# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_mo_D8V4611_0m_d_AL_DSR
_database_code_depnum_ccdc_archive 'CCDC 2281329'
loop_
_audit_author_name
_audit_author_address
'Jesper Bendix'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2023-07-13 deposited with the CCDC.	2023-10-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H24 N4 O8 Yb, 3(C4 H12 N), 2(Cl), 6(H2 O)'
_chemical_formula_sum            'C28 H72 Cl2 N7 O14 Yb'
_chemical_formula_weight         974.87

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'
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'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -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, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   17.3928(6)
_cell_length_b                   17.3928(6)
_cell_length_c                   6.7688(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2047.63(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9905
_cell_measurement_theta_max      32.99
_cell_measurement_theta_min      2.34
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.482
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.5748
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0956 before and 0.0736 after correction.
The Ratio of minimum to maximum transmission is 0.7698.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             1010
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_description       needle
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41527
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.342
_diffrn_reflns_theta_max         27.085
_diffrn_reflns_theta_full        25.242
_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 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2374
_reflns_number_gt                2055
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0124P)²+1.1000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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_abs_structure_details 
;
 Refined as an inversion twin.
;

_refine_ls_abs_structure_Flack   0.369(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2374
_refine_ls_number_parameters     148
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0150
_refine_ls_wR_factor_ref         0.0344
_refine_ls_wR_factor_gt          0.0328
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.000000 0.000000 0.84610(6) 0.00658(6) Uani 1 4 d S T P . .
Cl1 Cl -0.16315(6) 0.33685(6) 1.09823(19) 0.0230(3) Uani 1 2 d S T P . .
O1 O 0.05205(13) 0.10281(13) 0.6878(3) 0.0099(4) Uani 1 1 d . . . . .
O2 O 0.03284(14) 0.22622(13) 0.6119(4) 0.0164(5) Uani 1 1 d . . . . .
N1 N 0.00490(17) 0.11801(15) 1.0618(3) 0.0094(5) Uani 1 1 d . . . . .
C1 C 0.0275(2) 0.1704(2) 0.7249(5) 0.0105(8) Uani 1 1 d . . . . .
C2 C -0.0100(2) 0.1826(2) 0.9252(6) 0.0115(8) Uani 1 1 d . . . . .
H2A H 0.009910 0.230703 0.984329 0.014 Uiso 1 1 calc R U . . .
H2B H -0.066160 0.188481 0.907228 0.014 Uiso 1 1 calc R U . . .
C3 C 0.08328(19) 0.12861(19) 1.1481(5) 0.0112(6) Uani 1 1 d . . . . .
H3A H 0.080422 0.165546 1.259199 0.013 Uiso 1 1 calc R U . . .
H3B H 0.117942 0.150446 1.046614 0.013 Uiso 1 1 calc R U . . .
C4 C 0.11601(19) 0.05324(19) 1.2216(4) 0.0108(7) Uani 1 1 d . . . . .
H4A H 0.168756 0.061761 1.272090 0.013 Uiso 1 1 calc R U . . .
H4B H 0.084134 0.033871 1.332118 0.013 Uiso 1 1 calc R U . . .
N1_1 N 0.24940(16) 0.25060(16) 0.5937(5) 0.0135(8) Uani 1 2 d DS T P . .
C1_1 C 0.2165(2) 0.2835(2) 0.7800(7) 0.0190(12) Uani 1 2 d DS T P . .
H1A_1 H 0.229561 0.338201 0.788805 0.029 Uiso 0.5 1 calc R U P . .
H1B_1 H 0.237959 0.256254 0.894137 0.029 Uiso 0.5 2 calc R U P . .
H1C_1 H 0.160475 0.277550 0.778969 0.029 Uiso 0.5 1 calc R U P . .
C2_1 C 0.23601(19) 0.16575(19) 0.5880(5) 0.0169(7) Uani 1 1 d D . . . .
H2A_1 H 0.257785 0.144530 0.466119 0.025 Uiso 1 1 calc R U . . .
H2B_1 H 0.180640 0.155428 0.591896 0.025 Uiso 1 1 calc R U . . .
H2C_1 H 0.260828 0.141650 0.702302 0.025 Uiso 1 1 calc R U . . .
C3_1 C 0.2122(2) 0.2878(2) 0.4198(7) 0.0201(12) Uani 1 2 d DS T P . .
H3A_1 H 0.229351 0.262398 0.298362 0.030 Uiso 0.5 1 calc R U P . .
H3B_1 H 0.226491 0.342303 0.415357 0.030 Uiso 0.5 1 calc R U P . .
H3C_1 H 0.156183 0.283274 0.431301 0.030 Uiso 0.5 1 calc R U P . .
N1_2 N 0.000000 0.500000 0.7862(10) 0.0288(18) Uani 1 4 d DS T P . .
C1_2 C 0.000000 0.500000 1.0096(14) 0.053(3) Uani 1 4 d DS T P A .
H1A_2 H 0.053122 0.500253 1.057812 0.080 Uiso 0.25 1 calc R U P . .
H1B_2 H -0.026342 0.453868 1.057811 0.080 Uiso 0.25 1 calc R U P . .
H1C_2 H -0.026780 0.545879 1.057812 0.080 Uiso 0.25 1 calc R U P . .
C2_2 C 0.0768(7) 0.5200(8) 0.726(2) 0.089(6) Uani 0.5 1 d D . P A -1
H2A_2 H 0.113333 0.482925 0.780905 0.134 Uiso 0.5 1 calc R U P A -1
H2B_2 H 0.089304 0.571695 0.773397 0.134 Uiso 0.5 1 calc R U P A -1
H2C_2 H 0.080016 0.519031 0.581001 0.134 Uiso 0.5 1 calc R U P A -1
C3_2 C -0.062(3) 0.551(3) 0.697(3) 0.072(12) Uani 0.25 1 d D . P A -1
H3A_2 H -0.111304 0.539619 0.759645 0.108 Uiso 0.25 1 calc R U P A -1
H3B_2 H -0.065358 0.541085 0.554838 0.108 Uiso 0.25 1 calc R U P A -1
H3C_2 H -0.048531 0.605030 0.719251 0.108 Uiso 0.25 1 calc R U P A -1
O3 O 0.1321(2) 0.3679(2) 1.0846(8) 0.0532(13) Uani 1 2 d DS T P . .
H31 H 0.088(2) 0.355(2) 1.150(7) 0.080 Uiso 1 1 d D U . . .
O4 O 0.00202(18) 0.32851(17) 1.2998(4) 0.0338(8) Uani 1 1 d G . . . .
H41 H -0.043194 0.333628 1.253094 0.051 Uiso 1 1 d G U . . .
H42 H 0.002479 0.292755 1.384286 0.051 Uiso 1 1 d G U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O1 2.273(2) . ?
Yb1 O1 2.273(2) 2 ?
Yb1 O1 2.273(2) 3 ?
Yb1 O1 2.273(2) 4 ?
Yb1 N1 2.520(2) 4 ?
Yb1 N1 2.520(2) 3 ?
Yb1 N1 2.520(2) 2 ?
Yb1 N1 2.520(2) . ?
O1 C1 1.276(5) . ?
O2 C1 1.239(4) . ?
N1 C2 1.478(4) . ?
N1 C4 1.481(4) 3 ?
N1 C3 1.495(4) . ?
C1 C2 1.520(5) . ?
C3 C4 1.513(5) . ?
N1_1 C3_1 1.492(6) . ?
N1_1 C2_1 1.494(4) 7 ?
N1_1 C2_1 1.495(4) . ?
N1_1 C1_1 1.498(6) . ?
N1_2 C2_2 1.440(11) . ?
N1_2 C1_2 1.512(14) . ?
N1_2 C3_2 1.518(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
O1 Yb1 O1 123.74(11) . 2 ?
O1 Yb1 O1 77.16(5) . 3 ?
O1 Yb1 O1 77.15(5) 2 3 ?
O1 Yb1 O1 77.15(5) . 4 ?
O1 Yb1 O1 77.15(5) 2 4 ?
O1 Yb1 O1 123.74(11) 3 4 ?
O1 Yb1 N1 88.59(8) . 4 ?
O1 Yb1 N1 124.81(8) 2 4 ?
O1 Yb1 N1 158.03(8) 3 4 ?
O1 Yb1 N1 67.60(8) 4 4 ?
O1 Yb1 N1 124.81(8) . 3 ?
O1 Yb1 N1 88.59(8) 2 3 ?
O1 Yb1 N1 67.60(8) 3 3 ?
O1 Yb1 N1 158.03(8) 4 3 ?
N1 Yb1 N1 109.19(11) 4 3 ?
O1 Yb1 N1 158.03(8) . 2 ?
O1 Yb1 N1 67.60(8) 2 2 ?
O1 Yb1 N1 124.81(8) 3 2 ?
O1 Yb1 N1 88.59(8) 4 2 ?
N1 Yb1 N1 70.39(6) 4 2 ?
N1 Yb1 N1 70.39(6) 3 2 ?
O1 Yb1 N1 67.60(8) . . ?
O1 Yb1 N1 158.03(8) 2 . ?
O1 Yb1 N1 88.59(8) 3 . ?
O1 Yb1 N1 124.81(8) 4 . ?
N1 Yb1 N1 70.39(6) 4 . ?
N1 Yb1 N1 70.39(6) 3 . ?
N1 Yb1 N1 109.19(11) 2 . ?
C1 O1 Yb1 119.9(2) . . ?
C2 N1 C4 110.8(3) . 3 ?
C2 N1 C3 108.1(3) . . ?
C4 N1 C3 109.9(2) 3 . ?
C2 N1 Yb1 104.5(2) . . ?
C4 N1 Yb1 112.39(18) 3 . ?
C3 N1 Yb1 110.97(19) . . ?
O2 C1 O1 125.1(3) . . ?
O2 C1 C2 118.3(3) . . ?
O1 C1 C2 116.6(4) . . ?
O2 C1 Yb1 156.9(3) . . ?
O1 C1 Yb1 39.25(17) . . ?
C2 C1 Yb1 80.3(3) . . ?
N1 C2 C1 112.2(3) . . ?
N1 C3 C4 111.4(3) . . ?
N1 C4 C3 111.1(2) 4 . ?
C3_1 N1_1 C2_1 109.9(2) . 7 ?
C3_1 N1_1 C2_1 109.9(2) . . ?
C2_1 N1_1 C2_1 107.9(3) 7 . ?
C3_1 N1_1 C1_1 109.4(4) . . ?
C2_1 N1_1 C1_1 109.8(2) 7 . ?
C2_1 N1_1 C1_1 109.8(2) . . ?
C2_2 N1_2 C1_2 106.6(7) . . ?
C2_2 N1_2 C3_2 114(2) . . ?
C1_2 N1_2 C3_2 113.4(9) . . ?

