0.902702 0.435809 0.189 Uiso 1 1 calc R U . . .
H22B H 0.430146 0.958328 0.440338 0.189 Uiso 1 1 calc R U . . .
C23 C 0.4092(10) 0.9365(5) 0.3807(4) 0.140(5) Uani 1 1 d . . . . .
H23A H 0.399296 0.971891 0.375537 0.168 Uiso 1 1 calc R U . . .
H23B H 0.325775 0.920301 0.373868 0.168 Uiso 1 1 calc R U . . .
C24 C 0.5134(8) 0.9167(3) 0.3536(3) 0.085(2) Uani 1 1 d . . . . .
H24A H 0.537276 0.940464 0.331342 0.102 Uiso 1 1 calc R U . . .
H24B H 0.484771 0.886106 0.339841 0.102 Uiso 1 1 calc R U . . .
Br1 Br 0.99288(8) 0.64961(3) 0.32937(2) 0.0809(3) Uani 1 1 d . . . . .
Br2 Br 0.86765(7) 0.70137(3) 0.50052(2) 0.0721(2) Uani 1 1 d . . . . .
Br3 Br 0.20671(8) 0.82039(4) 0.33006(2) 0.0851(3) Uani 1 1 d . . . . .
O8 O 0.5994(6) 0.7354(2) 0.23669(13) 0.0782(15) Uani 1 1 d G . . . .
H8C H 0.636274 0.754971 0.218829 0.117 Uiso 1 1 d G U . . .
H8D H 0.578590 0.710033 0.221856 0.117 Uiso 1 1 d G U . . .
H3A H 0.391(7) 0.783(3) 0.423(2) 0.08(3) Uiso 1 1 d . . . . .
H3B H 0.361(7) 0.787(3) 0.382(2) 0.08(3) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O1 2.193(4) . ?
Ho1 O2 2.198(4) . ?
Ho1 O3 2.336(5) . ?
Ho1 O4 2.348(4) . ?
Ho1 O6 2.353(4) . ?
Ho1 O5 2.354(4) . ?
Ho1 O7 2.372(4) . ?
P1 O1 1.498(4) . ?
P1 N1 1.613(5) . ?
P1 N2 1.629(5) . ?
P1 N3 1.630(5) . ?
P2 O2 1.492(4) . ?
P2 N4 1.610(6) . ?
P2 N5 1.620(6) . ?
P2 N6 1.631(6) . ?
O3 H3A 0.84(7) . ?
O3 H3B 0.75(7) . ?
O4 H4A 0.8868 . ?
O4 H4B 0.8922 . ?
O5 H5A 0.8648 . ?
O5 H5B 0.8658 . ?
O6 H6A 0.8512 . ?
O6 H6B 0.8539 . ?
O7 H7A 0.8516 . ?
O7 H7B 0.8519 . ?
N1 C13 1.455(8) . ?
N1 C16 1.456(9) . ?
N2 C21 1.471(8) . ?
N2 C24 1.472(8) . ?
N3 C20 1.449(7) . ?
N3 C17 1.465(8) . ?
N4 C12 1.444(8) . ?
N4 C9 1.468(10) . ?
N5 C1 1.452(9) . ?
N5 C4 1.459(10) . ?
N6 C5 1.470(8) . ?
N6 C8 1.476(9) . ?
C1 C2 1.507(10) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.393(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.421(11) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.465(11) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 C7 1.407(13) . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.480(13) . ?
C7 H7C 0.9700 . ?
C7 H7D 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.387(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.435(13) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.504(11) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.495(10) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.427(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.415(11) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.426(10) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.395(10) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.501(9) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.467(11) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.394(12) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.444(11) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
O8 H8C 0.8485 . ?
O8 H8D 0.8477 . ?

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
O1 Ho1 O2 178.80(15) . . ?
O1 Ho1 O3 90.12(17) . . ?
O2 Ho1 O3 89.41(17) . . ?
O1 Ho1 O4 88.92(14) . . ?
O2 Ho1 O4 89.89(15) . . ?
O3 Ho1 O4 72.77(17) . . ?
O1 Ho1 O6 90.21(15) . . ?
O2 Ho1 O6 90.83(15) . . ?
O3 Ho1 O6 142.86(17) . . ?
O4 Ho1 O6 144.37(14) . . ?
O1 Ho1 O5 92.66(14) . . ?
O2 Ho1 O5 87.10(14) . . ?
O3 Ho1 O5 144.85(17) . . ?
O4 Ho1 O5 72.26(14) . . ?
