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

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

data_Sc_NH4_ox2
_database_code_depnum_ccdc_archive 'CCDC 1963550'
loop_
_audit_author_name
_audit_author_address
'Igor Huskic'
;McGill University
Canada
;
_audit_update_record             
;
2019-11-04 deposited with the CCDC.	2020-05-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT699_Sc_NH4_ox2          
;
PROBLEM: Missing _exptl_crystal_description Value .......     Please Do !
RESPONSE: Structure solved from powder data
;
_vrf_PLAT306_Sc_NH4_ox2          
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O5 Check
RESPONSE: Structure solved from powder data, insufficient information for modelling H atoms
;
# Added during the CSD deposition process: Monday 04 November 2019 03:30 PM
# end Validation Reply Form


_chemical_name_systematic        
; ?
;
_chemical_name_common            
'catena-(ammonium bis(m2-oxalato)-scandium dihydrate)'
_chemical_formula_moiety         'C4 O8 Sc, 2(O), (N)'
_chemical_formula_analytical     ?
_chemical_formula_sum            'C4 N O10 Sc1'
_chemical_formula_weight         267.00


#==============================================================================

# POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      hexagonal
_symmetry_space_group_name_H-M   'P 62 2 2'
_space_group_name_Hall           'P 62 2c (0 0 1)'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z '
'-x, -y, z '
'-x+y, -x, z+1/3 '
'-x+y, y, -z '
'-y, -x, -z-1/3 '
'-y, x-y, z-1/3 '
'y, -x+y, z-1/3 '
'y, x, -z-1/3 '
'x-y, -y, -z '
'x-y, x, z+1/3 '
'-x, -x+y, -z+1/3 '
'x, x-y, -z+1/3 '

_cell_length_a                   9.0093(2)
_cell_length_b                   9.0093(2)
_cell_length_c                   11.2503(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     790.81(5)

_cell_formula_units_Z            3
_cell_measurement_temperature    293
_cell_measurement_theta_min      4
_cell_measurement_theta_max      80
_cell_measurement_reflns_used    20
_exptl_crystal_density_diffrn    1.6819(1)
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             396

_cell_special_details            
; ?
;



# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
; 'packed powder pellet'
;
_pd_spec_mount_mode              resflection

_pd_spec_shape                   flat_sheet

_pd_char_particle_morphology     ?
_pd_char_colour                  white # use ICDD colour descriptions



_pd_prep_temperature             293


#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      293
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              ?
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_source_voltage           40
_diffrn_source_current           30
_diffrn_measurement_device_type  'Bruker D2 PHASER'
_diffrn_detector                 'Position Sensitive Detector'
_diffrn_detector_type            LYNXEYE
_pd_meas_scan_method             cont

_pd_meas_special_details         
;  ?
;

# The following six items are used for angular dispersive measurements only.

_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_monochromator  none

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        3822
_pd_meas_2theta_range_min        4.010
_pd_meas_2theta_range_max        80.0043
_pd_meas_2theta_range_inc        0.0199




#==============================================================================

# REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.


# The next three items are given as text.

_pd_proc_ls_profile_function     pseudo-Voigt
_pd_proc_ls_background_function  'Chebyshev polynomial'


_pd_proc_ls_prof_R_factor        0.051
_pd_proc_ls_prof_wR_factor       0.064
_pd_proc_ls_prof_wR_expected     0.007
_refine_ls_R_I_factor            0.029


_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_parameters     27
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   9.801


# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        9
_pd_proc_2theta_range_max        80
_pd_proc_2theta_range_inc        0.0199
_pd_proc_wavelength              1.5418

#


# The following items are used to identify the programs used.

_computing_data_collection       'Bruker DIFFRAC.SUITE'
_computing_cell_refinement       'TOPAS Academic v. 6'
_computing_structure_solution    'TOPAS Academic v. 6'
_computing_structure_refinement  'TOPAS Academic v. 6'
_computing_molecular_graphics    ?
_computing_publication_material  ?


#==============================================================================


# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
O1 O 12 -0.6575(4) -0.9286(4) -0.8969(3) 1 1.15(7)
O3 O 12 -0.3167(5) -0.5563(4) -0.7748(3) 1 1.15(7)
C1 C 6 -0.5941(10) -0.7971(5) -0.8333333 1 1.15(7)
C2 C 6 -0.3953(12) -0.6976(6) -0.8333333 1 1.15(7)
Sc1 Sc 3 -0.5 -1 -1 1 0.95(7)
O5 O 6 0 -0.7591(7) 0.1666667 1 1.93(13)
N1 N 3 0 0 -0.6666667 1 1.93(13)
#==============================================================================

# BOND LENGTHS AND ANGLES

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
Sc1 O1 2.165(4) . ?
Sc1 O3 2.302(4) 6_445 ?
Sc1 O1 2.165(4) 2_435 ?
Sc1 O3 2.302(4) 7_545 ?
Sc1 O1 2.165(5) 9_433 ?
Sc1 O3 2.302(4) 12_543 ?
Sc1 O1 2.165(5) 4_553 ?
Sc1 O3 2.302(4) 11_443 ?
O1 C1 1.251(5) . ?
O3 C2 1.287(5) . ?
C1 C2 1.551(13) . ?


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 Sc1 O3 82.78(13) . 6_445 ?
O1 Sc1 O1 115.20(13) . 2_435 ?
O1 Sc1 O3 133.77(14) . 7_545 ?
O1 Sc1 O1 72.95(15) . 9_433 ?
O1 Sc1 O3 73.01(15) . 12_543 ?
O1 Sc1 O1 150.17(12) . 4_553 ?
O1 Sc1 O3 74.10(15) . 11_443 ?
O1 Sc1 O3 133.77(14) 2_435 6_445 ?
O3 Sc1 O3 116.23(13) 6_445 7_545 ?
O1 Sc1 O3 74.10(14) 9_433 6_445 ?
O3 Sc1 O3 71.43(14) 6_445 12_543 ?
O1 Sc1 O3 73.01(15) 4_553 6_445 ?
O3 Sc1 O3 151.23(17) 6_445 11_443 ?
O1 Sc1 O3 82.78(13) 2_435 7_545 ?
O1 Sc1 O1 150.17(12) 2_435 9_433 ?
O1 Sc1 O3 74.10(15) 2_435 12_543 ?
O1 Sc1 O1 72.95(15) 2_435 4_553 ?
O1 Sc1 O3 73.01(15) 2_435 11_443 ?
O1 Sc1 O3 73.01(15) 9_433 7_545 ?
O3 Sc1 O3 151.23(17) 7_545 12_543 ?
O1 Sc1 O3 74.10(14) 4_553 7_545 ?
O3 Sc1 O3 71.43(14) 7_545 11_443 ?
O1 Sc1 O3 133.77(16) 9_433 12_543 ?
O1 Sc1 O1 115.20(15) 9_433 4_553 ?
O1 Sc1 O3 82.78(14) 9_433 11_443 ?
O1 Sc1 O3 82.78(14) 4_553 12_543 ?
O3 Sc1 O3 116.23(13) 12_543 11_443 ?
O1 Sc1 O3 133.77(16) 4_553 11_443 ?
Sc1 O1 C1 122.1(5) . . ?
Sc1 O3 C2 112.8(5) 10_455 . ?
O1 C1 C2 113.3(6) . . ?
O1 C1 O1 133.4(7) . 12_543 ?
O1 C1 C2 113.3(4) 12_543 . ?
O3 C2 C1 118.5(7) . . ?
O3 C2 O3 123.1(8) . 12_543 ?
O3 C2 C1 118.5(4) 12_543 . ?
_exptl_crystal_colour            colourless
_exptl_crystal_recrystallization_method 'accelerated ageing'
####################################################################### 
# 
# 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_Na3ScOx3
_database_code_depnum_ccdc_archive 'CCDC 1963557'
loop_
_audit_author_name
_audit_author_address
'Igor Huskic'
;McGill University
Canada
;
_audit_update_record             
;
2019-11-04 deposited with the CCDC.	2020-05-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        'Sodium scandium oxalate hexahydrate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H10 Na3 O18 Sc'
_chemical_compound_source        synthetic
_exptl_crystal_recrystallization_method water
_exptl_crystal_description       'monoclinic block'
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      253

_chemical_formula_weight         484.07

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

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

_cell_length_a                   17.851(2)
_cell_length_b                   11.0413(7)
_cell_length_c                   18.2806(13)
_cell_angle_alpha                90
_cell_angle_beta                 104.189(2)
_cell_angle_gamma                90
_cell_volume                     3493.1(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    253(2)
_cell_measurement_reflns_used    19296
_cell_measurement_theta_min      5.005
_cell_measurement_theta_max      55.006