_refine_diff_density_max         0.314
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.057

####################################################################### 
# 
# 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_d8v4233_0m_b
_database_code_depnum_ccdc_archive 'CCDC 2281615'
loop_
_audit_author_name
_audit_author_address
'Jesper Bendix'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2023-07-14 deposited with the CCDC.	2023-10-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT242_d8v4233_0m_b        
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        N0A Check
RESPONSE: Unmodeled disorder
;
_vrf_PLAT420_d8v4233_0m_b        
;
PROBLEM: D-H Bond Without Acceptor  O00D     --H00P     .     Please Check
RESPONSE: Unmodeled disorder
;
# Added during the CSD deposition process: Friday 14 July 2023 12:23 PM
# end Validation Reply Form

_audit_creation_date             2021-01-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.11(C16 H24 Dy N4 O8), 0.22(Cl), 0.67(H2 O), 0.22(C4 H12 N), 0.11(C4 H4.5 N)'
_chemical_formula_sum            'C3.11 H6.72 Cl0.22 Dy0.11 N0.78 O1.56'
_chemical_formula_weight         105.86
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Dy Dy -0.1892 4.4098 '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'

_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      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   17.4527(9)
_cell_length_b                   17.4527(9)
_cell_length_c                   6.7995(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2071.1(2)
_cell_formula_units_Z            18
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.503
_cell_measurement_theta_min      3.301
_shelx_estimated_absorpt_T_max   0.797
_shelx_estimated_absorpt_T_min   0.493
_exptl_absorpt_coefficient_mu    2.000
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1610 before and 0.0925 after correction.
The Ratio of minimum to maximum transmission is 0.5715.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             979
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.119
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            22787
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.610
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                2315
_reflns_number_total             2466
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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         0.647
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 
;
 Flack x determined using 1019 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2466
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0169
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0184P)²+0.5835P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0414
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H00J(0.5) H00K(0.5) H00L(0.5) H00M(0.5) H00N(0.5) H00O(0.5)
 H00P(0.5) H00Q(0.5) C2(0.375) H2(0.375) C3(0.375) H1A(0.25) H1B(0.25) H1C(0.25)
3.a Free rotating group:
 O00D(H00P,H00Q)
3.b Ternary CH refined with riding coordinates:
 C2(H2)
3.c Secondary CH2 refined with riding coordinates:
 C00B(H00A,H00B), C00N(H00C,H00D), C00S(H00E,H00F)
3.d Idealised Me refined as rotating group:
 C008(H00G,H00H,H00I), C00A(H00J,H00K,H00L), C00C(H00M,H00N,H00O), C1(H1A,H1B,
 H1C)
;
_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
Dy01 Dy 0.500000 0.500000 -0.01375(9) 0.00713(7) Uani 1 4 d S T P . .
Cl02 Cl 0.66229(4) 0.16229(4) -0.27517(15) 0.0242(2) Uani 1 2 d S T P . .
O003 O 0.46849(12) 0.27085(11) 0.2095(3) 0.0190(4) Uani 1 1 d . . . . .
O004 O 0.44753(10) 0.39416(10) 0.1398(3) 0.0121(3) Uani 1 1 d . . . . .
O06 O 0.49729(17) 0.1719(2) 0.5265(4) 0.0336(9) Uani 1 1 d . . . . .
C008 C 0.26291(15) 0.33515(15) 0.2345(4) 0.0185(5) Uani 1 1 d . . . . .
H00G H 0.238286 0.358789 0.123831 0.028 Uiso 1 1 calc GR . . . .
H00H H 0.316976 0.345068 0.229286 0.028 Uiso 1 1 calc GR . . . .
H00I H 0.242218 0.355885 0.354047 0.028 Uiso 1 1 calc GR . . . .
C009 C 0.47237(17) 0.32725(16) 0.0993(4) 0.0122(5) Uani 1 1 d . . . . .
C00A C 0.28649(18) 0.21351(18) 0.4014(6) 0.0203(9) Uani 1 2 d S T P . .
H00J H 0.341156 0.216109 0.387178 0.030 Uiso 0.5 1 calc GR . . A -1
H00K H 0.270833 0.160852 0.408599 0.030 Uiso 0.5 1 calc GR . . A -1
H00L H 0.271474 0.239576 0.519609 0.030 Uiso 0.5 1 calc GR . . A -1
C00B C 0.41656(15) 0.37194(15) -0.3217(4) 0.0120(5) Uani 1 1 d . . . . .
H00A H 0.382529 0.350937 -0.222584 0.014 Uiso 1 1 calc R . . . .
H00B H 0.418974 0.335812 -0.429905 0.014 Uiso 1 1 calc R . . . .
C00C C 0.28228(18) 0.21772(18) 0.0446(5) 0.0196(9) Uani 1 2 d S T P . .
H00M H 0.257507 0.240335 -0.067326 0.029 Uiso 0.5 1 calc GR . . B -1
H00N H 0.274288 0.163303 0.043158 0.029 Uiso 0.5 1 calc GR . . B -1
H00O H 0.336208 0.228359 0.039466 0.029 Uiso 0.5 1 calc GR . . B -1
O00D O 0.36623(16) 0.13377(16) -0.2622(5) 0.0415(9) Uani 1 2 d S T P . .
H00P H 0.378877 0.146464 -0.142716 0.062 Uiso 0.5 1 d G . . . .
H00Q H 0.405267 0.143589 -0.332557 0.062 Uiso 0.5 1 d G . . . .
N00E N 0.49463(11) 0.38154(15) -0.2359(3) 0.0104(5) Uani 1 1 d . . . . .
N00F N 0.24930(10) 0.25070(10) 0.2291(5) 0.0139(7) Uani 1 2 d S T P . .
C00N C 0.50927(17) 0.31614(19) -0.1024(5) 0.0131(6) Uani 1 1 d . . . . .
H00C H 0.564124 0.309840 -0.086098 0.016 Uiso 1 1 calc R . . . .
H00D H 0.489331 0.269684 -0.161669 0.016 Uiso 1 1 calc R . . . .
C00S C 0.55256(15) 0.38429(15) -0.3953(4) 0.0127(5) Uani 1 1 d . . . . .
H00E H 0.533571 0.415964 -0.501941 0.015 Uiso 1 1 calc R . . . .
H00F H 0.560763 0.333033 -0.446276 0.015 Uiso 1 1 calc R . . . .
N0A N 0.500000 0.000000 1.0396(10) 0.0229(15) Uani 1 4 d S T P . .
H06A H 0.490(3) 0.213(4) 0.428(10) 0.06(2) Uiso 1 1 d . . . . .
C2 C 0.5533(6) 0.0533(6) 1.1015(19) 0.24(2) Uani 0.75 2 d S T P . .
H2 H 0.586114 0.086114 1.020509 0.293 Uiso 0.75 2 calc RS T P . .
C3 C 0.4451(7) 0.0549(7) 1.1225(19) 0.134(8) Uani 0.75 2 d S T P . .
C1 C 0.500000 0.000000 0.8194(16) 0.041(2) Uani 1 4 d S T P . .
H1A H 0.510251 -0.050837 0.772348 0.062 Uiso 0.25 1 calc GR . . C -1
H1B H 0.538900 0.034296 0.772348 0.062 Uiso 0.25 1 calc GR . . C -1
H1C H 0.450849 0.016541 0.772348 0.062 Uiso 0.25 1 calc GR . . C -1
H06B H 0.532(4) 0.175(4) 0.563(10) 0.09(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
Dy01 O004 2.3109(18) . ?
Dy01 O004 2.3109(18) 2_665 ?
Dy01 O004 2.3109(18) 3_655 ?
Dy01 O004 2.3109(18) 4_565 ?
Dy01 N00E 2.562(2) . ?
Dy01 N00E 2.562(2) 4_565 ?
Dy01 N00E 2.562(2) 2_665 ?
Dy01 N00E 2.562(2) 3_655 ?
O003 C009 1.239(3) . ?
O004 C009 1.276(3) . ?
C008 N00F 1.493(3) . ?
C009 C00N 1.528(4) . ?
C00A N00F 1.489(5) . ?
C00B N00E 1.492(3) . ?
C00B C00S 1.518(4) 4_565 ?
C00C N00F 1.495(5) . ?
N00E C00N 1.480(4) . ?
N00E C00S 1.483(3) . ?
N0A C2 1.380(14) . ?
N0A C2 1.380(14) 2_655 ?
N0A C3 1.468(16) . ?
N0A C3 1.468(16) 2_655 ?
N0A C1 1.497(15) . ?
C2 C3 1.894(19) . ?
C2 C3 1.894(19) 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
O004 Dy01 O004 126.30(9) . 2_665 ?
O004 Dy01 O004 78.23(4) 2_665 3_655 ?
O004 Dy01 O004 78.23(4) . 3_655 ?
O004 Dy01 O004 78.23(4) 2_665 4_565 ?
O004 Dy01 O004 78.23(4) . 4_565 ?
O004 Dy01 O004 126.30(9) 3_655 4_565 ?
O004 Dy01 N00E 66.84(7) . . ?
O004 Dy01 N00E 157.79(6) 2_665 . ?
O004 Dy01 N00E 66.84(7) 3_655 3_655 ?
O004 Dy01 N00E 123.83(6) 2_665 4_565 ?
O004 Dy01 N00E 66.84(7) 2_665 2_665 ?
O004 Dy01 N00E 123.83(6) 3_655 2_665 ?
O004 Dy01 N00E 157.79(6) 3_655 4_565 ?
O004 Dy01 N00E 66.84(7) 4_565 4_565 ?
O004 Dy01 N00E 88.61(7) 4_565 2_665 ?
O004 Dy01 N00E 157.79(6) . 2_665 ?
O004 Dy01 N00E 88.61(7) 3_655 . ?
O004 Dy01 N00E 123.83(6) . 3_655 ?
O004 Dy01 N00E 88.61(7) 2_665 3_655 ?
O004 Dy01 N00E 88.61(7) . 4_565 ?
