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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_sq
_database_code_depnum_ccdc_archive 'CCDC 1843640'
_audit_update_record             
;
2018-05-16 deposited with the CCDC.
2018-08-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H15 Er0.60 O12.50 Yb0.90'
_chemical_formula_weight         699.39

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'
Er Er -0.2586 4.9576 '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'
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      orthorhombic
_space_group_IT_number           72
_space_group_name_H-M_alt        'I b a m'
_space_group_name_Hall           '-I 2 2c'

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

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

_cell_length_a                   23.106(3)
_cell_length_b                   11.6464(14)
_cell_length_c                   18.610(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5008.1(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    6463
_cell_measurement_theta_min      2.1888
_cell_measurement_theta_max      28.0101

_exptl_crystal_description       Block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_F_000             2662
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    5.405
_shelx_estimated_absorpt_T_min   0.345
_shelx_estimated_absorpt_T_max   0.369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_process_details   
;
SADABS - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21006
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.811
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3214
_reflns_number_gt                2195
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0690P)²+123.2903P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00019(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3214
_refine_ls_number_parameters     175
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0547
_refine_ls_wR_factor_ref         0.1539
_refine_ls_wR_factor_gt          0.1316
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Er1 Er 0.18590(2) 0.16858(5) 0.0000 0.0329(2) Uani 0.4016 2 d S T P A 1
Er2 Er 0.0000 0.0000 0.2500 0.0539(3) Uani 0.4016 4 d S T P A 1
Yb1 Yb 0.18590(2) 0.16858(5) 0.0000 0.0329(2) Uani 0.5984 2 d S T P A 1
Yb2 Yb 0.0000 0.0000 0.2500 0.0539(3) Uani 0.5984 4 d S T P A 1
O1 O 0.0667(3) 0.0338(6) 0.1649(3) 0.0427(16) Uani 1 1 d . . . A 1
O2 O 0.1239(3) 0.1180(7) 0.0871(3) 0.0470(17) Uani 1 1 d . . . A 1
O3 O 0.2601(3) 0.1345(6) 0.0874(4) 0.0478(17) Uani 1 1 d . . . A 1
O4 O 0.2255(4) 0.3056(6) 0.0768(4) 0.059(2) Uani 1 1 d . . . A 1
O6 O 0.1175(6) 0.3143(10) 0.0000 0.071(3) Uani 1 2 d S T P A 1
O7 O 0.1946(5) -0.0300(8) 0.0000 0.055(3) Uani 1 2 d S T P A 1
C4 C 0.2932(4) 0.2778(8) 0.1710(5) 0.036(2) Uani 1 1 d . . . A 1
C7 C 0.1096(4) 0.0942(8) 0.1507(5) 0.0349(19) Uani 1 1 d . . . A 1
C1 C 0.1452(4) 0.1400(8) 0.2117(4) 0.0307(18) Uani 1 1 d . . . A 1
C8 C 0.2584(4) 0.2384(8) 0.1080(5) 0.036(2) Uani 1 1 d . . . A 1
C5 C 0.2956(4) 0.3954(8) 0.1845(4) 0.0331(18) Uani 1 1 d . . . A 1
H5 H 0.2764 0.4460 0.1540 0.040 Uiso 1 1 calc R U . A 1
C6 C 0.1735(3) 0.0617(7) 0.2569(5) 0.0287(17) Uani 1 1 d . . . A 1
C2 C 0.1488(4) 0.2577(8) 0.2248(5) 0.041(2) Uani 1 1 d . . . A 1
H2 H 0.1309 0.3095 0.1940 0.049 Uiso 1 1 calc R U . A 1
C3 C 0.3207(4) 0.2028(8) 0.2158(5) 0.041(2) Uani 1 1 d . . . A 1
H3 H 0.3189 0.1244 0.2066 0.049 Uiso 1 1 calc R U . A 1
C12 C 0.1847(7) -0.1703(15) 0.0000 0.058(4) Uani 1 2 d S T P A 1
H12A H 0.1891 -0.1993 0.0480 0.087 Uiso 0.5 1 calc R U P A 1
H12B H 0.2128 -0.2058 -0.0309 0.087 Uiso 0.5 1 calc R U P A 1
H12C H 0.1465 -0.1874 -0.0171 0.087 Uiso 0.5 1 calc R U P A 1
O5 O 0.0257(6) 0.1868(12) 0.3003(8) 0.052(4) Uani 0.5 1 d . U P B 2
C9 C 0.0000 0.232(3) 0.2500 0.063(6) Uani 0.5 2 d DS TU P B 2
C10 C 0.0000 0.363(3) 0.2500 0.070(6) Uani 0.5 2 d DS TU P B 2
C11 C 0.0044(13) 0.438(2) 0.3132(16) 0.082(6) Uani 0.5 1 d . U P B 2
H11 H 0.0136 0.4032 0.3569 0.099 Uiso 0.5 1 calc R U P B 2
O1W O 0.3633(7) 0.0038(17) 0.0911(13) 0.091(7) Uani 0.5 1 d . . P C 2