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_F_000             1952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.588
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6898
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS-2012/1, G. Sheldrick'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed x-ray tube'
_diffrn_measurement_device_type  'Bruker PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44915
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.859
_diffrn_reflns_theta_max         37.082
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             8442
_reflns_number_gt                6528
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX 2, Bruker-AXS'
_computing_cell_refinement       'SAINT V8.35A, Bruker-AXS'
_computing_data_reduction        'SAINT V8.35A, Bruker-AXS'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0420P)²+2.4056P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8442
_refine_ls_number_parameters     300
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.0915
_refine_ls_wR_factor_gt          0.0829
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.032
_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
Sc01 Sc 0.47254(2) 0.36689(2) 0.29198(2) 0.00966(4) Uani 1 1 d . . . . .
Na1 Na 0.15053(3) 0.29588(5) 0.11092(3) 0.02043(9) Uani 1 1 d . . . . .
C1 C 0.33026(6) 0.35168(10) 0.16249(6) 0.01624(18) Uani 1 1 d . . . . .
O1 O 0.40336(5) 0.34891(9) 0.17713(5) 0.02222(17) Uani 1 1 d . . . . .
C2 C 0.29691(6) 0.37435(9) 0.23161(6) 0.01428(16) Uani 1 1 d . . . . .
O2 O 0.34767(4) 0.37524(7) 0.29404(4) 0.01532(13) Uani 1 1 d . . . . .
Na2 Na 0.250000 0.49124(8) 0.000000 0.03338(17) Uani 1 2 d S T P B .
Na3 Na 0.35994(3) 0.55890(6) 0.38418(3) 0.02982(12) Uani 1 1 d . . . . .
C3 C 0.52641(5) 0.59464(8) 0.22244(5) 0.01201(15) Uani 1 1 d . . . . .
O3 O 0.28531(5) 0.33700(9) 0.09957(5) 0.02475(17) Uani 1 1 d . . . . .
C4 C 0.47033(5) 0.63881(8) 0.26798(5) 0.01186(15) Uani 1 1 d . . . . .
O4 O 0.22664(5) 0.38920(9) 0.22297(5) 0.02450(18) Uani 1 1 d . . . . .
Na4 Na 0.750000 0.54294(7) 0.500000 0.02344(14) Uani 1 2 d S T P . .
C5 C 0.59286(6) 0.38222(9) 0.44162(6) 0.01577(17) Uani 1 1 d . . . . .
O5 O 0.53961(5) 0.48351(7) 0.22513(5) 0.01828(15) Uani 1 1 d . . . . .
O7 O 0.55201(4) 0.67441(6) 0.18613(4) 0.01637(14) Uani 1 1 d . . . . .
O8 O 0.45423(4) 0.74892(6) 0.26414(5) 0.01672(14) Uani 1 1 d . . . . .
O6 O 0.44464(5) 0.55916(6) 0.30424(4) 0.01684(14) Uani 1 1 d . . . . .
C6 C 0.51547(6) 0.36901(8) 0.46422(5) 0.01296(16) Uani 1 1 d . . . . .
O9 O 0.58681(5) 0.37842(8) 0.37092(5) 0.02161(16) Uani 1 1 d . . . . .
O10 O 0.45686(4) 0.36562(7) 0.40871(4) 0.01589(14) Uani 1 1 d . . . . .
O11 O 0.51510(5) 0.36286(8) 0.53186(4) 0.01973(15) Uani 1 1 d . . . . .
O12 O 0.65315(5) 0.39512(10) 0.49140(5) 0.02590(18) Uani 1 1 d . . . . .
O13 O 0.84929(5) 0.68741(9) 0.50761(5) 0.02442(17) Uani 1 1 d G . . . .
H13A H 0.896814 0.669073 0.522881 0.036(5) Uiso 1 1 d G . . . .
H13B H 0.840144 0.731635 0.542488 0.042(5) Uiso 1 1 d G . . . .
O15 O 0.22645(5) 0.49880(10) 0.36319(5) 0.0313(2) Uani 1 1 d G . . . .
H15A H 0.220461 0.463827 0.320727 0.056(6) Uiso 1 1 d G . . . .
H15B H 0.185354 0.539868 0.359147 0.049(6) Uiso 1 1 d G . . . .
O14A O 0.18888(10) 0.7497(2) 0.18405(10) 0.0440(6) Uani 0.742(5) 1 d G U P A 1
H14A H 0.152043 0.723511 0.201615 0.066 Uiso 0.742(5) 1 d G U P A 1
H14B H 0.225544 0.762399 0.222796 0.066 Uiso 0.742(5) 1 d G U P A 1
O14B O 0.1854(3) 0.6605(6) 0.1982(3) 0.0481(19) Uani 0.258(5) 1 d G U P A 2
H14C H 0.206229 0.693127 0.165950 0.072 Uiso 0.258(5) 1 d G U P A 2
H14D H 0.138083 0.680441 0.184073 0.072 Uiso 0.258(5) 1 d G U P A 2
O16 O 0.12047(6) 0.46487(10) 0.02150(7) 0.0364(2) Uani 1 1 d G . . B 2
H16A H 0.084625 0.436497 -0.013855 0.057(7) Uiso 1 1 d G . . B 2
H16B H 0.098518 0.519280 0.041757 0.058(7) Uiso 1 1 d G . . B 2
O17 O 0.52332(8) 0.11724(10) 0.57707(6) 0.0399(3) Uani 1 1 d G . . C 2
H17A H 0.524601 0.193336 0.570435 0.069(7) Uiso 1 1 d G . . C 2
H17B H 0.529697 0.108954 0.624436 0.088(9) Uiso 1 1 d G . . C 2
O18A O 0.2951(5) 0.6324(9) 0.1102(7) 0.060(2) Uani 0.413(19) 1 d . U P B 1
O18B O 0.2683(5) 0.6691(6) 0.0741(6) 0.073(2) Uani 0.587(19) 1 d . U P B 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
Sc01 O1 2.1682(8) . ?
Sc01 O9 2.1946(8) . ?
Sc01 O6 2.2045(7) . ?
Sc01 O10 2.2192(8) . ?
Sc01 O7 2.2259(7) 4_545 ?
Sc01 O2 2.2406(8) . ?
Sc01 O8 2.2616(7) 4_545 ?
Sc01 O5 2.3026(8) . ?
Sc01 Na3 3.6106(6) . ?
Sc01 Na1 3.6221(5) 7 ?
Na1 O4 2.3957(10) . ?
Na1 O16 2.4518(12) . ?
Na1 O13 2.4763(11) 4_545 ?
Na1 O7 2.5054(8) 6_565 ?
Na1 O3 2.5065(10) . ?
Na1 O2 2.5617(9) 7 ?
Na1 O10 2.5780(9) 7 ?
Na1 C2 3.1016(11) . ?
Na1 Na2 3.6989(7) . ?
Na1 Na3 3.9237(8) 7 ?
Na1 Na4 4.1023(7) 3_444 ?
C1 O3 1.2413(13) . ?
C1 O1 1.2665(13) . ?
C1 C2 1.5434(14) . ?
C2 O4 1.2362(12) . ?
C2 O2 1.2715(12) . ?
O2 Na3 2.5880(9) . ?
Na2 O18B 2.362(4) . ?
Na2 O18B 2.362(4) 2 ?
Na2 O16 2.4558(11) . ?
Na2 O16 2.4559(11) 2 ?
Na2 O3 2.4592(11) 2 ?
Na2 O3 2.4593(11) . ?
Na2 O18A 2.519(6) 2 ?
Na2 O18A 2.519(6) . ?
Na3 O6 2.3462(9) . ?
Na3 O12 2.3971(10) 5_666 ?
Na3 O15 2.4120(11) . ?
Na3 O14A 2.500(2) 7_565 ?
Na3 O11 2.5298(10) 5_666 ?
Na3 O10 2.7145(10) . ?
Na3 Na4 3.4111(6) 5_666 ?
C3 O5 1.2481(12) . ?
C3 O7 1.2546(11) . ?
C3 C4 1.5303(13) . ?
C4 O8 1.2473(11) . ?
C4 O6 1.2537(11) . ?
Na4 O12 2.3547(10) . ?
Na4 O12 2.3547(10) 2_656 ?
Na4 O13 2.3631(10) . ?
Na4 O13 2.3631(10) 2_656 ?
Na4 O15 2.4756(10) 6_665 ?
Na4 O15 2.4756(10) 5_666 ?
Na4 H13B 2.6307 . ?
C5 O12 1.2355(13) . ?
C5 O9 1.2710(13) . ?
C5 C6 1.5427(14) . ?
C6 O11 1.2399(12) . ?
C6 O10 1.2671(12) . ?
O13 H13A 0.8500 . ?
O13 H13B 0.8501 . ?
O15 H15A 0.8500 . ?
O15 H15B 0.8501 . ?
O14A H14A 0.8500 . ?
O14A H14B 0.8501 . ?
O14B H14C 0.8500 . ?
O14B H14D 0.8500 . ?
O16 H16A 0.8500 . ?
O16 H16B 0.8501 . ?
O17 H17A 0.8500 . ?
O17 H17B 0.8501 . ?