O004 Dy01 N00E 123.83(6) 4_565 . ?
O004 Dy01 N00E 157.79(6) 4_565 3_655 ?
N00E Dy01 N00E 69.67(5) . 4_565 ?
N00E Dy01 N00E 69.67(5) 2_665 3_655 ?
N00E Dy01 N00E 69.67(5) . 3_655 ?
N00E Dy01 N00E 107.76(11) . 2_665 ?
N00E Dy01 N00E 69.67(5) 4_565 2_665 ?
N00E Dy01 N00E 107.76(11) 4_565 3_655 ?
C009 O004 Dy01 119.98(16) . . ?
O003 C009 O004 125.3(3) . . ?
O003 C009 C00N 117.7(3) . . ?
O004 C009 C00N 116.9(3) . . ?
N00E C00B C00S 111.7(2) . 4_565 ?
C00B N00E Dy01 110.77(16) . . ?
C00N N00E Dy01 104.74(17) . . ?
C00N N00E C00B 108.1(2) . . ?
C00N N00E C00S 110.8(2) . . ?
C00S N00E Dy01 112.32(16) . . ?
C00S N00E C00B 109.90(19) . . ?
C008 N00F C008 108.3(3) . 7 ?
C008 N00F C00C 109.9(2) 7 . ?
C008 N00F C00C 109.9(2) . . ?
C00A N00F C008 110.0(2) . 7 ?
C00A N00F C008 110.0(2) . . ?
C00A N00F C00C 108.9(3) . . ?
N00E C00N C009 112.3(3) . . ?
N00E C00S C00B 111.3(2) . 3_655 ?
C2 N0A C2 144.5(13) . 2_655 ?
C2 N0A C3 83.3(3) . . ?
C2 N0A C3 83.3(3) 2_655 . ?
C2 N0A C3 83.3(3) . 2_655 ?
C2 N0A C3 83.3(3) 2_655 2_655 ?
C2 N0A C1 107.7(6) 2_655 . ?
C2 N0A C1 107.7(6) . . ?
C3 N0A C3 134.8(12) . 2_655 ?
C3 N0A C1 112.6(6) . . ?
C3 N0A C1 112.6(6) 2_655 . ?
N0A C2 C3 50.4(4) . . ?
N0A C2 C3 50.4(4) . 2_655 ?
C3 C2 C3 91.4(7) . 2_655 ?
N0A C3 C2 46.4(4) . . ?
N0A C3 C2 46.4(4) . 2_655 ?
C2 C3 C2 87.9(7) . 2_655 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_d8v4649_0m
_database_code_depnum_ccdc_archive 'CCDC 2281620'
loop_
_audit_author_name
_audit_author_address
'Jesper Bendix'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2023-07-14 deposited with the CCDC.	2023-10-27 downloaded from the CCDC.
;
_audit_creation_date             2021-01-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C16 H24 N4 O8 Y, 2(Cl), C4 H7 N, 6(H2 O), 2(C4 H12 N)'
_chemical_formula_sum            'C28 H67 Cl2 N7 O14 Y'
_chemical_formula_weight         885.69
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
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'
Y Y -2.7962 3.5667 '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      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   17.4345(6)
_cell_length_b                   17.4345(6)
_cell_length_c                   6.7946(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2065.30(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.32
_cell_measurement_theta_min      2.34
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.609
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.5093
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1211 before and 0.0786 after correction.
The Ratio of minimum to maximum transmission is 0.6821.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             938
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            30819
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         1.652
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1847
_reflns_number_total             2068
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         0.396
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 
;
 Flack x determined using 782 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.401(3)
_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     152
_refine_ls_number_reflns         2068
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0459
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0633P)²+7.2744P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1221
_refine_special_details          ?
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.59954
 0.40046
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Others
 Fixed Sof: H00U(0.5) H00V(0.5) H00J(0.5) H00K(0.5) H00L(0.5) H00Q(0.25)
 H00R(0.25) H00P(0.25) H00M(0.5) H00N(0.5) H00O(0.5) C1(0.25) C2(0.5)
4.a Free rotating group:
 O006(H00S,H00T), O007(H00U,H00V)
4.b Secondary CH2 refined with riding coordinates:
 C00A(H00A,H00B), C00E(H00C,H00D), C00G(H00E,H00F)
4.c Idealised Me refined as rotating group:
 C00C(H00G,H00H,H00I), C00D(H00J,H00K,H00L), C00F(H00Q,H00R,H00P), C00H(H00M,
 H00N,H00O)
;
_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
Y001 Y 0.500000 0.500000 0.01855(16) 0.0066(3) Uani 1 4 d S T P . .
Cl02 Cl 0.66199(10) 0.16199(10) 0.2787(4) 0.0235(5) Uani 1 2 d S T P . .
O003 O 0.4477(2) 0.3951(2) -0.1357(7) 0.0127(9) Uani 1 1 d . . . . .
O004 O 0.4682(3) 0.2716(3) -0.2070(7) 0.0181(10) Uani 1 1 d . . . . .
N005 N 0.500000 0.000000 -0.0362(18) 0.024(3) Uani 1 4 d S T P . .
O006 O 0.4971(3) 0.1723(3) 0.4768(8) 0.0346(15) Uani 1 1 d . . . . .
H00S H 0.542737 0.172659 0.432847 0.052 Uiso 1 1 d G . . . .
H00T H 0.494704 0.210994 0.552339 0.052 Uiso 1 1 d G . . . .
O007 O 0.3658(3) 0.1342(3) 0.2643(13) 0.039(2) Uani 1 2 d S T P . .
H00U H 0.366109 0.088960 0.309680 0.059 Uiso 0.5 1 d G . . . .
H00V H 0.404299 0.155790 0.319753 0.059 Uiso 0.5 1 d G . . . .
N008 N 0.4945(3) 0.3816(3) 0.2392(7) 0.0107(11) Uani 1 1 d . . . . .
N009 N 0.2492(3) 0.2508(3) -0.2251(12) 0.0155(16) Uani 1 2 d S T P . .
C00A C 0.4164(4) 0.3720(4) 0.3250(9) 0.0123(13) Uani 1 1 d . . . . .
H00A H 0.418854 0.335828 0.433389 0.015 Uiso 1 1 calc R . . . .
H00B H 0.382360 0.350910 0.225914 0.015 Uiso 1 1 calc R . . . .
C00B C 0.4723(4) 0.3277(4) -0.0960(9) 0.0113(13) Uani 1 1 d . . . . .
C00C C 0.2627(4) 0.3356(4) -0.2313(11) 0.0184(14) Uani 1 1 d . . . . .
H00G H 0.243844 0.355890 -0.353370 0.028 Uiso 1 1 calc GR . . . .
H00H H 0.316712 0.345701 -0.220740 0.028 Uiso 1 1 calc GR . . . .
H00I H 0.236342 0.359639 -0.123652 0.028 Uiso 1 1 calc GR . . . .
C00D C 0.2864(5) 0.2136(5) -0.4002(15) 0.021(2) Uani 1 2 d S T P . .
H00J H 0.258738 0.227247 -0.517289 0.031 Uiso 0.5 1 calc GR . . A -1
H00K H 0.285657 0.158938 -0.384093 0.031 Uiso 0.5 1 calc GR . . A -1
H00L H 0.338457 0.230963 -0.410984 0.031 Uiso 0.5 1 calc GR . . A -1
C00E C 0.5095(4) 0.3164(4) 0.1050(10) 0.0131(14) Uani 1 1 d . . . . .
H00C H 0.489841 0.269666 0.163877 0.016 Uiso 1 1 calc R . . . .
H00D H 0.564402 0.310434 0.088165 0.016 Uiso 1 1 calc R . . . .
C00F C 0.500000 0.000000 0.183(3) 0.043(5) Uani 1 4 d S T P . .
H00P H 0.499696 -0.051913 0.230039 0.065 Uiso 0.25 1 calc GR . . B -1
H00R H 0.455194 0.026220 0.230039 0.065 Uiso 0.25 1 calc GR . . B -1
H00Q H 0.545110 0.025693 0.230039 0.065 Uiso 0.25 1 calc GR . . B -1
C00G C 0.5525(4) 0.3841(4) 0.3986(9) 0.0118(13) Uani 1 1 d . . . . .
H00E H 0.560719 0.332700 0.449170 0.014 Uiso 1 1 calc R . . . .
H00F H 0.533548 0.415663 0.505600 0.014 Uiso 1 1 calc R . . . .
C00H C 0.2824(4) 0.2176(4) -0.0417(14) 0.018(2) Uani 1 2 d S T P . .
H00M H 0.337277 0.221777 -0.045892 0.027 Uiso 0.5 1 calc GR . . C -1
H00N H 0.268130 0.164567 -0.031647 0.027 Uiso 0.5 1 calc GR . . C -1
H00O H 0.263178 0.245071 0.070342 0.027 Uiso 0.5 1 calc GRS T P C -1
C1 C 0.4441(13) 0.0559(13) -0.121(5) 0.065(10) Uani 0.5 2 d S T P . .
C2 C 0.520(3) 0.0775(17) -0.089(4) 0.113(17) Uani 0.5 1 d . . . . .
H1 H 0.505(11) 0.077(12) -0.20(2) 0.16(9) 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
Y001 O003 2.297(4) . ?
Y001 O003 2.297(4) 4_565 ?
Y001 O003 2.297(4) 2_665 ?
Y001 O003 2.297(4) 3_655 ?
Y001 N008 2.553(5) 3_655 ?
Y001 N008 2.553(5) 4_565 ?
Y001 N008 2.553(5) . ?
Y001 N008 2.553(5) 2_665 ?
O003 C00B 1.279(8) . ?
O004 C00B 1.238(8) . ?
N005 C00F 1.49(2) . ?
N005 C1 1.49(3) 2_655 ?
N005 C1 1.49(3) . ?
N005 C2 1.44(3) 2_655 ?
N005 C2 1.44(3) . ?
N005 C2 1.44(3) 7 ?
N005 C2 1.44(3) 8_545 ?
N008 C00A 1.491(8) . ?
N008 C00E 1.480(8) . ?
N008 C00G 1.482(8) . ?
N009 C00C 1.498(8) 7 ?
N009 C00C 1.498(8) . ?
N009 C00D 1.502(13) . ?
N009 C00H 1.491(12) . ?
C00A C00G 1.517(9) 4_565 ?
C00B C00E 1.525(9) . ?
C1 C2 1.39(4) 7 ?
C1 C2 1.39(4) . ?
C2 C2 1.43(9) 8_545 ?