O6 Ho1 O5 72.20(14) . . ?
O1 Ho1 O7 89.38(14) . . ?
O2 Ho1 O7 91.51(15) . . ?
O3 Ho1 O7 71.06(17) . . ?
O4 Ho1 O7 143.77(14) . . ?
O6 Ho1 O7 71.81(14) . . ?
O5 Ho1 O7 143.96(14) . . ?
O1 P1 N1 107.0(3) . . ?
O1 P1 N2 116.8(3) . . ?
N1 P1 N2 104.9(3) . . ?
O1 P1 N3 108.4(2) . . ?
N1 P1 N3 115.5(3) . . ?
N2 P1 N3 104.5(3) . . ?
O2 P2 N4 107.0(3) . . ?
O2 P2 N5 108.4(3) . . ?
N4 P2 N5 115.2(4) . . ?
O2 P2 N6 116.6(3) . . ?
N4 P2 N6 105.9(3) . . ?
N5 P2 N6 104.1(3) . . ?
P1 O1 Ho1 171.6(3) . . ?
P2 O2 Ho1 169.8(3) . . ?
Ho1 O3 H3A 126(5) . . ?
Ho1 O3 H3B 119(6) . . ?
H3A O3 H3B 111(7) . . ?
Ho1 O4 H4A 110.0 . . ?
Ho1 O4 H4B 112.1 . . ?
H4A O4 H4B 102.1 . . ?
Ho1 O5 H5A 109.9 . . ?
Ho1 O5 H5B 109.5 . . ?
H5A O5 H5B 103.6 . . ?
Ho1 O6 H6A 109.7 . . ?
Ho1 O6 H6B 108.9 . . ?
H6A O6 H6B 104.3 . . ?
Ho1 O7 H7A 109.4 . . ?
Ho1 O7 H7B 109.0 . . ?
H7A O7 H7B 104.4 . . ?
C13 N1 C16 109.1(6) . . ?
C13 N1 P1 125.7(5) . . ?
C16 N1 P1 122.5(5) . . ?
C21 N2 C24 107.7(6) . . ?
C21 N2 P1 120.3(5) . . ?
C24 N2 P1 120.6(5) . . ?
C20 N3 C17 109.5(5) . . ?
C20 N3 P1 121.5(4) . . ?
C17 N3 P1 125.2(5) . . ?
C12 N4 C9 108.7(7) . . ?
C12 N4 P2 125.1(5) . . ?
C9 N4 P2 123.7(6) . . ?
C1 N5 C4 109.5(6) . . ?
C1 N5 P2 123.1(5) . . ?
C4 N5 P2 124.8(6) . . ?
C5 N6 C8 109.3(7) . . ?
C5 N6 P2 118.8(5) . . ?
C8 N6 P2 120.2(5) . . ?
N5 C1 C2 105.4(6) . . ?
N5 C1 H1A 110.7 . . ?
C2 C1 H1A 110.7 . . ?
N5 C1 H1B 110.7 . . ?
C2 C1 H1B 110.7 . . ?
H1A C1 H1B 108.8 . . ?
C3 C2 C1 105.5(8) . . ?
C3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
C3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.8 . . ?
C2 C3 C4 113.0(9) . . ?
C2 C3 H3C 109.0 . . ?
C4 C3 H3C 109.0 . . ?
C2 C3 H3D 109.0 . . ?
C4 C3 H3D 109.0 . . ?
H3C C3 H3D 107.8 . . ?
C3 C4 N5 104.9(8) . . ?
C3 C4 H4C 110.8 . . ?
N5 C4 H4C 110.8 . . ?
C3 C4 H4D 110.8 . . ?
N5 C4 H4D 110.8 . . ?
H4C C4 H4D 108.8 . . ?
C6 C5 N6 105.1(8) . . ?
C6 C5 H5C 110.7 . . ?
N6 C5 H5C 110.7 . . ?
C6 C5 H5D 110.7 . . ?
N6 C5 H5D 110.7 . . ?
H5C C5 H5D 108.8 . . ?
C7 C6 C5 108.5(10) . . ?
C7 C6 H6C 110.0 . . ?
C5 C6 H6C 110.0 . . ?
C7 C6 H6D 110.0 . . ?
C5 C6 H6D 110.0 . . ?
H6C C6 H6D 108.4 . . ?
C6 C7 C8 109.2(10) . . ?
C6 C7 H7C 109.8 . . ?
C8 C7 H7C 109.8 . . ?
C6 C7 H7D 109.8 . . ?
C8 C7 H7D 109.8 . . ?