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 Sc01 O9 149.21(3) . . ?
O1 Sc01 O6 95.59(3) . . ?
O9 Sc01 O6 94.25(3) . . ?
O1 Sc01 O10 138.96(3) . . ?
O9 Sc01 O10 71.58(3) . . ?
O6 Sc01 O10 79.83(3) . . ?
O1 Sc01 O7 89.78(3) . 4_545 ?
O9 Sc01 O7 97.43(3) . 4_545 ?
O6 Sc01 O7 147.33(3) . 4_545 ?
O10 Sc01 O7 75.18(3) . 4_545 ?
O1 Sc01 O2 71.77(3) . . ?
O9 Sc01 O2 139.00(3) . . ?
O6 Sc01 O2 73.03(3) . . ?
O10 Sc01 O2 67.89(3) . . ?
O7 Sc01 O2 78.21(3) 4_545 . ?
O1 Sc01 O8 76.32(3) . 4_545 ?
O9 Sc01 O8 77.54(3) . 4_545 ?
O6 Sc01 O8 140.43(3) . 4_545 ?
O10 Sc01 O8 130.97(3) . 4_545 ?
O7 Sc01 O8 72.11(3) 4_545 4_545 ?
O2 Sc01 O8 136.00(3) . 4_545 ?
O1 Sc01 O5 77.53(3) . . ?
O9 Sc01 O5 78.24(3) . . ?
O6 Sc01 O5 71.05(3) . . ?
O10 Sc01 O5 135.92(3) . . ?
O7 Sc01 O5 141.28(3) 4_545 . ?
O2 Sc01 O5 129.40(3) . . ?
O8 Sc01 O5 69.38(3) 4_545 . ?
O1 Sc01 Na3 104.81(2) . . ?
O9 Sc01 Na3 101.13(2) . . ?
O6 Sc01 Na3 38.88(2) . . ?
O10 Sc01 Na3 48.62(2) . . ?
O7 Sc01 Na3 108.66(2) 4_545 . ?
O2 Sc01 Na3 45.41(2) . . ?
O8 Sc01 Na3 178.58(2) 4_545 . ?
O5 Sc01 Na3 109.92(2) . . ?
O1 Sc01 Na1 99.16(2) . 7 ?
O9 Sc01 Na1 106.51(2) . 7 ?
O6 Sc01 Na1 104.40(2) . 7 ?
O10 Sc01 Na1 44.85(2) . 7 ?
O7 Sc01 Na1 42.98(2) 4_545 7 ?
O2 Sc01 Na1 44.50(2) . 7 ?
O8 Sc01 Na1 115.08(2) 4_545 7 ?
O5 Sc01 Na1 173.88(2) . 7 ?
Na3 Sc01 Na1 65.708(14) . 7 ?
O4 Na1 O16 103.20(4) . . ?
O4 Na1 O13 146.51(3) . 4_545 ?
O4 Na1 O7 78.57(3) . 6_565 ?
O13 Na1 O7 134.04(3) 4_545 6_565 ?
O4 Na1 O3 68.79(3) . . ?
O16 Na1 O3 82.22(4) . . ?
O13 Na1 O3 78.93(3) 4_545 . ?
O7 Na1 O3 147.03(3) 6_565 . ?
O4 Na1 O2 80.04(3) . 7 ?
O13 Na1 O2 103.54(3) 4_545 7 ?
O7 Na1 O2 67.55(3) 6_565 7 ?
O3 Na1 O2 109.70(3) . 7 ?
O4 Na1 O10 131.53(3) . 7 ?
O13 Na1 O10 72.79(3) 4_545 7 ?
O7 Na1 O10 64.46(3) 6_565 7 ?
O3 Na1 O10 144.09(4) . 7 ?
O2 Na1 O10 57.96(3) 7 7 ?
O4 Na1 C2 21.45(3) . . ?
O16 Na1 C2 105.67(4) . . ?
O13 Na1 C2 125.16(3) 4_545 . ?
O7 Na1 C2 98.94(3) 6_565 . ?
O3 Na1 C2 49.45(3) . . ?
O2 Na1 C2 81.68(3) 7 . ?
O10 Na1 C2 139.49(3) 7 . ?
O4 Na1 Sc01 94.55(3) . 7 ?
O13 Na1 Sc01 108.66(3) 4_545 7 ?
O7 Na1 Sc01 37.276(18) 6_565 7 ?
O3 Na1 Sc01 147.17(3) . 7 ?
O2 Na1 Sc01 37.806(18) 7 7 ?
O10 Na1 Sc01 37.376(18) 7 7 ?
C2 Na1 Sc01 107.24(2) . 7 ?
O4 Na1 Na2 88.28(3) . . ?
O16 Na1 Na2 41.13(3) . . ?
O13 Na1 Na2 72.46(3) 4_545 . ?
O7 Na1 Na2 136.09(3) 6_565 . ?
O3 Na1 Na2 41.37(2) . . ?
O2 Na1 Na2 150.93(2) 7 . ?
O10 Na1 Na2 140.14(2) 7 . ?
C2 Na1 Na2 78.06(2) . . ?
Sc01 Na1 Na2 171.239(17) 7 . ?
O4 Na1 Na3 115.47(3) . 7 ?
O13 Na1 Na3 63.09(2) 4_545 7 ?
O7 Na1 Na3 94.27(2) 6_565 7 ?
O3 Na1 Na3 103.58(3) . 7 ?
O2 Na1 Na3 40.61(2) 7 7 ?
O10 Na1 Na3 43.51(2) 7 7 ?
C2 Na1 Na3 107.41(2) . 7 ?
Sc01 Na1 Na3 57.005(10) 7 7 ?
Na2 Na1 Na3 128.805(18) . 7 ?
O4 Na1 Na4 119.47(3) . 3_444 ?
O13 Na1 Na4 31.21(2) 4_545 3_444 ?
O7 Na1 Na4 143.85(2) 6_565 3_444 ?
O3 Na1 Na4 62.73(2) . 3_444 ?
O2 Na1 Na4 84.15(2) 7 3_444 ?
O10 Na1 Na4 81.81(2) 7 3_444 ?
C2 Na1 Na4 98.66(2) . 3_444 ?
Sc01 Na1 Na4 107.005(15) 7 3_444 ?
Na2 Na1 Na4 78.578(17) . 3_444 ?
Na3 Na1 Na4 50.242(12) 7 3_444 ?
O3 C1 O1 126.24(10) . . ?
O3 C1 C2 119.23(9) . . ?
O1 C1 C2 114.52(9) . . ?
C1 O1 Sc01 121.02(7) . . ?
O4 C2 O2 126.23(9) . . ?
O4 C2 C1 119.99(9) . . ?
O2 C2 C1 113.77(9) . . ?
O4 C2 Na1 45.14(5) . . ?
O2 C2 Na1 158.65(7) . . ?
C1 C2 Na1 78.41(6) . . ?
C2 O2 Sc01 118.52(6) . . ?
C2 O2 Na1 119.40(6) . 7 ?
Sc01 O2 Na1 97.70(3) . 7 ?
C2 O2 Na3 120.53(6) . . ?
Sc01 O2 Na3 96.53(3) . . ?
Na1 O2 Na3 99.27(3) 7 . ?
O18B Na2 O18B 67.5(6) . 2 ?
O18B Na2 O16 90.59(13) . . ?
O18B Na2 O16 100.77(16) 2 . ?
O18B Na2 O3 100.2(3) . . ?
O18B Na2 O3 167.0(3) 2 . ?
O16 Na2 O3 83.11(4) . . ?
O16 Na2 O3 87.47(4) 2 . ?
O3 Na2 O3 92.35(5) 2 . ?
O3 Na2 O18A 82.1(3) 2 2 ?
O3 Na2 O18A 173.9(3) . 2 ?
O3 Na2 O18A 173.9(3) 2 . ?
O3 Na2 O18A 82.1(3) . . ?
O18A Na2 O18A 103.5(7) 2 . ?
O3 Na2 Na1 42.34(2) 2 2 ?
O3 Na2 Na1 86.07(3) . 2 ?
O18A Na2 Na1 91.4(2) 2 2 ?
O18A Na2 Na1 134.19(19) . 2 ?
O18B Na2 Na1 100.84(16) . . ?
O18B Na2 Na1 141.39(13) 2 . ?
O16 Na2 Na1 41.05(3) . . ?
O16 Na2 Na1 128.02(4) 2 . ?
O3 Na2 Na1 86.07(3) 2 . ?
O3 Na2 Na1 42.34(2) . . ?
O18A Na2 Na1 134.19(19) 2 . ?
O18A Na2 Na1 91.4(2) . . ?
Na1 Na2 Na1 108.65(3) 2 . ?
O6 Na3 O12 144.91(4) . 5_666 ?
O6 Na3 O15 131.58(4) . . ?
O12 Na3 O15 83.51(3) 5_666 . ?
O6 Na3 O14A 83.53(5) . 7_565 ?
O12 Na3 O14A 101.02(5) 5_666 7_565 ?
O15 Na3 O14A 86.75(5) . 7_565 ?
O6 Na3 O11 76.73(3) . 5_666 ?
O12 Na3 O11 68.19(3) 5_666 5_666 ?
O15 Na3 O11 151.67(4) . 5_666 ?
O14A Na3 O11 99.31(5) 7_565 5_666 ?
O6 Na3 O2 64.62(3) . . ?
O12 Na3 O2 139.23(4) 5_666 . ?
O15 Na3 O2 75.94(3) . . ?
O14A Na3 O2 112.34(5) 7_565 . ?
O11 Na3 O2 125.33(3) 5_666 . ?
O6 Na3 O10 67.78(3) . . ?
O12 Na3 O10 102.48(4) 5_666 . ?
O15 Na3 O10 112.01(4) . . ?
O14A Na3 O10 151.31(5) 7_565 . ?
O11 Na3 O10 74.73(3) 5_666 . ?
O2 Na3 O10 55.96(3) . . ?
O6 Na3 Na4 160.67(3) . 5_666 ?
O12 Na3 Na4 43.63(2) 5_666 5_666 ?
O15 Na3 Na4 46.51(3) . 5_666 ?
O14A Na3 Na4 113.90(4) 7_565 5_666 ?
O11 Na3 Na4 106.97(3) 5_666 5_666 ?
O2 Na3 Na4 99.50(3) . 5_666 ?
O10 Na3 Na4 94.51(3) . 5_666 ?
O6 Na3 Sc01 36.15(2) . . ?
O12 Na3 Sc01 139.66(3) 5_666 . ?
O15 Na3 Sc01 113.93(3) . . ?
O14A Na3 Sc01 115.43(4) 7_565 . ?
O11 Na3 Sc01 88.55(2) 5_666 . ?
O2 Na3 Sc01 38.063(18) . . ?
O10 Na3 Sc01 37.840(17) . . ?
Na4 Na3 Sc01 124.54(2) 5_666 . ?
O6 Na3 Na1 93.27(3) . 7 ?
O12 Na3 Na1 99.99(3) 5_666 7 ?
O15 Na3 Na1 71.23(3) . 7 ?
O14A Na3 Na1 147.43(5) 7_565 7 ?
O11 Na3 Na1 111.52(3) 5_666 7 ?
O2 Na3 Na1 40.12(2) . 7 ?
O10 Na3 Na1 40.830(19) . 7 ?
Na4 Na3 Na1 67.596(17) 5_666 7 ?
Sc01 Na3 Na1 57.287(12) . 7 ?
O5 C3 O7 128.41(9) . . ?
O5 C3 C4 115.74(8) . . ?
O7 C3 C4 115.84(8) . . ?
C1 O3 Na2 125.85(8) . . ?
C1 O3 Na1 111.25(7) . . ?
Na2 O3 Na1 96.29(3) . . ?
O8 C4 O6 127.19(9) . . ?
O8 C4 C3 116.90(8) . . ?
O6 C4 C3 115.91(8) . . ?
C2 O4 Na1 113.40(7) . . ?
O12 Na4 O12 92.24(6) . 2_656 ?
O12 Na4 O13 178.48(4) . . ?
O12 Na4 O13 86.34(3) 2_656 . ?
O12 Na4 O13 86.34(3) . 2_656 ?
O12 Na4 O13 178.48(4) 2_656 2_656 ?
O13 Na4 O13 95.09(5) . 2_656 ?
O12 Na4 O15 82.15(3) . 6_665 ?
O12 Na4 O15 83.02(4) 2_656 6_665 ?
O13 Na4 O15 97.1 . 6_665 ?
O13 Na4 O15 97.3 2_656 6_665 ?
O12 Na4 O15 83.02(4) . 5_666 ?
O12 Na4 O15 82.15(3) 2_656 5_666 ?
O13 Na4 O15 97.3 . 5_666 ?
O13 Na4 O15 97.1 2_656 5_666 ?
O15 Na4 O15 158.54(6) 6_665 5_666 ?
O12 Na4 Na3 44.62(2) . 5_666 ?
O12 Na4 Na3 104.76(3) 2_656 5_666 ?
O13 Na4 Na3 136.33(3) . 5_666 ?
O13 Na4 Na3 73.84(2) 2_656 5_666 ?
O15 Na4 Na3 125.78(3) 6_665 5_666 ?
O15 Na4 Na3 44.98(2) 5_666 5_666 ?
O12 Na4 Na3 104.76(3) . 6_665 ?
O12 Na4 Na3 44.62(2) 2_656 6_665 ?
O13 Na4 Na3 73.84(2) . 6_665 ?
O13 Na4 Na3 136.33(3) 2_656 6_665 ?
O15 Na4 Na3 44.98(2) 6_665 6_665 ?
O15 Na4 Na3 125.78(3) 5_666 6_665 ?
Na3 Na4 Na3 141.51(3) 5_666 6_665 ?
O12 Na4 Na1 96.04(3) . 3 ?
O12 Na4 Na1 146.99(2) 2_656 3 ?
O13 Na4 Na1 85.45(3) . 3 ?
O13 Na4 Na1 32.89(2) 2_656 3 ?
O15 Na4 Na1 129.73(3) 6_665 3 ?
O15 Na4 Na1 67.31(3) 5_666 3 ?
Na3 Na4 Na1 62.163(14) 5_666 3 ?
Na3 Na4 Na1 156.32(2) 6_665 3 ?
O12 Na4 Na1 146.99(2) . 4 ?
O12 Na4 Na1 96.04(3) 2_656 4 ?
O13 Na4 Na1 32.89(2) . 4 ?
O13 Na4 Na1 85.45(3) 2_656 4 ?
O15 Na4 Na1 67.31(3) 6_665 4 ?
O15 Na4 Na1 129.73(3) 5_666 4 ?
Na3 Na4 Na1 156.32(2) 5_666 4 ?
Na3 Na4 Na1 62.163(14) 6_665 4 ?
Na1 Na4 Na1 94.19(2) 3 4 ?
O12 Na4 H13B 162.7 . . ?
O12 Na4 H13B 98.2 2_656 . ?
O13 Na4 H13B 18.6 . . ?
O13 Na4 H13B 83.0 2_656 . ?
O15 Na4 H13B 112.7 6_665 . ?
O15 Na4 H13B 84.8 5_666 . ?
Na3 Na4 H13B 118.8 5_666 . ?
Na3 Na4 H13B 92.3 6_665 . ?
Na1 Na4 H13B 67.8 3 . ?
Na1 Na4 H13B 45.5 4 . ?
O12 C5 O9 126.46(10) . . ?
O12 C5 C6 119.29(9) . . ?
O9 C5 C6 114.26(9) . . ?
C3 O5 Sc01 116.93(6) . . ?
C3 O7 Sc01 117.51(6) . 4 ?
C3 O7 Na1 141.08(6) . 6_665 ?
Sc01 O7 Na1 99.75(3) 4 6_665 ?
C4 O8 Sc01 115.86(6) . 4 ?
C4 O6 Sc01 120.04(6) . . ?
C4 O6 Na3 134.84(6) . . ?
Sc01 O6 Na3 104.97(3) . . ?
O11 C6 O10 126.29(9) . . ?
O11 C6 C5 119.76(9) . . ?
O10 C6 C5 113.96(8) . . ?
C5 O9 Sc01 120.27(7) . . ?
C6 O10 Sc01 119.73(6) . . ?
C6 O10 Na1 124.87(6) . 7 ?
Sc01 O10 Na1 97.78(3) . 7 ?
C6 O10 Na3 118.48(6) . . ?
Sc01 O10 Na3 93.54(3) . . ?
Na1 O10 Na3 95.66(3) 7 . ?
C6 O11 Na3 111.52(7) . 5_666 ?
C5 O12 Na4 128.45(8) . . ?
C5 O12 Na3 116.96(7) . 5_666 ?
Na4 O12 Na3 91.75(3) . 5_666 ?
Na4 O13 Na1 115.90(4) . 4 ?
Na4 O13 H13A 122.2 . . ?
Na1 O13 H13A 100.8 4 . ?
Na4 O13 H13B 98.8 . . ?
Na1 O13 H13B 114.8 4 . ?
H13A O13 H13B 104.5 . . ?
Na3 O15 Na4 88.51(3) . 5_666 ?
Na3 O15 H15A 99.7 . . ?
Na4 O15 H15A 142.2 5_666 . ?
Na3 O15 H15B 131.7 . . ?
Na4 O15 H15B 96.7 5_666 . ?
H15A O15 H15B 104.5 . . ?
Na3 O14A H14A 105.6 7_565 . ?
Na3 O14A H14B 112.3 7_565 . ?
H14A O14A H14B 104.5 . . ?
H14C O14B H14D 104.5 . . ?
Na1 O16 Na2 97.82(4) . . ?
Na1 O16 H16A 103.1 . . ?
Na2 O16 H16A 119.0 . . ?
Na1 O16 H16B 107.2 . . ?
Na2 O16 H16B 122.6 . . ?
H16A O16 H16B 104.5 . . ?
H17A O17 H17B 104.5 . . ?