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
O003 Y001 O003 77.98(10) . 4_565 ?
O003 Y001 O003 125.7(2) . 2_665 ?
O003 Y001 O003 77.98(10) 4_565 2_665 ?
O003 Y001 O003 77.98(10) . 3_655 ?
O003 Y001 O003 125.7(2) 4_565 3_655 ?
O003 Y001 O003 77.98(10) 2_665 3_655 ?
O003 Y001 N008 88.65(16) 2_665 3_655 ?
O003 Y001 N008 157.92(16) 3_655 4_565 ?
O003 Y001 N008 88.65(16) . 4_565 ?
O003 Y001 N008 88.65(16) 3_655 . ?
O003 Y001 N008 67.00(16) 2_665 2_665 ?
O003 Y001 N008 124.02(15) 4_565 . ?
O003 Y001 N008 67.00(16) 3_655 3_655 ?
O003 Y001 N008 157.92(16) . 2_665 ?
O003 Y001 N008 124.02(15) . 3_655 ?
O003 Y001 N008 157.92(16) 4_565 3_655 ?
O003 Y001 N008 157.92(16) 2_665 . ?
O003 Y001 N008 124.02(15) 3_655 2_665 ?
O003 Y001 N008 67.00(16) 4_565 4_565 ?
O003 Y001 N008 88.65(16) 4_565 2_665 ?
O003 Y001 N008 67.00(16) . . ?
O003 Y001 N008 124.02(15) 2_665 4_565 ?
N008 Y001 N008 69.84(12) 2_665 3_655 ?
N008 Y001 N008 108.1(2) 2_665 . ?
N008 Y001 N008 69.84(12) 4_565 . ?
N008 Y001 N008 108.1(2) 3_655 4_565 ?
N008 Y001 N008 69.84(12) 2_665 4_565 ?
N008 Y001 N008 69.84(12) 3_655 . ?
C00B O003 Y001 120.1(4) . . ?
C00F N005 C1 112.7(14) . . ?
C00F N005 C1 112.7(14) . 2_655 ?
C1 N005 C1 135(3) 2_655 . ?
C2 N005 C00F 104.5(12) 8_545 . ?
C2 N005 C00F 104.5(12) 7 . ?
C2 N005 C00F 104.5(12) . . ?
C2 N005 C00F 104.5(12) 2_655 . ?
C2 N005 C1 56.3(18) 2_655 2_655 ?
C2 N005 C1 56.3(18) . . ?
C2 N005 C1 56.3(18) 7 . ?
C2 N005 C1 111.2(17) 7 2_655 ?
C2 N005 C1 111.2(17) . 2_655 ?
C2 N005 C1 111.2(17) 2_655 . ?
C2 N005 C1 111.2(17) 8_545 . ?
C2 N005 C1 56.3(18) 8_545 2_655 ?
C2 N005 C2 112(4) 2_655 8_545 ?
C2 N005 C2 151(2) 7 8_545 ?
C2 N005 C2 151(2) 2_655 . ?
C2 N005 C2 60(4) 8_545 . ?
C2 N005 C2 112(4) 7 . ?
C2 N005 C2 60(4) 7 2_655 ?
C00A N008 Y001 110.8(4) . . ?
C00E N008 Y001 104.6(4) . . ?
C00E N008 C00A 108.4(5) . . ?
C00E N008 C00G 110.7(5) . . ?
C00G N008 Y001 112.3(4) . . ?
C00G N008 C00A 109.9(5) . . ?
C00C N009 C00C 108.1(7) . 7 ?
C00C N009 C00D 109.6(5) 7 . ?
C00C N009 C00D 109.6(5) . . ?
C00H N009 C00C 110.2(5) . 7 ?
C00H N009 C00C 110.2(5) . . ?
C00H N009 C00D 109.0(7) . . ?
N008 C00A C00G 111.8(5) . 4_565 ?
O003 C00B C00E 116.8(6) . . ?
O004 C00B O003 125.4(6) . . ?
O004 C00B C00E 117.8(6) . . ?
N008 C00E C00B 112.2(6) . . ?
N008 C00G C00A 111.2(5) . 3_655 ?
C2 C1 N005 59.8(17) 7 . ?
C2 C1 N005 59.8(17) . . ?
C2 C1 C2 119(3) 7 . ?
C1 C2 N005 63.8(17) . . ?
C1 C2 C2 118.6(19) . 8_545 ?
C2 C2 N005 60.2(18) 8_545 . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.59954
2 0.40046

####################################################################### 
# 
# 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_mo_d8v4762_0m
_database_code_depnum_ccdc_archive 'CCDC 2281618'
loop_
_audit_author_name
_audit_author_address
'Jesper Bendix'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2023-07-14 deposited with the CCDC.	2023-10-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT214_mo_d8v4762_0m       
;
PROBLEM: Atom C9        (Anion/Solvent) ADP max/min Ratio        5.3 prolat
RESPONSE: Unmodeled disorder
;
# Added during the CSD deposition process: Friday 14 July 2023 12:23 PM
# end Validation Reply Form

_audit_creation_date             2021-02-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.5(C16 H24 N4 O8 Tm), 2(H2 O), C4 H12 N, 0.5(C4 H3 N), 0.5(H2 O2), Cl'
_chemical_formula_sum            'C14 H30.50 Cl N3.50 O7 Tm0.50'
_chemical_formula_weight         479.83
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
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'
Tm Tm -0.3139 5.2483 '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      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   17.3929(6)
_cell_length_b                   17.3929(6)
_cell_length_c                   6.7672(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2047.17(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9550
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      37.58
_cell_measurement_theta_min      2.62
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.365
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_correction_T_min  0.5001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1543 before and 0.0763 after correction.
The Ratio of minimum to maximum transmission is 0.6691.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             986
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            49189
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.967
_diffrn_reflns_theta_min         2.342
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                3616
_reflns_number_total             4595
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         2.262
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 
;
 Flack x determined using 1427 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         4595
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0255
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0219P)²+1.1616P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0561
_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 C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H00G(0.5) H00H(0.5) H00I(0.5) H00P(0.25) H00R(0.25) H00Q(0.25)
 H00M(0.5) H00N(0.5) H00O(0.5) H00U(0.5) C9(0.75)
3.a Free rotating group:
 O005(H00S,H00T), O00K(H00U)
3.b Secondary CH2 refined with riding coordinates:
 C009(H00A,H00B), C00A(H00C,H00D), C00D(H00E,H00F)
3.c Idealised Me refined as rotating group:
 C007(H00G,H00H,H00I), C008(H00J,H00K,H00L), C00B(H00P,H00R,H00Q), C00C(H00M,
 H00N,H00O)
;
_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
Tm01 Tm 0.500000 0.500000 0.53634(8) 0.00638(5) Uani 1 4 d S T P . .
O003 O 0.72696(12) 0.46754(13) 0.3049(4) 0.0158(4) Uani 1 1 d . . . . .
C004 C 0.67110(18) 0.47230(19) 0.4171(5) 0.0103(5) Uani 1 1 d . . . . .
O005 O 0.82846(19) 0.49800(16) -0.0087(4) 0.0342(8) Uani 1 1 d . . . . .
H00S H 0.790710 0.498235 0.070733 0.051 Uiso 1 1 d G . . . .
H00T H 0.826521 0.541519 -0.065455 0.051 Uiso 1 1 d G . . . .
O006 O 0.60342(11) 0.44773(12) 0.3798(3) 0.0100(4) Uani 1 1 d . . . . .
C007 C 0.7878(2) 0.2878(2) 1.1126(7) 0.0201(9) Uani 1 2 d S T P . .
H00G H 0.762452 0.271224 0.993909 0.030 Uiso 0.5 1 calc GR . . A -1
H00H H 0.841005 0.273339 1.107376 0.030 Uiso 0.5 1 calc GR . . A -1
H00I H 0.783733 0.342626 1.124276 0.030 Uiso 0.5 1 calc GR . . A -1
C008 C 0.66576(17) 0.26427(17) 1.2804(5) 0.0167(6) Uani 1 1 d . . . . .
H00J H 0.655760 0.318546 1.281017 0.025 Uiso 1 1 calc GR . . . .
H00K H 0.642211 0.241035 1.394001 0.025 Uiso 1 1 calc GR . . . .
H00L H 0.644832 0.241888 1.162452 0.025 Uiso 1 1 calc GR . . . .
C009 C 0.55322(16) 0.38409(16) 0.9141(4) 0.0099(5) Uani 1 1 d . . . . .
H00A H 0.561764 0.332515 0.963974 0.012 Uiso 1 1 calc R . . . .
H00B H 0.534147 0.415431 1.022006 0.012 Uiso 1 1 calc R . . . .
C00A C 0.62850(16) 0.41704(16) 0.8397(4) 0.0101(5) Uani 1 1 d . . . . .
H00C H 0.664803 0.419776 0.948288 0.012 Uiso 1 1 calc R . . . .
H00D H 0.649770 0.383028 0.740141 0.012 Uiso 1 1 calc R . . . .
C00B C 1.000000 0.500000 -0.2978(18) 0.052(3) Uani 1 4 d S T P . .
H00P H 1.024676 0.454185 -0.250514 0.077 Uiso 0.25 1 calc GR . . B -1
H00R H 0.947984 0.501537 -0.250515 0.077 Uiso 0.25 1 calc GR . . B -1
H00Q H 1.027339 0.544278 -0.250514 0.077 Uiso 0.25 1 calc GR . . B -1
C00C C 0.7837(2) 0.2837(2) 1.4712(7) 0.0178(9) Uani 1 2 d S T P . .
H00M H 0.837916 0.273319 1.475971 0.027 Uiso 0.5 1 calc GR . . C -1
H00N H 0.759099 0.260863 1.583692 0.027 Uiso 0.5 1 calc GR . . C -1
H00O H 0.775482 0.338315 1.472947 0.027 Uiso 0.5 1 calc GR . . C -1
C00D C 0.68316(17) 0.51013(17) 0.6176(5) 0.0102(5) Uani 1 1 d . . . . .
H00E H 0.730303 0.490824 0.675892 0.012 Uiso 1 1 calc R . . . .
H00F H 0.688753 0.565183 0.599697 0.012 Uiso 1 1 calc R . . . .
N00F N 0.61831(14) 0.49500(13) 0.7537(3) 0.0091(4) Uani 1 1 d . . . . .
N00H N 0.75074(14) 0.25074(14) 1.2865(6) 0.0148(6) Uani 1 2 d S T P . .
O00K O 0.8685(2) 0.3685(2) -0.2231(9) 0.0514(13) Uani 1 2 d S T P . .
H00U H 0.860716 0.409367 -0.164128 0.077 Uiso 0.5 1 d G . . . .
N00L N 1.000000 0.500000 -0.5228(12) 0.0287(14) Uani 1 4 d S T P . .
Cl1 Cl 0.83675(5) 0.66325(5) -0.20944(19) 0.0228(2) Uani 1 2 d S T P . .
C9 C 0.9252(7) 0.5001(10) -0.5860(19) 0.249(17) Uani 0.75 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
Tm01 O006 2.277(2) . ?
Tm01 O006 2.277(2) 4_565 ?
Tm01 O006 2.277(2) 2_665 ?
Tm01 O006 2.277(2) 3_655 ?
Tm01 N00F 2.531(2) 3_655 ?
Tm01 N00F 2.531(2) 4_565 ?
Tm01 N00F 2.531(2) 2_665 ?
Tm01 N00F 2.531(2) . ?
O003 C004 1.236(4) . ?
C004 O006 1.278(4) . ?
C004 C00D 1.522(5) . ?
C007 N00H 1.488(6) . ?
C008 N00H 1.497(4) . ?
C009 C00A 1.515(4) . ?
C009 N00F 1.485(4) 4_565 ?
C00A N00F 1.486(4) . ?
C00B N00L 1.523(18) . ?
C00C N00H 1.491(6) . ?
C00D N00F 1.480(4) . ?
N00L C9 1.369(12) 8_545 ?
N00L C9 1.369(12) 2_765 ?
N00L C9 1.369(12) . ?
N00L C9 1.369(12) 7_665 ?
C9 C9 1.84(3) 7_665 ?
C9 C9 1.84(3) 8_545 ?