H7C C7 H7D 108.3 . . ?
N6 C8 C7 104.4(9) . . ?
N6 C8 H8A 110.9 . . ?
C7 C8 H8A 110.9 . . ?
N6 C8 H8B 110.9 . . ?
C7 C8 H8B 110.9 . . ?
H8A C8 H8B 108.9 . . ?
C10 C9 N4 108.7(9) . . ?
C10 C9 H9A 109.9 . . ?
N4 C9 H9A 109.9 . . ?
C10 C9 H9B 109.9 . . ?
N4 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
C9 C10 C11 109.3(10) . . ?
C9 C10 H10A 109.8 . . ?
C11 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
C11 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
C10 C11 C12 108.1(8) . . ?
C10 C11 H11A 110.1 . . ?
C12 C11 H11A 110.1 . . ?
C10 C11 H11B 110.1 . . ?
C12 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
N4 C12 C11 104.5(7) . . ?
N4 C12 H12A 110.8 . . ?
C11 C12 H12A 110.8 . . ?
N4 C12 H12B 110.8 . . ?
C11 C12 H12B 110.8 . . ?
H12A C12 H12B 108.9 . . ?
N1 C13 C14 104.7(7) . . ?
N1 C13 H13A 110.8 . . ?
C14 C13 H13A 110.8 . . ?
N1 C13 H13B 110.8 . . ?
C14 C13 H13B 110.8 . . ?
H13A C13 H13B 108.9 . . ?
C15 C14 C13 108.0(7) . . ?
C15 C14 H14A 110.1 . . ?
C13 C14 H14A 110.1 . . ?
C15 C14 H14B 110.1 . . ?
C13 C14 H14B 110.1 . . ?
H14A C14 H14B 108.4 . . ?
C16 C15 C14 109.8(8) . . ?
C16 C15 H15A 109.7 . . ?
C14 C15 H15A 109.7 . . ?
C16 C15 H15B 109.7 . . ?
C14 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C15 C16 N1 107.3(8) . . ?
C15 C16 H16A 110.3 . . ?
N1 C16 H16A 110.3 . . ?
C15 C16 H16B 110.3 . . ?
N1 C16 H16B 110.3 . . ?
H16A C16 H16B 108.5 . . ?
C18 C17 N3 104.9(7) . . ?
C18 C17 H17A 110.8 . . ?
N3 C17 H17A 110.8 . . ?
C18 C17 H17B 110.8 . . ?
N3 C17 H17B 110.8 . . ?
H17A C17 H17B 108.8 . . ?
C19 C18 C17 112.6(8) . . ?
C19 C18 H18A 109.1 . . ?
C17 C18 H18A 109.1 . . ?
C19 C18 H18B 109.1 . . ?
C17 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
C18 C19 C20 106.2(7) . . ?
C18 C19 H19A 110.5 . . ?
C20 C19 H19A 110.5 . . ?
C18 C19 H19B 110.5 . . ?
C20 C19 H19B 110.5 . . ?
H19A C19 H19B 108.7 . . ?
N3 C20 C19 105.4(6) . . ?
N3 C20 H20A 110.7 . . ?
C19 C20 H20A 110.7 . . ?
N3 C20 H20B 110.7 . . ?
C19 C20 H20B 110.7 . . ?
H20A C20 H20B 108.8 . . ?
C22 C21 N2 105.1(7) . . ?
C22 C21 H21A 110.7 . . ?
N2 C21 H21A 110.7 . . ?
C22 C21 H21B 110.7 . . ?
N2 C21 H21B 110.7 . . ?
H21A C21 H21B 108.8 . . ?
C23 C22 C21 110.2(9) . . ?
C23 C22 H22A 109.6 . . ?
C21 C22 H22A 109.6 . . ?
C23 C22 H22B 109.6 . . ?
C21 C22 H22B 109.6 . . ?
H22A C22 H22B 108.1 . . ?
C22 C23 C24 108.6(9) . . ?
C22 C23 H23A 110.0 . . ?
C24 C23 H23A 110.0 . . ?
C22 C23 H23B 110.0 . . ?
C24 C23 H23B 110.0 . . ?
H23A C23 H23B 108.4 . . ?
C23 C24 N2 106.5(7) . . ?
C23 C24 H24A 110.4 . . ?
N2 C24 H24A 110.4 . . ?
C23 C24 H24B 110.4 . . ?
N2 C24 H24B 110.4 . . ?
H24A C24 H24B 108.6 . . ?
H8C O8 H8D 104.8 . . ?

_refine_diff_density_max         0.755
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.105