_refine_diff_density_max         0.557
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.086

####################################################################### 
# 
# 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_Sc2K8ox7
_database_code_depnum_ccdc_archive 'CCDC 1963554'
loop_
_audit_author_name
_audit_author_address
'Igor Huskic'
;McGill University
Canada
;
_audit_update_record             
;
2019-11-04 deposited with the CCDC.	2020-05-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_Sc2K8ox7            
;
PROBLEM: Non-Solvent  Resd 1  O   Ueq(max)/Ueq(min) Range        8.2 Ratio
RESPONSE: O7 coordinated to K1 seems to be dynamically disordered.
;
_vrf_PLAT242_Sc2K8ox7            
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         K1 Check
RESPONSE: O7 coordinated to K1 seems to be dynamically disordered.
;
_vrf_PLAT417_Sc2K8ox7            
;
PROBLEM: Short Inter D-H..H-D       H2       ..H7       .       1.92 Ang.
RESPONSE: H2 and H7 are involved in hydrogen bonding
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H12 K3.50 O20 Sc'
_chemical_formula_weight         597.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.3119 1.5331 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   15.8839(14)
_cell_length_b                   11.4558(10)
_cell_length_c                   22.7314(19)
_cell_angle_alpha                90
_cell_angle_beta                 92.190(4)
_cell_angle_gamma                90
_cell_volume                     4133.2(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    38393
_cell_measurement_theta_min      7.784
_cell_measurement_theta_max      144.285