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
O006 Tm01 O006 77.50(5) . 4_565 ?
O006 Tm01 O006 77.50(5) 4_565 2_665 ?
O006 Tm01 O006 124.55(11) . 2_665 ?
O006 Tm01 O006 124.55(11) 4_565 3_655 ?
O006 Tm01 O006 77.50(5) . 3_655 ?
O006 Tm01 O006 77.50(5) 2_665 3_655 ?
O006 Tm01 N00F 157.89(7) . 2_665 ?
O006 Tm01 N00F 157.89(7) 3_655 4_565 ?
O006 Tm01 N00F 67.31(8) 3_655 3_655 ?
O006 Tm01 N00F 157.89(7) 4_565 3_655 ?
O006 Tm01 N00F 124.60(7) 3_655 2_665 ?
O006 Tm01 N00F 88.45(7) 2_665 3_655 ?
O006 Tm01 N00F 124.60(7) . 3_655 ?
O006 Tm01 N00F 124.60(7) 2_665 4_565 ?
O006 Tm01 N00F 67.31(8) . . ?
O006 Tm01 N00F 88.45(8) 3_655 . ?
O006 Tm01 N00F 157.89(7) 2_665 . ?
O006 Tm01 N00F 124.60(7) 4_565 . ?
O006 Tm01 N00F 88.44(7) . 4_565 ?
O006 Tm01 N00F 88.45(8) 4_565 2_665 ?
O006 Tm01 N00F 67.31(8) 4_565 4_565 ?
O006 Tm01 N00F 67.31(8) 2_665 2_665 ?
N00F Tm01 N00F 70.26(6) 4_565 2_665 ?
N00F Tm01 N00F 108.94(11) 3_655 4_565 ?
N00F Tm01 N00F 70.27(6) 3_655 . ?
N00F Tm01 N00F 70.26(5) 3_655 2_665 ?
N00F Tm01 N00F 70.26(6) 4_565 . ?
N00F Tm01 N00F 108.94(11) 2_665 . ?
O003 C004 O006 125.5(3) . . ?
O003 C004 C00D 117.9(3) . . ?
O006 C004 C00D 116.6(3) . . ?
C004 O006 Tm01 120.16(19) . . ?
N00F C009 C00A 110.9(2) 4_565 . ?
N00F C00A C009 111.8(2) . . ?
N00F C00D C004 111.9(2) . . ?
C009 N00F Tm01 112.24(16) 3_655 . ?
C009 N00F C00A 109.8(2) 3_655 . ?
C00A N00F Tm01 110.85(16) . . ?
C00D N00F Tm01 104.60(17) . . ?
C00D N00F C009 110.8(2) . 3_655 ?
C00D N00F C00A 108.4(2) . . ?
C007 N00H C008 109.7(2) . . ?
C007 N00H C008 109.7(2) . 8_545 ?
C007 N00H C00C 109.3(3) . . ?
C008 N00H C008 108.0(3) . 8_545 ?
C00C N00H C008 110.0(2) . 8_545 ?
C00C N00H C008 110.0(2) . . ?
C9 N00L C00B 108.2(7) 7_665 . ?
C9 N00L C00B 108.2(7) 8_545 . ?
C9 N00L C00B 108.2(7) . . ?
C9 N00L C00B 108.2(7) 2_765 . ?
C9 N00L C9 143.6(14) 2_765 . ?
C9 N00L C9 84.3(13) 7_665 . ?
C9 N00L C9 84.5(15) 8_545 . ?
C9 N00L C9 84.3(13) 8_545 2_765 ?
C9 N00L C9 84.5(15) 7_665 2_765 ?
C9 N00L C9 143.6(14) 8_545 7_665 ?
N00L C9 C9 47.9(7) . 7_665 ?
N00L C9 C9 47.7(8) . 8_545 ?
C9 C9 C9 89.999(3) 7_665 8_545 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_d8v4474_1_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2281616'
loop_
_audit_author_name
_audit_author_address
'Jesper Bendix'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2023-07-14 deposited with the CCDC.	2023-10-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_mo_d8v4474_1_0m_a   
;
PROBLEM: D-H Bond Without Acceptor  O00H     --H00S     .     Please Check
RESPONSE: Unmodeled disorder
;
# Added during the CSD deposition process: Friday 14 July 2023 12:23 PM
# end Validation Reply Form

_audit_creation_date             2021-01-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C16 H24 Er N4 O8, 2(Cl), 6(H2 O), 2(C4 H12 N), C4 H3 N'
_chemical_formula_sum            'C28 H0.50 Cl2 Er N7 O14'
_chemical_formula_weight         897.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 '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'

_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      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   17.4237(9)
_cell_length_b                   17.4237(9)
_cell_length_c                   6.7843(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2059.6(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9002
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      37.81
_cell_measurement_theta_min      3.00
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.231
_exptl_absorpt_correction_T_max  0.7477
_exptl_absorpt_correction_T_min  0.5955
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             863
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            47893
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.568
_diffrn_reflns_theta_min         2.338
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3337
_reflns_number_total             3912
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         0.378
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 
;
 Flack x determined using 1387 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3912
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0178
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0113P)²+0.4925P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0365
_refine_ls_wR_factor_ref         0.0386
_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 C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H00J(0.5) H00K(0.5) H00L(0.5) H00M(0.5) H00N(0.5) H00O(0.5)
 H00R(0.5) H00S(0.5) H1A(0.25) H1B(0.25) H1C(0.25) C2(0.5) C3(0.25)
3.a Free rotating group:
 O006(H00P,H00Q), O00H(H00R,H00S)
3.b Secondary CH2 refined with riding coordinates:
 C007(H00A,H00B), C00C(H00C,H00D), C00G(H00E,H00F)
3.c Idealised Me refined as rotating group:
 C008(H00G,H00H,H00I), C009(H00J,H00K,H00L), C00B(H00M,H00N,H00O), C1(H1A,H1B,
 H1C)
;
_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
Er01 Er 0.500000 0.500000 0.97210(6) 0.00564(4) Uani 1 4 d S T P . .
Cl02 Cl 0.33866(4) 0.83866(4) 0.71572(14) 0.01985(16) Uani 1 2 d S T P . .
O003 O 0.44721(9) 0.39622(9) 1.1284(2) 0.0100(3) Uani 1 1 d . . . . .
O004 O 0.46723(10) 0.27284(9) 1.2018(3) 0.0150(3) Uani 1 1 d . . . . .
C005 C 0.47166(14) 0.32876(14) 1.0902(4) 0.0098(4) Uani 1 1 d . . . . .
O006 O 0.50346(12) 0.82802(13) 0.5157(3) 0.0277(5) Uani 1 1 d . . . . .
H00P H 0.458150 0.826444 0.562208 0.041 Uiso 1 1 d G . . . .
H00Q H 0.504539 0.792181 0.430502 0.041 Uiso 1 1 d G . . . .
C007 C 0.44740(13) 0.61596(13) 0.5935(3) 0.0100(4) Uani 1 1 d . . . . .
H00A H 0.466313 0.584376 0.486273 0.012 Uiso 1 1 calc R . . . .
H00B H 0.439217 0.667407 0.543086 0.012 Uiso 1 1 calc R . . . .
C008 C 0.33589(13) 0.73766(13) 0.2250(4) 0.0153(4) Uani 1 1 d . . . . .
H00G H 0.359586 0.762815 0.114831 0.023 Uiso 1 1 calc GR . . . .
H00H H 0.345861 0.683539 0.218271 0.023 Uiso 1 1 calc GR . . . .
H00I H 0.356611 0.757891 0.345432 0.023 Uiso 1 1 calc GR . . . .
C009 C 0.21814(16) 0.71814(16) 0.0351(5) 0.0163(7) Uani 1 2 d S T P . .
H00J H 0.239257 0.744250 -0.077085 0.024 Uiso 0.5 1 calc GR . . A -1
H00K H 0.163398 0.724375 0.036199 0.024 Uiso 0.5 1 calc GR . . A -1
H00L H 0.230495 0.664524 0.027625 0.024 Uiso 0.5 1 calc GR . . A -1
N00A N 0.500000 1.000000 1.0277(7) 0.0175(8) Uani 1 4 d S T P . .
C00B C 0.21432(15) 0.71432(15) 0.3925(6) 0.0174(7) Uani 1 2 d S T P . .
H00M H 0.229431 0.661390 0.398892 0.026 Uiso 0.5 1 calc GR . . B -1
H00N H 0.159546 0.717555 0.379532 0.026 Uiso 0.5 1 calc GR . . B -1
H00O H 0.230066 0.740097 0.510841 0.026 Uiso 0.5 1 calc GR . . B -1
C00C C 0.58358(12) 0.62821(13) 0.6678(3) 0.0099(4) Uani 1 1 d . . . . .
H00C H 0.617673 0.649227 0.767128 0.012 Uiso 1 1 calc R . . . .
H00D H 0.581031 0.664464 0.559521 0.012 Uiso 1 1 calc R . . . .
N00E N 0.25127(10) 0.75127(10) 0.2198(4) 0.0118(5) Uani 1 2 d S T P . .
N00F N 0.50557(10) 0.61831(11) 0.7539(3) 0.0080(3) Uani 1 1 d . . . . .
C00G C 0.49073(14) 0.68306(14) 0.8891(4) 0.0101(5) Uani 1 1 d . . . . .
H00E H 0.435785 0.688899 0.906493 0.012 Uiso 1 1 calc R . . . .
H00F H 0.510230 0.729978 0.830605 0.012 Uiso 1 1 calc R . . . .
O00H O 0.63466(12) 0.86534(12) 0.7293(5) 0.0346(7) Uani 1 2 d S T P . .
H00R H 0.647133 0.907464 0.673930 0.052 Uiso 0.5 1 d G . . . .
H00S H 0.607054 0.871388 0.824781 0.052 Uiso 0.5 1 d G . . . .
C1 C 0.500000 1.000000 0.8076(11) 0.0314(14) Uani 1 4 d S T P . .
H1A H 0.532075 1.040861 0.760395 0.047 Uiso 0.25 1 calc GR . . C -1
H1B H 0.448576 1.007347 0.760394 0.047 Uiso 0.25 1 calc GR . . C -1
H1C H 0.519350 0.951792 0.760394 0.047 Uiso 0.25 1 calc GR . . C -1
C2 C 0.4800(7) 0.9214(5) 1.0894(15) 0.086(4) Uani 0.5 1 d . . . . .
C3 C 0.5564(5) 0.9436(5) 1.1126(18) 0.078(6) Uani 0.5 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er01 O003 2.2891(16) . ?
Er01 O003 2.2891(16) 3_655 ?
Er01 O003 2.2891(16) 2_665 ?
Er01 O003 2.2891(16) 4_565 ?
Er01 N00F 2.5399(18) 2_665 ?
Er01 N00F 2.5399(18) 3_655 ?
Er01 N00F 2.5399(18) 4_565 ?
Er01 N00F 2.5399(18) . ?
O003 C005 1.277(3) . ?
O004 C005 1.236(3) . ?
C005 C00G 1.528(4) 2_665 ?
C007 C00C 1.519(3) 3_655 ?
C007 N00F 1.487(3) . ?
C008 N00E 1.494(3) . ?
C009 N00E 1.495(4) . ?
N00A C1 1.493(10) . ?
N00A C2 1.475(8) . ?
N00A C2 1.475(8) 8_455 ?
N00A C2 1.475(8) 2_675 ?
N00A C2 1.475(8) 7_665 ?
N00A C3 1.503(11) . ?
N00A C3 1.503(11) 2_675 ?
C00B N00E 1.484(5) . ?
C00C N00F 1.489(3) . ?
N00F C00G 1.477(3) . ?
C2 C2 1.44(2) 8_455 ?
C2 C3 1.395(12) . ?