_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
Er1 O2 2.242(6) 10 ?
Er1 O2 2.242(6) . ?
Er1 O6 2.319(13) . ?
Er1 O7 2.322(10) . ?
Er1 O4 2.330(7) 10 ?
Er1 O4 2.330(7) . ?
Er1 O3 2.397(7) . ?
Er1 O3 2.397(7) 10 ?
Er1 C8 2.740(9) . ?
Er1 C8 2.740(9) 10 ?
Er2 O1 2.245(6) 2 ?
Er2 O1 2.245(6) 8_445 ?
Er2 O1 2.245(6) 7_445 ?
Er2 O1 2.245(6) . ?
O1 C7 1.244(11) . ?
O2 C7 1.261(10) . ?
O3 C8 1.270(11) . ?
O4 C8 1.235(12) . ?
O7 C12 1.649(19) . ?
C4 C3 1.366(13) . ?
C4 C5 1.393(13) . ?
C4 C8 1.494(12) . ?
C7 C1 1.499(12) . ?
C1 C2 1.395(13) . ?
C1 C6 1.403(12) . ?
C5 C6 1.396(12) 13 ?
C6 C5 1.396(12) 13 ?
C6 C6 1.460(16) 8_445 ?
C2 C3 1.388(13) 13 ?
C3 C2 1.388(13) 13 ?
O5 C9 1.23(2) . ?
C9 O5 1.23(2) 7_445 ?
C9 C10 1.517(19) . ?
C10 C11 1.47(3) 7_445 ?
C10 C11 1.47(3) . ?
C11 C11 1.47(5) 2_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Er1 O2 92.6(3) 10 . ?
O2 Er1 O6 75.9(3) 10 . ?
O2 Er1 O6 75.9(3) . . ?
O2 Er1 O7 78.1(3) 10 . ?
O2 Er1 O7 78.1(3) . . ?
O6 Er1 O7 142.0(4) . . ?
O2 Er1 O4 89.3(3) 10 10 ?
O2 Er1 O4 151.0(3) . 10 ?
O6 Er1 O4 76.5(3) . 10 ?
O7 Er1 O4 130.4(3) . 10 ?
O2 Er1 O4 151.0(3) 10 . ?
O2 Er1 O4 89.3(3) . . ?
O6 Er1 O4 76.5(3) . . ?
O7 Er1 O4 130.4(3) . . ?
O4 Er1 O4 75.7(4) 10 . ?
O2 Er1 O3 154.7(3) 10 . ?
O2 Er1 O3 85.6(3) . . ?
O6 Er1 O3 127.5(2) . . ?
O7 Er1 O3 76.9(3) . . ?
O4 Er1 O3 104.4(3) 10 . ?
O4 Er1 O3 54.3(2) . . ?
O2 Er1 O3 85.6(3) 10 10 ?
O2 Er1 O3 154.7(3) . 10 ?
O6 Er1 O3 127.5(2) . 10 ?
O7 Er1 O3 76.9(3) . 10 ?
O4 Er1 O3 54.3(2) 10 10 ?
O4 Er1 O3 104.4(3) . 10 ?
O3 Er1 O3 85.5(4) . 10 ?
O2 Er1 C8 177.4(3) 10 . ?
O2 Er1 C8 86.5(3) . . ?
O6 Er1 C8 101.5(3) . . ?
O7 Er1 C8 104.1(3) . . ?
O4 Er1 C8 90.3(3) 10 . ?
O4 Er1 C8 26.7(3) . . ?
O3 Er1 C8 27.6(3) . . ?
O3 Er1 C8 96.2(3) 10 . ?