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_F_000             2412
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    10.281
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4751
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_process_details   'SADABS-2012/1, G. Sheldrick'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed x-ray tube'
_diffrn_measurement_device_type  'Bruker PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35859
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.892
_diffrn_reflns_theta_max         72.485
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4080
_reflns_number_gt                3354
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX 2, Bruker-AXS'
_computing_cell_refinement       'SAINT V8.35A, Bruker-AXS'
_computing_data_reduction        'SAINT V8.35A, Bruker-AXS'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0693P)²+16.4014P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4080
_refine_ls_number_parameters     337
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1425
_refine_ls_wR_factor_gt          0.1263
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.051
_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
Sc1 Sc 0.38473(4) 0.31729(5) 0.64468(2) 0.02211(17) Uani 1 1 d . . . . .
K1 K 0.59773(6) 0.45529(9) 0.59487(4) 0.0525(3) Uani 1 1 d D . . . .
C1 C 0.3379(3) 0.3687(4) 0.51710(16) 0.0392(8) Uani 1 1 d . . . . .
O1 O 0.3015(2) 0.4004(4) 0.47091(13) 0.0601(9) Uani 1 1 d . . . . .
K2 K 0.27232(5) 0.81927(6) 0.72721(4) 0.0378(2) Uani 1 1 d . . . . .
O2 O 0.41875(16) 0.1309(2) 0.64204(12) 0.0372(6) Uani 1 1 d . . . . .
C2 C 0.4328(3) 0.3453(4) 0.51791(15) 0.0382(8) Uani 1 1 d . . . . .
O3 O 0.4717(2) 0.3563(4) 0.47228(14) 0.0742(12) Uani 1 1 d . . . . .
C3 C 0.3673(2) 0.0542(3) 0.65901(16) 0.0330(7) Uani 1 1 d . . . . .
K3 K 0.000000 0.35904(15) 0.750000 0.0626(4) Uani 1 2 d DS T P . .
K4 K 0.14417(6) 0.32941(10) 0.59986(4) 0.0504(3) Uani 1 1 d D . . . .
C4 C 0.2773(2) 0.1006(3) 0.66745(14) 0.0274(7) Uani 1 1 d . . . . .
O4 O 0.5310(2) 0.0982(3) 0.54418(13) 0.0497(7) Uani 1 1 d D . . . .
H2 H 0.567(3) 0.115(5) 0.5776(13) 0.075 Uiso 1 1 d D U . . .
H1 H 0.549(3) 0.147(4) 0.5134(14) 0.075 Uiso 1 1 d D U . . .
O5 O 0.0783(2) 0.5108(3) 0.6719(2) 0.0747(11) Uani 1 1 d D . . . .
C5 C 0.3815(2) 0.5800(3) 0.66211(18) 0.0376(8) Uani 1 1 d . . . . .
H8 H 0.1295(3) 0.5237(3) 0.69388(16) 0.056 Uiso 1 1 d D U . . .
C6 C 0.2894(2) 0.5430(3) 0.66988(15) 0.0320(7) Uani 1 1 d . . . . .
O6 O 0.1318(3) 0.4378(5) 0.4921(2) 0.0928(14) Uani 1 1 d D . . . .
H4 H 0.160(4) 0.510(2) 0.4993(7) 0.139 Uiso 1 1 d D U . . .
H3 H 0.0727(4) 0.442(5) 0.4844(13) 0.139 Uiso 1 1 d D U . . .
C7 C 0.4613(2) 0.3072(3) 0.76888(13) 0.0239(6) Uani 1 1 d . . . . .
O8 O 0.0806(2) 0.1919(4) 0.68603(19) 0.0710(11) Uani 1 1 d D . . . .
O10 O 0.46388(16) 0.3131(2) 0.56704(10) 0.0327(5) Uani 1 1 d . . . . .
O11 O 0.43033(16) 0.4977(2) 0.64802(12) 0.0366(6) Uani 1 1 d . . . . .
O12 O 0.27846(15) 0.4342(2) 0.67221(11) 0.0313(5) Uani 1 1 d . . . . .
O13 O 0.23441(18) 0.6186(2) 0.67290(17) 0.0543(8) Uani 1 1 d . . . . .
O14 O 0.4020(2) 0.6824(3) 0.6702(2) 0.0689(11) Uani 1 1 d . . . . .
O15 O 0.22001(16) 0.0327(2) 0.67874(13) 0.0403(6) Uani 1 1 d . . . . .
O16 O 0.27134(14) 0.2106(2) 0.66257(10) 0.0297(5) Uani 1 1 d . . . . .
O17 O 0.38290(19) -0.0491(2) 0.66892(17) 0.0561(9) Uani 1 1 d . . . . .
O18 O 0.47423(14) 0.3086(2) 0.82323(10) 0.0299(5) Uani 1 1 d . . . . .
O19 O 0.39108(14) 0.3067(2) 0.74186(10) 0.0304(5) Uani 1 1 d . . . . .
O9 O 0.30577(17) 0.3507(3) 0.56558(11) 0.0407(6) Uani 1 1 d . . . . .
H10 H 0.1286(3) 0.1740(4) 0.71055(16) 0.061 Uiso 1 1 d D U . . .
H9 H 0.0352(3) 0.1522(3) 0.66648(18) 0.061 Uiso 1 1 d D U . . .
H5 H 0.0351(11) 0.5679(19) 0.6678(14) 0.061 Uiso 1 1 d D U . . .
O7 O 0.7024(8) 0.2619(9) 0.5680(4) 0.244(6) Uani 1 1 d D . . . .
H7 H 0.669(3) 0.2044(13) 0.586(4) 0.366 Uiso 1 1 d D U . . .
H6 H 0.696(5) 0.269(5) 0.5264(4) 0.366 Uiso 1 1 d D U . . .
O5A O 0.5374(5) 0.1545(8) 0.4304(3) 0.0697(19) Uani 0.5673 1 d D . P A 1
H12A H 0.531(8) 0.085(4) 0.453(3) 0.105 Uiso 0.5673 1 d D U P B 1
H11A H 0.541(9) 0.227(3) 0.451(3) 0.105 Uiso 0.5673 1 d D U P C 1
O5B O 0.6078(6) 0.1837(7) 0.4499(4) 0.064(2) Uani 0.4327 1 d D . P D 2
H12B H 0.661(3) 0.199(12) 0.433(4) 0.096 Uiso 0.4327 1 d D U P E 2
H11B H 0.560(3) 0.18(2) 0.423(3) 0.096 Uiso 0.4327 1 d D U P F 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
Sc1 O9 2.186(3) . ?
Sc1 O11 2.190(3) . ?
Sc1 O2 2.204(2) . ?
Sc1 O10 2.206(2) . ?
Sc1 O19 2.211(2) . ?
Sc1 O16 2.227(2) . ?
Sc1 O12 2.262(2) . ?
Sc1 O18 2.332(2) 2_656 ?
Sc1 K2 3.9064(10) 4_546 ?
Sc1 K4 3.9193(11) . ?
Sc1 K1 3.9396(11) . ?
K1 O10 2.733(3) . ?
K1 O1 2.777(3) 5_666 ?
K1 O18 2.786(2) 2_656 ?
K1 O15 2.813(3) 3 ?
K1 O3 2.842(4) 5_666 ?
K1 O7 2.850(9) . ?
K1 O11 3.002(3) . ?
K1 C2 3.341(4) . ?
K1 O8 3.429(4) 3 ?
K1 C1 3.433(4) 5_666 ?
K1 C2 3.454(4) 5_666 ?
C1 O1 1.234(5) . ?
C1 O9 1.249(5) . ?
C1 C2 1.530(6) . ?
C1 K4 3.515(4) 7_556 ?
O1 K4 3.220(4) 7_556 ?
K2 O13 2.667(3) . ?
K2 O17 2.701(3) 1_565 ?
K2 O19 2.718(2) 4_556 ?
K2 O12 2.784(2) 4_556 ?
K2 O15 2.796(3) 1_565 ?
K2 O16 2.905(2) 4_556 ?
K2 O14 2.930(3) . ?
K2 O8 3.335(4) 4_556 ?
K2 C6 3.438(4) . ?
K2 C3 3.479(3) 1_565 ?
K2 C4 3.499(3) 1_565 ?
K2 K3 3.6621(9) 3 ?
O2 C3 1.270(4) . ?
C2 O3 1.233(5) . ?
C2 O10 1.259(4) . ?
C2 K4 3.524(4) 7_556 ?
O3 K4 3.220(5) 7_556 ?
C3 O17 1.228(4) . ?
C3 C4 1.544(5) . ?
K3 O8 2.750(4) 2_556 ?
K3 O8 2.750(4) . ?
K3 O17 2.775(4) 4_556 ?
K3 O17 2.775(4) 3_455 ?
K3 O5 2.808(4) 2_556 ?
K3 O5 2.808(4) . ?
K3 O14 3.098(4) 3_445 ?
K3 O14 3.098(4) 4_546 ?
K3 K4 4.1958(10) . ?
K3 K4 4.1958(10) 2_556 ?
K4 O9 2.722(3) . ?
K4 O8 2.736(4) . ?
K4 O6 2.747(5) . ?
K4 O16 2.783(2) . ?
K4 O5 2.868(4) . ?
K4 O12 2.903(3) . ?
K4 O5A 2.944(9) 7_556 ?
C4 O15 1.231(4) . ?
C4 O16 1.268(4) . ?
O4 H2 0.951(2) . ?
O4 H1 0.951(2) . ?
O5 H8 0.949(2) . ?
O5 H5 0.950(2) . ?
C5 O14 1.229(5) . ?
C5 O11 1.269(5) . ?
C5 C6 1.540(5) . ?
C6 O13 1.234(4) . ?
C6 O12 1.259(4) . ?
O6 H4 0.950(2) . ?
O6 H3 0.950(2) . ?
C7 O18 1.245(4) . ?
C7 O19 1.253(4) . ?
C7 C7 1.525(6) 2_656 ?
O8 H10 0.949(2) . ?
O8 H9 0.949(2) . ?
O7 H7 0.950(2) . ?
O7 H6 0.950(2) . ?
O5A H12A 0.950(2) . ?
O5A H11A 0.950(2) . ?
O5B H12B 0.950(2) . ?
O5B H11B 0.950(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
O9 Sc1 O11 92.41(11) . . ?
O9 Sc1 O2 106.30(11) . . ?