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
O003 Er01 O003 124.81(9) . 2_665 ?
O003 Er01 O003 77.61(4) . 4_565 ?
O003 Er01 O003 77.61(4) 2_665 4_565 ?
O003 Er01 O003 77.61(4) 2_665 3_655 ?
O003 Er01 O003 77.61(4) . 3_655 ?
O003 Er01 O003 124.81(9) 3_655 4_565 ?
O003 Er01 N00F 67.27(6) . 2_665 ?
O003 Er01 N00F 124.47(6) 3_655 . ?
O003 Er01 N00F 124.47(6) . 4_565 ?
O003 Er01 N00F 157.90(6) 2_665 2_665 ?
O003 Er01 N00F 157.90(6) 4_565 4_565 ?
O003 Er01 N00F 88.52(6) 3_655 2_665 ?
O003 Er01 N00F 157.90(6) 3_655 3_655 ?
O003 Er01 N00F 67.27(6) 4_565 3_655 ?
O003 Er01 N00F 88.52(6) 4_565 . ?
O003 Er01 N00F 157.89(6) . . ?
O003 Er01 N00F 67.27(6) 2_665 . ?
O003 Er01 N00F 124.47(6) 4_565 2_665 ?
O003 Er01 N00F 124.47(6) 2_665 3_655 ?
O003 Er01 N00F 88.52(6) 2_665 4_565 ?
O003 Er01 N00F 67.27(6) 3_655 4_565 ?
O003 Er01 N00F 88.52(6) . 3_655 ?
N00F Er01 N00F 70.13(4) 2_665 3_655 ?
N00F Er01 N00F 70.13(4) 2_665 4_565 ?
N00F Er01 N00F 108.68(8) 2_665 . ?
N00F Er01 N00F 70.13(4) 3_655 . ?
N00F Er01 N00F 108.68(8) 3_655 4_565 ?
N00F Er01 N00F 70.13(4) 4_565 . ?
C005 O003 Er01 119.94(15) . . ?
O003 C005 C00G 116.6(2) . 2_665 ?
O004 C005 O003 125.5(2) . . ?
O004 C005 C00G 117.9(2) . 2_665 ?
N00F C007 C00C 111.01(18) . 3_655 ?
C1 N00A C3 112.5(5) . . ?
C1 N00A C3 112.5(5) . 2_675 ?
C2 N00A C1 106.5(5) 8_455 . ?
C2 N00A C1 106.5(5) 7_665 . ?
C2 N00A C1 106.5(5) 2_675 . ?
C2 N00A C1 106.5(5) . . ?
C2 N00A C2 147.0(9) . 2_675 ?
C2 N00A C2 111.0(9) 2_675 8_455 ?
C2 N00A C2 111.0(9) . 7_665 ?
C2 N00A C2 147.0(9) 7_665 8_455 ?
C2 N00A C2 58.6(9) 7_665 2_675 ?
C2 N00A C2 58.6(9) . 8_455 ?
C2 N00A C3 110.1(5) 7_665 2_675 ?
C2 N00A C3 55.9(5) 8_455 2_675 ?
C2 N00A C3 55.9(5) 7_665 . ?
C2 N00A C3 55.9(5) . . ?
C2 N00A C3 55.9(5) 2_675 2_675 ?
C2 N00A C3 110.1(5) 2_675 . ?
C2 N00A C3 110.1(5) 8_455 . ?
C2 N00A C3 110.1(5) . 2_675 ?
C3 N00A C3 134.9(10) 2_675 . ?
N00F C00C C007 111.63(18) . 4_565 ?
C008 N00E C008 108.2(2) . 8_455 ?
C008 N00E C009 109.87(18) 8_455 . ?
C008 N00E C009 109.87(18) . . ?
C00B N00E C008 109.90(19) . 8_455 ?
C00B N00E C008 109.90(19) . . ?
C00B N00E C009 109.1(2) . . ?
C007 N00F Er01 112.21(13) . . ?
C007 N00F C00C 109.79(17) . . ?
C00C N00F Er01 110.93(13) . . ?
C00G N00F Er01 104.55(13) . . ?
C00G N00F C007 110.86(17) . . ?
C00G N00F C00C 108.34(18) . . ?
N00F C00G C005 112.1(2) . 2_665 ?
C2 C2 N00A 60.7(5) 8_455 . ?
C3 C2 N00A 63.1(5) . . ?
C3 C2 C2 118.5(6) . 8_455 ?
C2 C3 N00A 61.0(5) 7_665 . ?
C2 C3 N00A 61.0(5) . . ?
C2 C3 C2 121.2(11) . 7_665 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_d8v4568_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2281619'
loop_
_audit_author_name
_audit_author_address
'Jesper Bendix'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2023-07-14 deposited with the CCDC.	2023-10-27 downloaded from the CCDC.
;
_audit_creation_date             2021-01-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.5(C16 H24 Ho N4 O8), Cl, 3(H2 O), C4 H12 N, 0.5(C4 H7 N)'
_chemical_formula_sum            'C14 H35.50 Cl Ho0.50 N3.50 O7'
_chemical_formula_weight         482.87
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'