O2 Er1 C8 86.5(3) 10 10 ?
O2 Er1 C8 177.4(3) . 10 ?
O6 Er1 C8 101.5(3) . 10 ?
O7 Er1 C8 104.1(3) . 10 ?
O4 Er1 C8 26.7(3) 10 10 ?
O4 Er1 C8 90.3(3) . 10 ?
O3 Er1 C8 96.3(3) . 10 ?
O3 Er1 C8 27.6(3) 10 10 ?
C8 Er1 C8 94.3(4) . 10 ?
O1 Er2 O1 159.8(4) 2 8_445 ?
O1 Er2 O1 93.3(3) 2 7_445 ?
O1 Er2 O1 90.3(3) 8_445 7_445 ?
O1 Er2 O1 90.3(3) 2 . ?
O1 Er2 O1 93.3(3) 8_445 . ?
O1 Er2 O1 159.8(4) 7_445 . ?
C7 O1 Er2 142.7(6) . . ?
C7 O2 Er1 154.7(6) . . ?
C8 O3 Er1 91.4(6) . . ?
C8 O4 Er1 95.5(5) . . ?
C12 O7 Er1 167.1(10) . . ?
C3 C4 C5 120.0(8) . . ?
C3 C4 C8 122.2(9) . . ?
C5 C4 C8 117.7(8) . . ?
O1 C7 O2 122.1(8) . . ?
O1 C7 C1 118.6(8) . . ?
O2 C7 C1 119.3(8) . . ?
C2 C1 C6 120.4(8) . . ?
C2 C1 C7 121.0(8) . . ?
C6 C1 C7 118.6(8) . . ?
O4 C8 O3 118.7(8) . . ?
O4 C8 C4 120.3(8) . . ?
O3 C8 C4 120.8(9) . . ?
O4 C8 Er1 57.8(5) . . ?
O3 C8 Er1 61.0(5) . . ?
C4 C8 Er1 174.8(7) . . ?
C4 C5 C6 120.9(8) . 13 ?
C5 C6 C1 118.3(8) 13 . ?
C5 C6 C6 119.3(8) 13 8_445 ?
C1 C6 C6 122.4(9) . 8_445 ?
C3 C2 C1 119.7(9) 13 . ?
C4 C3 C2 120.7(9) . 13 ?
O5 C9 O5 129(3) 7_445 . ?
O5 C9 C10 115.5(15) 7_445 . ?
O5 C9 C10 115.5(15) . . ?
C11 C10 C11 107(3) 7_445 . ?
C11 C10 C9 126.5(15) 7_445 . ?
C11 C10 C9 126.5(15) . . ?
C11 C11 C10 125.4(17) 2_565 . ?

_refine_diff_density_max         2.139
_refine_diff_density_min         -2.289
_refine_diff_density_rms         0.216

# start Validation Reply Form

_vrf_CHEMW03_1_sq                
;
PROBLEM: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.99 <> 1.01
RESPONSE: Half of additional H2O estimated from PLATON
squeeze and TGA experiment, H atoms on coordinated H2O and CH3OH
that can not be properly added were included in the molecular formula directly.
;
# end Validation Reply Form