O11 Sc1 O2 146.51(10) . . ?
O9 Sc1 O10 70.88(10) . . ?
O11 Sc1 O10 81.40(9) . . ?
O2 Sc1 O10 79.01(9) . . ?
O9 Sc1 O19 146.52(10) . . ?
O11 Sc1 O19 90.83(10) . . ?
O2 Sc1 O19 88.41(10) . . ?
O10 Sc1 O19 142.43(9) . . ?
O9 Sc1 O16 78.68(10) . . ?
O11 Sc1 O16 141.29(9) . . ?
O2 Sc1 O16 70.96(9) . . ?
O10 Sc1 O16 128.59(9) . . ?
O19 Sc1 O16 78.10(9) . . ?
O9 Sc1 O12 73.33(10) . . ?
O11 Sc1 O12 71.39(9) . . ?
O2 Sc1 O12 140.14(9) . . ?
O10 Sc1 O12 133.49(9) . . ?
O19 Sc1 O12 76.23(9) . . ?
O16 Sc1 O12 69.96(9) . . ?
O9 Sc1 O18 141.17(9) . 2_656 ?
O11 Sc1 O18 73.56(9) . 2_656 ?
O2 Sc1 O18 74.54(9) . 2_656 ?
O10 Sc1 O18 71.30(9) . 2_656 ?
O19 Sc1 O18 71.24(8) . 2_656 ?
O16 Sc1 O18 133.90(9) . 2_656 ?
O12 Sc1 O18 131.08(9) . 2_656 ?
O9 Sc1 K2 104.44(7) . 4_546 ?
O11 Sc1 K2 100.86(7) . 4_546 ?
O2 Sc1 K2 100.96(7) . 4_546 ?
O10 Sc1 K2 174.98(7) . 4_546 ?
O19 Sc1 K2 42.39(6) . 4_546 ?
O16 Sc1 K2 47.40(6) . 4_546 ?
O12 Sc1 K2 44.42(6) . 4_546 ?
O18 Sc1 K2 113.60(6) 2_656 4_546 ?
O9 Sc1 K4 42.01(7) . . ?
O11 Sc1 K4 107.07(7) . . ?
O2 Sc1 K4 105.36(7) . . ?
O10 Sc1 K4 111.87(7) . . ?
O19 Sc1 K4 105.57(6) . . ?
O16 Sc1 K4 43.92(6) . . ?
O12 Sc1 K4 47.19(6) . . ?
O18 Sc1 K4 176.80(6) 2_656 . ?
K2 Sc1 K4 63.23(2) 4_546 . ?
O9 Sc1 K1 99.52(7) . . ?
O11 Sc1 K1 49.07(7) . . ?
O2 Sc1 K1 99.60(7) . . ?
O10 Sc1 K1 42.01(7) . . ?
O19 Sc1 K1 107.59(6) . . ?
O16 Sc1 K1 169.16(7) . . ?
O12 Sc1 K1 120.00(6) . . ?
O18 Sc1 K1 44.08(6) 2_656 . ?
K2 Sc1 K1 142.36(3) 4_546 . ?
K4 Sc1 K1 138.64(3) . . ?
O10 K1 O1 133.57(9) . 5_666 ?
O10 K1 O18 57.30(7) . 2_656 ?
O1 K1 O18 168.12(8) 5_666 2_656 ?
O10 K1 O15 148.84(8) . 3 ?
O1 K1 O15 77.29(9) 5_666 3 ?
O18 K1 O15 91.59(7) 2_656 3 ?
O10 K1 O3 92.64(11) . 5_666 ?
O1 K1 O3 58.55(10) 5_666 5_666 ?
O18 K1 O3 131.04(9) 2_656 5_666 ?
O15 K1 O3 111.59(12) 3 5_666 ?
O10 K1 O7 86.7(3) . . ?
O1 K1 O7 89.7(3) 5_666 . ?
O18 K1 O7 86.1(2) 2_656 . ?
O15 K1 O7 89.8(3) 3 . ?
O3 K1 O7 133.9(2) 5_666 . ?
O10 K1 O11 59.76(7) . . ?
O1 K1 O11 131.14(10) 5_666 . ?
O18 K1 O11 55.68(7) 2_656 . ?
O15 K1 O11 105.99(8) 3 . ?
O3 K1 O11 76.23(9) 5_666 . ?
O7 K1 O11 138.1(3) . . ?
O10 K1 C2 21.02(8) . . ?
O1 K1 C2 113.52(9) 5_666 . ?
O18 K1 C2 77.81(8) 2_656 . ?
O15 K1 C2 168.89(9) 3 . ?
O3 K1 C2 74.04(12) 5_666 . ?
O7 K1 C2 92.7(3) . . ?
O11 K1 C2 65.34(8) . . ?
O10 K1 O8 122.14(8) . 3 ?
O1 K1 O8 85.15(11) 5_666 3 ?
O18 K1 O8 91.66(9) 2_656 3 ?
O15 K1 O8 53.82(9) 3 3 ?
O3 K1 O8 71.70(12) 5_666 3 ?
O7 K1 O8 143.5(3) . 3 ?
O11 K1 O8 62.42(8) . 3 ?
C2 K1 O8 122.40(10) . 3 ?
O10 K1 C1 115.42(8) . 5_666 ?
O1 K1 C1 19.48(9) 5_666 5_666 ?
O18 K1 C1 172.38(9) 2_656 5_666 ?
O15 K1 C1 95.73(9) 3 5_666 ?
O3 K1 C1 43.61(10) 5_666 5_666 ?
O7 K1 C1 96.0(2) . 5_666 ?
O11 K1 C1 119.77(9) . 5_666 ?
C2 K1 C1 94.76(9) . 5_666 ?
O8 K1 C1 90.93(10) 3 5_666 ?
O10 K1 C2 97.84(9) . 5_666 ?
O1 K1 C2 43.46(9) 5_666 5_666 ?
O18 K1 C2 147.72(9) 2_656 5_666 ?
O15 K1 C2 111.61(9) 3 5_666 ?
O3 K1 C2 19.68(9) 5_666 5_666 ?
O7 K1 C2 114.9(2) . 5_666 ?
O11 K1 C2 95.18(9) . 5_666 ?
C2 K1 C2 77.04(11) . 5_666 ?
O8 K1 C2 85.04(10) 3 5_666 ?
C1 K1 C2 25.66(10) 5_666 5_666 ?
O10 K1 Sc1 32.69(5) . . ?
O1 K1 Sc1 155.85(7) 5_666 . ?
O18 K1 Sc1 35.61(5) 2_656 . ?
O15 K1 Sc1 120.67(6) 3 . ?
O3 K1 Sc1 98.02(8) 5_666 . ?
O7 K1 Sc1 105.3(3) . . ?
O11 K1 Sc1 33.45(5) . . ?
C2 K1 Sc1 48.26(6) . . ?
O8 K1 Sc1 93.14(6) 3 . ?
C1 K1 Sc1 137.05(7) 5_666 . ?
C2 K1 Sc1 112.39(7) 5_666 . ?
O1 C1 O9 127.2(4) . . ?
O1 C1 C2 119.4(3) . . ?
O9 C1 C2 113.4(3) . . ?
O1 C1 K1 48.7(2) . 5_666 ?
O9 C1 K1 153.4(3) . 5_666 ?
C2 C1 K1 77.9(2) . 5_666 ?
O1 C1 K4 66.2(3) . 7_556 ?
O9 C1 K4 127.5(3) . 7_556 ?
C2 C1 K4 77.8(2) . 7_556 ?
K1 C1 K4 77.50(8) 5_666 7_556 ?
C1 O1 K1 111.9(3) . 5_666 ?
C1 O1 K4 93.3(3) . 7_556 ?
K1 O1 K4 92.68(10) 5_666 7_556 ?
O13 K2 O17 113.19(11) . 1_565 ?
O13 K2 O19 82.72(9) . 4_556 ?
O17 K2 O19 143.29(9) 1_565 4_556 ?
O13 K2 O12 136.08(9) . 4_556 ?
O17 K2 O12 110.67(9) 1_565 4_556 ?
O19 K2 O12 60.22(7) 4_556 4_556 ?
O13 K2 O15 120.87(10) . 1_565 ?
O17 K2 O15 60.47(8) 1_565 1_565 ?
O19 K2 O15 82.86(8) 4_556 1_565 ?
O12 K2 O15 79.56(8) 4_556 1_565 ?
O13 K2 O16 88.43(9) . 4_556 ?
O17 K2 O16 147.52(10) 1_565 4_556 ?
O19 K2 O16 59.52(7) 4_556 4_556 ?
O12 K2 O16 53.74(7) 4_556 4_556 ?
O15 K2 O16 129.62(8) 1_565 4_556 ?
O13 K2 O14 58.93(9) . . ?
O17 K2 O14 66.45(9) 1_565 . ?
O19 K2 O14 141.28(9) 4_556 . ?
O12 K2 O14 147.90(11) 4_556 . ?
O15 K2 O14 119.81(10) 1_565 . ?
O16 K2 O14 110.31(10) 4_556 . ?
O13 K2 O8 92.14(10) . 4_556 ?
O17 K2 O8 94.61(10) 1_565 4_556 ?
O19 K2 O8 118.56(8) 4_556 4_556 ?
O12 K2 O8 86.55(9) 4_556 4_556 ?
O15 K2 O8 143.77(10) 1_565 4_556 ?
O16 K2 O8 59.17(8) 4_556 4_556 ?
O14 K2 O8 62.57(12) . 4_556 ?
O13 K2 C6 18.32(9) . . ?
O17 K2 C6 105.42(9) 1_565 . ?
O19 K2 C6 98.01(8) 4_556 . ?
O12 K2 C6 140.92(8) 4_556 . ?
O15 K2 C6 133.05(9) 1_565 . ?
O16 K2 C6 87.54(8) 4_556 . ?
O14 K2 C6 43.31(8) . . ?
O8 K2 C6 75.98(10) 4_556 . ?
O13 K2 C3 123.68(10) . 1_565 ?
O17 K2 C3 17.82(8) 1_565 1_565 ?
O19 K2 C3 126.21(8) 4_556 1_565 ?
O12 K2 C3 98.29(8) 4_556 1_565 ?
O15 K2 C3 43.54(8) 1_565 1_565 ?
O16 K2 C3 146.91(8) 4_556 1_565 ?
O14 K2 C3 83.83(9) . 1_565 ?
O8 K2 C3 107.21(9) 4_556 1_565 ?
C6 K2 C3 120.09(9) . 1_565 ?
O13 K2 C4 128.47(10) . 1_565 ?
O17 K2 C4 43.15(8) 1_565 1_565 ?
O19 K2 C4 100.66(8) 4_556 1_565 ?
O12 K2 C4 83.96(7) 4_556 1_565 ?
O15 K2 C4 18.59(8) 1_565 1_565 ?
O16 K2 C4 137.66(7) 4_556 1_565 ?
O14 K2 C4 107.12(9) . 1_565 ?
O8 K2 C4 127.35(9) 4_556 1_565 ?
C6 K2 C4 134.22(8) . 1_565 ?
C3 K2 C4 25.57(8) 1_565 1_565 ?
O13 K2 K3 112.15(7) . 3 ?
O17 K2 K3 48.90(8) 1_565 3 ?
O19 K2 K3 156.55(6) 4_556 3 ?
O12 K2 K3 98.08(6) 4_556 3 ?
O15 K2 K3 102.94(6) 1_565 3 ?
O16 K2 K3 101.44(5) 4_556 3 ?
O14 K2 K3 54.71(8) . 3 ?
O8 K2 K3 45.98(7) 4_556 3 ?
C6 K2 K3 94.38(7) . 3 ?
C3 K2 K3 61.57(7) 1_565 3 ?
C4 K2 K3 84.46(6) 1_565 3 ?
C3 O2 Sc1 120.1(2) . . ?
O3 C2 O10 125.7(4) . . ?
O3 C2 C1 119.8(4) . . ?
O10 C2 C1 114.5(3) . . ?
O3 C2 K1 89.7(3) . . ?
O10 C2 K1 51.16(19) . . ?
C1 C2 K1 133.8(2) . . ?
O3 C2 K1 50.9(2) . 5_666 ?
O10 C2 K1 153.0(3) . 5_666 ?
C1 C2 K1 76.4(2) . 5_666 ?
K1 C2 K1 102.96(11) . 5_666 ?
O3 C2 K4 65.7(3) . 7_556 ?
O10 C2 K4 128.3(3) . 7_556 ?
C1 C2 K4 77.1(2) . 7_556 ?
K1 C2 K4 148.69(13) . 7_556 ?
K1 C2 K4 77.11(8) 5_666 7_556 ?
C2 O3 K1 109.4(3) . 5_666 ?
C2 O3 K4 93.8(3) . 7_556 ?
K1 O3 K4 91.48(11) 5_666 7_556 ?
O17 C3 O2 126.5(3) . . ?
O17 C3 C4 119.3(3) . . ?
O2 C3 C4 114.1(3) . . ?
O17 C3 K2 42.31(19) . 1_545 ?