_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      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   17.4077(7)
_cell_length_b                   17.4077(7)
_cell_length_c                   6.7730(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2052.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      35.916
_cell_measurement_theta_min      2.340
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.126
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_correction_T_min  0.5043
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_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    1.563
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            43892
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.576
_diffrn_reflns_theta_min         2.340
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                3118
_reflns_number_total             3892
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         0.676
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 
;
 Flack x determined using 1296 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         3892
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0220
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0136P)²+0.9126P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0490
_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 C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H00J(0.5) H00K(0.5) H00L(0.5) H00M(0.5) H00N(0.5) H00O(0.5)
 H00R(0.5) H00S(0.5) H3C(0.25) H3A(0.25) H3B(0.25) C1AA(0.5) C1(0.25)
3.a Free rotating group:
 O008(H00P,H00Q), O00G(H00R,H00S)
3.b Secondary CH2 refined with riding coordinates:
 C006(H00A,H00B), C007(H00C,H00D), C00E(H00E,H00F)
3.c Idealised Me refined as rotating group:
 C009(H00G,H00H,H00I), C00A(H00J,H00K,H00L), C00D(H00M,H00N,H00O), C3(H3C,H3A,
 H3B)
;
_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
Ho01 Ho 0.500000 0.500000 0.97912(7) 0.00662(5) Uani 1 4 d S T P . .
Cl02 Cl 0.16391(5) 0.66391(5) 0.72247(19) 0.0234(2) Uani 1 2 d S T P . .
O003 O 0.39471(12) 0.44815(12) 1.1351(3) 0.0112(4) Uani 1 1 d . . . . .
O004 O 0.27100(12) 0.46853(14) 1.2063(4) 0.0172(4) Uani 1 1 d . . . . .
C005 C 0.3274(2) 0.4728(2) 1.0953(5) 0.0110(6) Uani 1 1 d . . . . .
C006 C 0.38398(17) 0.55314(17) 0.5986(4) 0.0112(5) Uani 1 1 d . . . . .
H00A H 0.332485 0.561564 0.548338 0.013 Uiso 1 1 calc R . . . .
H00B H 0.415422 0.534061 0.491017 0.013 Uiso 1 1 calc R . . . .
C007 C 0.41677(17) 0.62862(17) 0.6728(4) 0.0108(5) Uani 1 1 d . . . . .
H00C H 0.419381 0.664885 0.564271 0.013 Uiso 1 1 calc R . . . .
H00D H 0.382791 0.649814 0.772385 0.013 Uiso 1 1 calc R . . . .
O008 O 0.17116(17) 0.49857(17) 0.5231(4) 0.0350(8) Uani 1 1 d . . . . .
H00P H 0.173747 0.543558 0.571356 0.052 Uiso 1 1 d G . . . .
H00Q H 0.209634 0.495642 0.446042 0.052 Uiso 1 1 d G . . . .
C009 C 0.26461(18) 0.66624(18) 1.2321(5) 0.0180(6) Uani 1 1 d . . . . .
H00G H 0.241967 0.645096 1.349360 0.027 Uiso 1 1 calc GR . . . .
H00H H 0.318860 0.656304 1.232370 0.027 Uiso 1 1 calc GR . . . .
H00I H 0.241732 0.642882 1.117971 0.027 Uiso 1 1 calc GR . . . .
C00A C 0.2841(2) 0.7841(2) 1.0415(7) 0.0207(10) Uani 1 2 d S T P . .
H00J H 0.337188 0.769684 1.030760 0.031 Uiso 0.5 1 calc GR . . A -1
H00K H 0.280114 0.839114 1.045336 0.031 Uiso 0.5 1 calc GR . . A -1
H00L H 0.256326 0.764830 0.929643 0.031 Uiso 0.5 1 calc GR . . A -1
N00B N 0.38148(14) 0.49505(14) 0.7589(3) 0.0092(4) Uani 1 1 d . . . . .
C00D C 0.2881(2) 0.7881(2) 1.4004(7) 0.0206(10) Uani 1 2 d S T P . .
H00M H 0.270933 0.763361 1.519214 0.031 Uiso 0.5 1 calc GR . . B -1
H00N H 0.274339 0.841466 1.404324 0.031 Uiso 0.5 1 calc GR . . B -1
H00O H 0.342861 0.783306 1.389718 0.031 Uiso 0.5 1 calc GR . . B -1
C00E C 0.3163(2) 0.51008(19) 0.8942(5) 0.0120(7) Uani 1 1 d . . . . .
H00E H 0.269427 0.490626 0.835114 0.014 Uiso 1 1 calc R . . . .
H00F H 0.310533 0.565099 0.911248 0.014 Uiso 1 1 calc R . . . .
N00F N 0.25104(15) 0.75104(15) 1.2268(5) 0.0143(6) Uani 1 2 d S T P . .
O00G O 0.1314(2) 0.3686(2) 0.7342(8) 0.0565(13) Uani 1 2 d S T P . .
H00R H 0.140207 0.410396 0.670988 0.085 Uiso 0.5 1 d G . . . .
H00S H 0.132914 0.382798 0.855371 0.085 Uiso 0.5 1 d G . . . .
C3 C 0.000000 0.500000 0.8124(17) 0.058(3) Uani 1 4 d S T P . .
H3C H 0.003159 0.448102 0.765144 0.087 Uiso 0.25 1 calc GR . . C -1
H3A H 0.043365 0.528685 0.765145 0.087 Uiso 0.25 1 calc GR . . C -1
H3B H -0.046525 0.523213 0.765144 0.087 Uiso 0.25 1 calc GR . . C -1
N4 N 0.000000 0.500000 1.0364(11) 0.0288(14) Uani 1 4 d S T P . .
C1AA C 0.0750(7) 0.5249(12) 1.094(3) 0.094(6) Uani 0.5 1 d . . . . .
C1 C 0.0579(6) 0.4421(6) 1.132(3) 0.062(5) Uani 0.5 2 d S T P . .
H1 H 0.016(4) 0.402(4) 1.065(10) 0.07(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
Ho01 O003 2.300(2) 2_665 ?
Ho01 O003 2.300(2) 4_565 ?
Ho01 O003 2.300(2) 3_655 ?
Ho01 O003 2.300(2) . ?
Ho01 N00B 2.547(2) 3_655 ?
Ho01 N00B 2.547(2) 4_565 ?
Ho01 N00B 2.547(2) . ?
Ho01 N00B 2.547(2) 2_665 ?
O003 C005 1.277(4) . ?
O004 C005 1.238(4) . ?
C005 C00E 1.521(5) . ?
C006 C007 1.518(4) . ?
C006 N00B 1.484(4) . ?
C007 N00B 1.492(4) 4_565 ?
C009 N00F 1.495(4) . ?
C00A N00F 1.496(6) . ?
N00B C00E 1.482(4) . ?
C00D N00F 1.488(6) . ?
C3 N4 1.517(16) . ?
N4 C1AA 1.430(14) 8_455 ?
N4 C1AA 1.430(14) 7 ?
N4 C1AA 1.430(14) 2_565 ?
N4 C1AA 1.431(14) . ?
N4 C1 1.566(16) . ?
N4 C1 1.566(16) 2_565 ?
C1AA C1AA 1.23(3) 8_455 ?
C1AA C1 1.49(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O003 Ho01 O003 77.82(5) 2_665 4_565 ?
O003 Ho01 O003 125.31(11) 4_565 3_655 ?
O003 Ho01 O003 77.82(5) 2_665 3_655 ?
O003 Ho01 O003 77.82(5) 4_565 . ?
O003 Ho01 O003 125.31(11) 2_665 . ?
O003 Ho01 O003 77.82(5) 3_655 . ?
O003 Ho01 N00B 158.08(8) . 2_665 ?
O003 Ho01 N00B 158.08(8) 3_655 4_565 ?
O003 Ho01 N00B 88.75(8) . 3_655 ?
O003 Ho01 N00B 67.07(7) 4_565 4_565 ?
O003 Ho01 N00B 124.04(8) . 4_565 ?
O003 Ho01 N00B 158.07(8) 2_665 . ?
O003 Ho01 N00B 124.04(8) 2_665 3_655 ?
O003 Ho01 N00B 88.75(8) 3_655 2_665 ?
O003 Ho01 N00B 158.08(8) 4_565 3_655 ?
O003 Ho01 N00B 67.07(8) . . ?
O003 Ho01 N00B 124.04(8) 3_655 . ?
O003 Ho01 N00B 88.75(8) 4_565 . ?
O003 Ho01 N00B 67.07(8) 2_665 2_665 ?
O003 Ho01 N00B 88.75(8) 2_665 4_565 ?
O003 Ho01 N00B 124.04(8) 4_565 2_665 ?
O003 Ho01 N00B 67.07(7) 3_655 3_655 ?
N00B Ho01 N00B 69.95(5) 3_655 2_665 ?
N00B Ho01 N00B 69.94(5) 4_565 . ?
N00B Ho01 N00B 108.31(11) 3_655 4_565 ?
N00B Ho01 N00B 108.31(11) 2_665 . ?
N00B Ho01 N00B 69.95(5) 2_665 4_565 ?
N00B Ho01 N00B 69.95(5) 3_655 . ?
C005 O003 Ho01 120.1(2) . . ?
O003 C005 C00E 116.7(3) . . ?
O004 C005 O003 125.4(3) . . ?
O004 C005 C00E 118.0(3) . . ?
N00B C006 C007 111.0(2) . . ?
N00B C007 C006 111.7(2) 4_565 . ?
C006 N00B Ho01 112.43(17) . . ?
C006 N00B C007 109.9(2) . 3_655 ?
C007 N00B Ho01 110.80(17) 3_655 . ?
C00E N00B Ho01 104.59(18) . . ?
C00E N00B C006 110.8(2) . . ?
C00E N00B C007 108.2(2) . 3_655 ?
N00B C00E C005 112.4(3) . . ?
C009 N00F C009 108.1(3) . 8_455 ?
C009 N00F C00A 109.8(2) . . ?
C009 N00F C00A 109.8(2) 8_455 . ?
C00D N00F C009 109.9(2) . 8_455 ?
C00D N00F C009 109.9(2) . . ?
C00D N00F C00A 109.2(4) . . ?
C3 N4 C1 114.4(7) . . ?
C3 N4 C1 114.4(7) . 2_565 ?
C1AA N4 C3 105.9(8) 8_455 . ?
C1AA N4 C3 105.9(8) . . ?
C1AA N4 C3 105.9(8) 2_565 . ?
C1AA N4 C3 105.9(8) 7 . ?
C1AA N4 C1AA 118.6(17) 7 . ?
C1AA N4 C1AA 118.6(17) 8_455 2_565 ?
C1AA N4 C1AA 51.1(16) 7 2_565 ?
C1AA N4 C1AA 51.1(16) 8_455 . ?
C1AA N4 C1AA 148.3(16) 8_455 7 ?
C1AA N4 C1AA 148.3(16) 2_565 . ?
C1AA N4 C1 106.2(8) 8_455 . ?
C1AA N4 C1 106.2(8) . 2_565 ?
C1AA N4 C1 59.6(8) . . ?
C1AA N4 C1 59.6(8) 8_455 2_565 ?
C1AA N4 C1 106.2(8) 2_565 . ?
C1AA N4 C1 59.6(8) 2_565 2_565 ?
C1AA N4 C1 59.6(8) 7 . ?
C1AA N4 C1 106.2(8) 7 2_565 ?
C1 N4 C1 131.2(14) . 2_565 ?
N4 C1AA C1 64.7(9) . . ?
C1AA C1AA N4 64.5(8) 8_455 . ?
C1AA C1AA C1 122.8(8) 8_455 . ?
C1AA C1 N4 55.7(7) 7 . ?
C1AA C1 N4 55.7(7) . . ?
C1AA C1 C1AA 110.8(14) 7 . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_d8v4545_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2281617'
loop_
_audit_author_name
_audit_author_address
'Jesper Bendix'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2023-07-14 deposited with the CCDC.	2023-10-27 downloaded from the CCDC.
;
_audit_creation_date             2021-01-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.5(C16 H24 N4 O8 Tb), Cl, 3(H2 O), C4 H12 N, 0.5(C4 H9 N)'
_chemical_formula_sum            'C14 H34.50 Cl N3.50 O7 Tb0.50'
_chemical_formula_weight         478.86
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
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'
Tb Tb -0.1723 4.1537 '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      tetragonal
_space_group_IT_number           100
_space_group_name_H-M_alt        'P 4 b m'
_space_group_name_Hall           'P 4 -2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   17.4148(6)
_cell_length_b                   17.4148(6)
_cell_length_c                   6.7819(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2056.78(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9748
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      34.810
_cell_measurement_theta_min      3.003
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.917
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6085
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             994
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            51344
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.574
_diffrn_reflns_theta_min         2.339
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3263
_reflns_number_total             3910
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         0.655
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 
;
 Flack x determined using 1381 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3910
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0195
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.093
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0142P)²+0.7700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0414
_refine_ls_wR_factor_ref         0.0439
_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 C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H00J(0.5) H00K(0.5) H00L(0.5) H00M(0.5) H00N(0.5) H00O(0.5)
 H00R(0.5) H00S(0.5) H1B(0.25) H1C(0.25) H1A(0.25) C2(0.25) C4(0.5)
3.a Free rotating group:
 O006(H00P,H00Q), O00H(H00R,H00S)
3.b Secondary CH2 refined with riding coordinates:
 C005(H00A,H00B), C00D(H00C,H00D), C00E(H00E,H00F)
3.c Idealised Me refined as rotating group:
 C007(H00G,H00H,H00I), C008(H00J,H00K,H00L), C00A(H00M,H00N,H00O), C1(H1B,H1C,
 H1A)
;
_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
Tb01 Tb 0.500000 0.500000 0.98463(5) 0.00618(4) Uani 1 4 d S T P . .
Cl02 Cl 0.66395(4) 0.16395(4) 0.72340(16) 0.02238(19) Uani 1 2 d S T P . .
O003 O 0.46919(11) 0.26914(10) 1.2055(3) 0.0169(4) Uani 1 1 d . . . . .
C004 C 0.47273(17) 0.32587(16) 1.0958(4) 0.0105(5) Uani 1 1 d . . . . .
C005 C 0.41661(14) 0.37160(14) 0.6741(4) 0.0108(4) Uani 1 1 d . . . . .
H00A H 0.382506 0.350466 0.773341 0.013 Uiso 1 1 calc R . . . .
H00B H 0.419045 0.335451 0.565503 0.013 Uiso 1 1 calc R . . . .
O006 O 0.49862(14) 0.17089(15) 0.5248(4) 0.0334(7) Uani 1 1 d . . . . .
H00P H 0.496333 0.208699 0.445364 0.050 Uiso 1 1 d G . . . .
H00Q H 0.543441 0.168408 0.573675 0.050 Uiso 1 1 d G . . . .
C007 C 0.26437(15) 0.33373(15) 1.2333(4) 0.0169(5) Uani 1 1 d . . . . .
H00G H 0.240845 0.357288 1.120438 0.025 Uiso 1 1 calc GR . . . .
H00H H 0.318594 0.343643 1.231555 0.025 Uiso 1 1 calc GR . . . .
H00I H 0.242425 0.354660 1.351459 0.025 Uiso 1 1 calc GR . . . .
C008 C 0.28825(18) 0.21175(18) 1.4004(6) 0.0198(8) Uani 1 2 d S T P . .
H00J H 0.343026 0.215074 1.386930 0.030 Uiso 0.5 1 calc GR . . A -1
H00K H 0.273195 0.158767 1.406260 0.030 Uiso 0.5 1 calc GR . . A -1
H00L H 0.272645 0.237293 1.519273 0.030 Uiso 0.5 1 calc GR . . A -1
N009 N 0.49486(11) 0.38097(11) 0.7604(3) 0.0086(3) Uani 1 1 d . . . . .
C00A C 0.28372(18) 0.21628(18) 1.0420(6) 0.0192(8) Uani 1 2 d S T P . .
H00M H 0.259391 0.239652 0.930020 0.029 Uiso 0.5 1 calc GR . . B -1
H00N H 0.274963 0.161867 1.039285 0.029 Uiso 0.5 1 calc GR . . B -1
H00O H 0.337914 0.226212 1.037655 0.029 Uiso 0.5 1 calc GR . . B -1
N00B N 0.500000 0.000000 1.0375(9) 0.0256(12) Uani 1 4 d S T P . .
O00C O 0.44804(10) 0.39285(10) 1.1378(3) 0.0102(3) Uani 1 1 d . . . . .
C00D C 0.55298(14) 0.38410(14) 0.6005(4) 0.0108(4) Uani 1 1 d . . . . .
H00C H 0.533813 0.415825 0.493764 0.013 Uiso 1 1 calc R . . . .
H00D H 0.561400 0.332794 0.549195 0.013 Uiso 1 1 calc R . . . .
C00E C 0.50980(16) 0.31535(16) 0.8931(4) 0.0114(5) Uani 1 1 d . . . . .
H00E H 0.564805 0.309261 0.909370 0.014 Uiso 1 1 calc R . . . .
H00F H 0.490048 0.268819 0.833040 0.014 Uiso 1 1 calc R . . . .
N00F N 0.25078(12) 0.24922(12) 1.2275(5) 0.0140(5) Uani 1 2 d S T P . .
O00H O 0.36802(18) 0.13198(18) 0.7351(7) 0.0507(10) Uani 1 2 d S T P . .
H00R H 0.386387 0.135050 0.853563 0.076 Uiso 0.5 1 d G . . . .
H00S H 0.407750 0.141451 0.665938 0.076 Uiso 0.5 1 d G . . . .
C1 C 0.500000 0.000000 0.8160(14) 0.054(3) Uani 1 4 d S T P . .
H1B H 0.451601 0.018941 0.768781 0.080 Uiso 0.25 1 calc GR . . C -1
H1C H 0.507796 -0.051385 0.768781 0.080 Uiso 0.25 1 calc GR . . C -1
H1A H 0.540602 0.032444 0.768782 0.080 Uiso 0.25 1 calc GR . . C -1
C2 C 0.4420(6) 0.0580(6) 1.128(2) 0.061(4) Uani 0.5 2 d S T P . .
C4 C 0.5249(11) 0.0758(6) 1.095(2) 0.090(5) Uani 0.5 1 d . . . . .
H2A H 0.459(6) 0.041(6) 1.28(2) 0.22(6) Uiso 1 2 d S T P . .
H2B H 0.397(5) 0.014(4) 1.070(12) 0.13(4) 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
Tb01 N009 2.573(2) . ?
Tb01 N009 2.573(2) 4_565 ?
Tb01 N009 2.573(2) 3_655 ?
Tb01 N009 2.573(2) 2_665 ?
Tb01 O00C 2.3194(17) 2_665 ?
Tb01 O00C 2.3194(17) 3_655 ?
Tb01 O00C 2.3194(17) 4_565 ?
Tb01 O00C 2.3195(17) . ?
O003 C004 1.238(3) . ?
C004 O00C 1.275(3) . ?
C004 C00E 1.530(4) . ?
C005 N009 1.492(3) . ?
C005 C00D 1.515(4) 4_565 ?
C007 N00F 1.491(3) . ?
C008 N00F 1.492(5) . ?
N009 C00D 1.484(3) . ?
N009 C00E 1.478(3) . ?
C00A N00F 1.497(5) . ?
N00B C1 1.503(13) . ?
N00B C2 1.555(14) 2_655 ?
N00B C2 1.556(14) . ?
N00B C4 1.444(10) 7 ?
N00B C4 1.444(10) 8_545 ?
N00B C4 1.444(10) . ?
N00B C4 1.444(10) 2_655 ?
C2 C4 1.49(2) 7 ?
C2 C4 1.49(2) . ?
C4 C4 1.25(3) 8_545 ?

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
N009 Tb01 N009 69.54(5) . 4_565 ?
N009 Tb01 N009 69.54(5) 2_665 3_655 ?
N009 Tb01 N009 69.54(5) . 3_655 ?
N009 Tb01 N009 69.54(5) 4_565 2_665 ?
N009 Tb01 N009 107.52(9) . 2_665 ?
N009 Tb01 N009 107.52(9) 4_565 3_655 ?
O00C Tb01 N009 123.44(6) 2_665 4_565 ?
O00C Tb01 N009 123.44(6) 3_655 2_665 ?
O00C Tb01 N009 66.60(6) 2_665 2_665 ?
O00C Tb01 N009 66.60(6) 3_655 3_655 ?
O00C Tb01 N009 157.91(6) 2_665 . ?
O00C Tb01 N009 123.44(6) . 3_655 ?
O00C Tb01 N009 88.76(6) 3_655 . ?
O00C Tb01 N009 66.60(6) 4_565 4_565 ?
O00C Tb01 N009 123.44(6) 4_565 . ?
O00C Tb01 N009 88.76(6) 2_665 3_655 ?
O00C Tb01 N009 66.60(6) . . ?
O00C Tb01 N009 157.91(6) 3_655 4_565 ?
O00C Tb01 N009 88.76(6) 4_565 2_665 ?
O00C Tb01 N009 88.76(6) . 4_565 ?
O00C Tb01 N009 157.91(6) 4_565 3_655 ?
O00C Tb01 N009 157.91(6) . 2_665 ?
O00C Tb01 O00C 126.79(9) 2_665 . ?
O00C Tb01 O00C 78.43(4) 4_565 . ?
O00C Tb01 O00C 78.43(4) 3_655 . ?
O00C Tb01 O00C 126.79(9) 3_655 4_565 ?
O00C Tb01 O00C 78.43(4) 2_665 4_565 ?
O00C Tb01 O00C 78.43(4) 2_665 3_655 ?
O003 C004 O00C 125.4(3) . . ?
O003 C004 C00E 117.7(2) . . ?
O00C C004 C00E 116.9(2) . . ?
N009 C005 C00D 112.07(19) . 4_565 ?
C005 N009 Tb01 110.59(14) . . ?
C00D N009 Tb01 112.24(13) . . ?
C00D N009 C005 109.91(18) . . ?
C00E N009 Tb01 104.88(15) . . ?
C00E N009 C005 108.37(19) . . ?
C00E N009 C00D 110.68(19) . . ?
C1 N00B C2 113.2(6) . . ?
C1 N00B C2 113.2(6) . 2_655 ?
C2 N00B C2 133.5(12) 2_655 . ?
C4 N00B C1 105.6(7) 8_545 . ?
C4 N00B C1 105.6(7) . . ?
C4 N00B C1 105.6(7) 2_655 . ?
C4 N00B C1 105.6(7) 7 . ?
C4 N00B C2 59.7(7) 8_545 2_655 ?
C4 N00B C2 59.7(7) 7 . ?
C4 N00B C2 107.0(7) 8_545 . ?
C4 N00B C2 59.7(7) . . ?
C4 N00B C2 107.0(7) 7 2_655 ?
C4 N00B C2 59.7(7) 2_655 2_655 ?
C4 N00B C2 107.0(7) . 2_655 ?
C4 N00B C2 107.0(7) 2_655 . ?
C4 N00B C4 118.5(14) 8_545 2_655 ?
C4 N00B C4 51.5(14) 8_545 . ?
C4 N00B C4 148.7(13) 8_545 7 ?
C4 N00B C4 148.7(13) 2_655 . ?
C4 N00B C4 51.5(14) 7 2_655 ?
C4 N00B C4 118.5(14) 7 . ?
C004 O00C Tb01 120.28(16) . . ?
N009 C00D C005 111.36(19) . 3_655 ?
N009 C00E C004 112.4(2) . . ?
C007 N00F C007 108.2(3) . 7 ?
C007 N00F C008 110.0(2) 7 . ?
C007 N00F C008 110.0(2) . . ?
C007 N00F C00A 109.8(2) . . ?
C007 N00F C00A 109.8(2) 7 . ?
C008 N00F C00A 109.0(3) . . ?
C4 C2 N00B 56.5(6) 7 . ?
C4 C2 N00B 56.5(6) . . ?
C4 C2 C4 112.2(12) 7 . ?
N00B C4 C2 63.9(7) . . ?
C4 C4 N00B 64.3(7) 8_545 . ?
C4 C4 C2 122.5(6) 8_545 . ?

_olex2_submission_original_sample_id D8V4545
_olex2_submission_special_instructions 'No special instructions were received'