O2 C3 K2 165.0(3) . 1_545 ?
C4 C3 K2 77.96(17) . 1_545 ?
O8 K3 O8 91.75(18) 2_556 . ?
O8 K3 O17 103.10(11) 2_556 4_556 ?
O8 K3 O17 107.54(10) . 4_556 ?
O8 K3 O17 107.54(10) 2_556 3_455 ?
O8 K3 O17 103.10(11) . 3_455 ?
O17 K3 O17 135.42(14) 4_556 3_455 ?
O8 K3 O5 82.56(12) 2_556 2_556 ?
O8 K3 O5 172.54(13) . 2_556 ?
O17 K3 O5 69.33(10) 4_556 2_556 ?
O17 K3 O5 83.30(12) 3_455 2_556 ?
O8 K3 O5 172.54(14) 2_556 . ?
O8 K3 O5 82.56(12) . . ?
O17 K3 O5 83.30(12) 4_556 . ?
O17 K3 O5 69.33(10) 3_455 . ?
O5 K3 O5 103.50(18) 2_556 . ?
O8 K3 O14 67.74(13) 2_556 3_445 ?
O8 K3 O14 57.94(11) . 3_445 ?
O17 K3 O14 161.06(11) 4_556 3_445 ?
O17 K3 O14 63.23(10) 3_455 3_445 ?
O5 K3 O14 123.36(10) 2_556 3_445 ?
O5 K3 O14 105.00(12) . 3_445 ?
O8 K3 O14 57.94(11) 2_556 4_546 ?
O8 K3 O14 67.74(13) . 4_546 ?
O17 K3 O14 63.23(10) 4_556 4_546 ?
O17 K3 O14 161.06(11) 3_455 4_546 ?
O5 K3 O14 105.00(12) 2_556 4_546 ?
O5 K3 O14 123.36(10) . 4_546 ?
O14 K3 O14 98.43(16) 3_445 4_546 ?
O8 K3 K2 60.72(8) 2_556 3_445 ?
O8 K3 K2 108.41(9) . 3_445 ?
O17 K3 K2 140.74(7) 4_556 3_445 ?
O17 K3 K2 47.16(6) 3_455 3_445 ?
O5 K3 K2 73.01(8) 2_556 3_445 ?
O5 K3 K2 116.50(8) . 3_445 ?
O14 K3 K2 50.53(6) 3_445 3_445 ?
O14 K3 K2 118.24(7) 4_546 3_445 ?
O8 K3 K2 108.41(9) 2_556 4_546 ?
O8 K3 K2 60.72(8) . 4_546 ?
O17 K3 K2 47.16(6) 4_556 4_546 ?
O17 K3 K2 140.74(7) 3_455 4_546 ?
O5 K3 K2 116.50(8) 2_556 4_546 ?
O5 K3 K2 73.01(8) . 4_546 ?
O14 K3 K2 118.24(7) 3_445 4_546 ?
O14 K3 K2 50.53(6) 4_546 4_546 ?
K2 K3 K2 165.71(6) 3_445 4_546 ?
O8 K3 K4 130.80(10) 2_556 . ?
O8 K3 K4 39.99(9) . . ?
O17 K3 K4 101.43(7) 4_556 . ?
O17 K3 K4 82.14(7) 3_455 . ?
O5 K3 K4 146.38(10) 2_556 . ?
O5 K3 K4 42.90(9) . . ?
O14 K3 K4 75.43(7) 3_445 . ?
O14 K3 K4 98.39(8) 4_546 . ?
K2 K3 K4 116.20(2) 3_445 . ?
K2 K3 K4 62.503(19) 4_546 . ?
O8 K3 K4 40.00(9) 2_556 2_556 ?
O8 K3 K4 130.81(10) . 2_556 ?
O17 K3 K4 82.14(7) 4_556 2_556 ?
O17 K3 K4 101.43(7) 3_455 2_556 ?
O5 K3 K4 42.90(9) 2_556 2_556 ?
O5 K3 K4 146.38(10) . 2_556 ?
O14 K3 K4 98.39(8) 3_445 2_556 ?
O14 K3 K4 75.43(7) 4_546 2_556 ?
K2 K3 K4 62.504(19) 3_445 2_556 ?
K2 K3 K4 116.20(2) 4_546 2_556 ?
K4 K3 K4 170.72(6) . 2_556 ?
O9 K4 O8 129.36(10) . . ?
O9 K4 O6 74.93(11) . . ?
O8 K4 O6 152.00(14) . . ?
O9 K4 O16 61.09(7) . . ?
O8 K4 O16 68.42(10) . . ?
O6 K4 O16 134.71(11) . . ?
O9 K4 O5 117.87(10) . . ?
O8 K4 O5 81.68(12) . . ?
O6 K4 O5 99.61(15) . . ?
O16 K4 O5 109.60(10) . . ?
O9 K4 O12 56.26(7) . . ?
O8 K4 O12 96.64(10) . . ?
O6 K4 O12 110.13(13) . . ?
O16 K4 O12 53.77(7) . . ?
O5 K4 O12 69.71(9) . . ?
O9 K4 O5A 148.58(14) . 7_556 ?
O8 K4 O5A 79.54(16) . 7_556 ?
O6 K4 O5A 74.19(16) . 7_556 ?
O16 K4 O5A 146.66(16) . 7_556 ?
O5 K4 O5A 73.29(18) . 7_556 ?
O12 K4 O5A 142.96(18) . 7_556 ?
O9 K4 O3 116.11(9) . 7_556 ?
O8 K4 O3 76.41(11) . 7_556 ?
O6 K4 O3 79.89(14) . 7_556 ?
O16 K4 O3 109.09(9) . 7_556 ?
O5 K4 O3 123.74(10) . 7_556 ?
O12 K4 O3 162.72(9) . 7_556 ?
O5A K4 O3 52.20(19) 7_556 7_556 ?
O9 K4 O1 69.91(9) . 7_556 ?
O8 K4 O1 90.02(10) . 7_556 ?
O6 K4 O1 86.28(13) . 7_556 ?
O16 K4 O1 69.69(7) . 7_556 ?
O5 K4 O1 171.16(10) . 7_556 ?
O12 K4 O1 114.58(8) . 7_556 ?
O5A K4 O1 102.31(18) 7_556 7_556 ?
O3 K4 O1 50.53(9) 7_556 7_556 ?
O9 K4 C1 74.74(9) . 7_556 ?
O8 K4 C1 102.27(11) . 7_556 ?
O6 K4 C1 67.80(14) . 7_556 ?
O16 K4 C1 89.63(9) . 7_556 ?
O5 K4 C1 160.29(11) . 7_556 ?
O12 K4 C1 128.07(9) . 7_556 ?
O5A K4 C1 88.31(17) 7_556 7_556 ?
O3 K4 C1 41.37(9) 7_556 7_556 ?
O1 K4 C1 20.52(8) 7_556 7_556 ?
O9 K4 C2 97.87(9) . 7_556 ?
O8 K4 C2 95.17(11) . 7_556 ?
O6 K4 C2 64.42(14) . 7_556 ?
O16 K4 C2 109.58(9) . 7_556 ?
O5 K4 C2 136.19(11) . 7_556 ?
O12 K4 C2 153.04(9) . 7_556 ?
O5A K4 C2 63.25(17) 7_556 7_556 ?
O3 K4 C2 20.44(8) 7_556 7_556 ?
O1 K4 C2 41.23(9) 7_556 7_556 ?
C1 K4 C2 25.10(9) 7_556 7_556 ?
O9 K4 Sc1 32.52(5) . . ?
O8 K4 Sc1 100.15(9) . . ?
O6 K4 Sc1 106.46(10) . . ?
O16 K4 Sc1 33.72(5) . . ?
O5 K4 Sc1 104.52(8) . . ?
O12 K4 Sc1 34.86(5) . . ?
O5A K4 Sc1 177.81(17) 7_556 . ?
O3 K4 Sc1 129.90(8) 7_556 . ?
O1 K4 Sc1 79.85(6) 7_556 . ?
C1 K4 Sc1 93.87(7) 7_556 . ?
C2 K4 Sc1 118.94(7) 7_556 . ?
O15 C4 O16 126.3(3) . . ?
O15 C4 C3 120.3(3) . . ?
O16 C4 C3 113.4(3) . . ?
O15 C4 K2 46.37(18) . 1_545 ?
O16 C4 K2 161.1(2) . 1_545 ?
C3 C4 K2 76.47(17) . 1_545 ?
H2 O4 H1 106(3) . . ?
K3 O5 K4 95.31(12) . . ?
K3 O5 H8 98.9(3) . . ?
K4 O5 H8 95.1(3) . . ?
K3 O5 H5 98.9(3) . . ?
K4 O5 H5 136(2) . . ?
H8 O5 H5 123(3) . . ?
O14 C5 O11 125.9(4) . . ?
O14 C5 C6 119.5(3) . . ?
O11 C5 C6 114.6(3) . . ?
O13 C6 O12 126.4(3) . . ?
O13 C6 C5 119.4(3) . . ?
O12 C6 C5 114.2(3) . . ?
O13 C6 K2 42.80(19) . . ?
O12 C6 K2 151.9(2) . . ?
C5 C6 K2 83.06(19) . . ?
K4 O6 H4 102.8(3) . . ?
K4 O6 H3 102.8(3) . . ?
H4 O6 H3 116(4) . . ?
O18 C7 O19 126.6(3) . . ?
O18 C7 C7 116.9(3) . 2_656 ?
O19 C7 C7 116.5(3) . 2_656 ?
K4 O8 K3 99.78(14) . . ?
K4 O8 K2 84.39(10) . 4_546 ?
K3 O8 K2 73.30(10) . 4_546 ?
K4 O8 K1 89.00(11) . 3_445 ?
K3 O8 K1 156.81(13) . 3_445 ?
K2 O8 K1 129.28(11) 4_546 3_445 ?
K4 O8 H10 103.6(3) . . ?
K3 O8 H10 102.7(3) . . ?
K2 O8 H10 38.7(4) 4_546 . ?
K1 O8 H10 95.9(4) 3_445 . ?
K4 O8 H9 103.6(3) . . ?
K3 O8 H9 102.7(3) . . ?
K2 O8 H9 171.7(3) 4_546 . ?
K1 O8 H9 54.2(4) 3_445 . ?
H10 O8 H9 138.6(7) . . ?
C2 O10 Sc1 119.2(2) . . ?
C2 O10 K1 107.8(2) . . ?
Sc1 O10 K1 105.30(9) . . ?
C5 O11 Sc1 120.4(2) . . ?
C5 O11 K1 141.3(2) . . ?
Sc1 O11 K1 97.49(9) . . ?
C6 O12 Sc1 117.9(2) . . ?
C6 O12 K2 123.2(2) . 4_546 ?
Sc1 O12 K2 100.94(9) . 4_546 ?
C6 O12 K4 119.0(2) . . ?
Sc1 O12 K4 97.95(8) . . ?
K2 O12 K4 92.29(7) 4_546 . ?
C6 O13 K2 118.9(3) . . ?
C5 O14 K2 113.0(3) . . ?
C5 O14 K3 146.6(4) . 3 ?
K2 O14 K3 74.76(8) . 3 ?
C4 O15 K2 115.0(2) . 1_545 ?
C4 O15 K1 123.7(2) . 3_445 ?
K2 O15 K1 100.27(9) 1_545 3_445 ?
C4 O16 Sc1 120.2(2) . . ?
C4 O16 K4 125.5(2) . . ?
Sc1 O16 K4 102.36(9) . . ?
C4 O16 K2 111.72(19) . 4_546 ?
Sc1 O16 K2 98.25(8) . 4_546 ?
K4 O16 K2 92.26(7) . 4_546 ?
C3 O17 K2 119.9(2) . 1_545 ?
C3 O17 K3 127.8(3) . 3_545 ?
K2 O17 K3 83.93(9) 1_545 3_545 ?
C7 O18 Sc1 115.5(2) . 2_656 ?
C7 O18 K1 128.0(2) . 2_656 ?
Sc1 O18 K1 100.31(8) 2_656 2_656 ?
C7 O19 Sc1 119.7(2) . . ?
C7 O19 K2 135.6(2) . 4_546 ?
Sc1 O19 K2 104.36(9) . 4_546 ?
C1 O9 Sc1 120.9(3) . . ?
C1 O9 K4 133.6(2) . . ?
Sc1 O9 K4 105.46(10) . . ?
K1 O7 H7 96.2(6) . . ?
K1 O7 H6 96.2(6) . . ?
H7 O7 H6 117(4) . . ?
K4 O5A H12A 93(8) 7_556 . ?
K4 O5A H11A 96(8) 7_556 . ?
H12A O5A H11A 119(4) . . ?
H12B O5B H11B 116(4) . . ?

_refine_diff_density_max         0.483
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.098

####################################################################### 
# 
# 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_Yb_NH4_ox2
_database_code_depnum_ccdc_archive 'CCDC 1963553'
loop_
_audit_author_name
_audit_author_address
'Igor Huskic'
;McGill University
Canada
;
_audit_update_record             
;
2019-11-04 deposited with the CCDC.	2020-05-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT699_Yb_NH4_ox2          
;
PROBLEM: Missing _exptl_crystal_description Value .......     Please Do !
RESPONSE: Structure solved from powder data
;
# Added during the CSD deposition process: Monday 04 November 2019 03:30 PM
# end Validation Reply Form


_chemical_name_systematic        
; ?
;
_chemical_name_common            
'catena-(ammonium bis(m2-oxalato)-ytterbium hydrate)'
_chemical_formula_moiety         'C4 O9 Yb, N'
_chemical_formula_analytical     ?
_chemical_formula_sum            'C4 N O9 Yb'
_chemical_formula_weight         379.09


#==============================================================================

# POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      monoclinic
_symmetry_space_group_name_H-M   P2/n
_space_group_name_Hall           '-p 2yac'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z '
'-x+1/2, y, -z+1/2 '
'-x, -y, -z '
'x+1/2, -y, z+1/2 '
_cell_length_a                   9.0427(2)
_cell_length_b                   6.09117(12)
_cell_length_c                   7.8999(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.182(3)
_cell_angle_gamma                90
_cell_volume                     435.133(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293
_cell_measurement_theta_min      4
_cell_measurement_theta_max      100
_cell_measurement_reflns_used    20
_exptl_crystal_density_diffrn    2.8933(1)
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             346

_cell_special_details            
; ?
;



# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
; 'packed powder pellet'
;
_pd_spec_mount_mode              resflection

_pd_spec_shape                   flat_sheet

_pd_char_particle_morphology     ?
_pd_char_colour                  white # use ICDD colour descriptions



_pd_prep_temperature             293


#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      293
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              ?
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_source_voltage           40
_diffrn_source_current           30
_diffrn_measurement_device_type  'Bruker D2 PHASER'
_diffrn_detector                 'Position Sensitive Detector'
_diffrn_detector_type            LYNXEYE
_pd_meas_scan_method             cont

_pd_meas_special_details         
;  ?
;

# The following six items are used for angular dispersive measurements only.

_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_monochromator  none

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        4826
_pd_meas_2theta_range_min        4.020
_pd_meas_2theta_range_max        100.037
_pd_meas_2theta_range_inc        0.0199




#==============================================================================

# REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.


# The next three items are given as text.

_pd_proc_ls_profile_function     pseudo-Voigt
_pd_proc_ls_background_function  'Chebyshev polynomial'


_pd_proc_ls_prof_R_factor        0.031
_pd_proc_ls_prof_wR_factor       0.047
_pd_proc_ls_prof_wR_expected     0.014
_refine_ls_R_I_factor            0.015


_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_parameters     48
_refine_ls_number_restraints     1
_refine_ls_number_constraints    0

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   3.396


# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        10
_pd_proc_2theta_range_max        100
_pd_proc_2theta_range_inc        0.0199
_pd_proc_wavelength              1.5418

#


# The following items are used to identify the programs used.

_computing_data_collection       'Bruker DIFFRAC.SUITE'
_computing_cell_refinement       'TOPAS Academic v. 6'
_computing_structure_solution    'TOPAS Academic v. 6'
_computing_structure_refinement  'TOPAS Academic v. 6'
_computing_molecular_graphics    ?
_computing_publication_material  ?


#==============================================================================


# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
C1 C 4 0.5369(16) -0.107(4) 0.4686(19) 1 0.82(11)
C2 C 4 0.4739(19) -0.109(3) 0.9592(18) 1 0.82(11)
O1 O 4 0.6751(8) -0.1244(17) 0.5105(10) 1 0.82(11)
O2 O 4 0.4780(9) -0.2293(13) 0.3650(12) 1 0.82(11)
O3 O 4 0.5656(8) -0.1506(14) 0.8274(10) 1 0.82(11)
O4 O 4 0.3842(9) -0.2381(14) 1.0073(12) 1 0.82(11)
O5 O 2 0.75 0.4938(13) 0.75 1 0.82(11)
Yb1 Yb 2 0.75 0.1044(2) 0.75 1 0.69(3)
N1 N 2 1.25 0.4880(16) -0.25 1 0.82(11)
#==============================================================================

# BOND LENGTHS AND ANGLES

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 2.444(9) . ?
Yb1 O3 2.361(8) . ?
Yb1 O5 2.372(8) . ?
Yb1 O1 2.444(9) 2_656 ?
Yb1 O3 2.361(8) 2_656 ?
Yb1 O2 2.376(8) 3_656 ?
Yb1 O4 2.414(9) 3_657 ?
Yb1 O4 2.414(9) 4_554 ?
Yb1 O2 2.376(8) 4_555 ?
O1 C1 1.296(16) . ?
O2 C1 1.23(2) . ?
O3 C2 1.357(17) . ?
O4 C2 1.193(19) . ?
C1 C1 1.55(3) 3_656 ?
C2 C2 1.55(2) 3_657 ?


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 O3 68.4(3) . . ?
O1 Yb1 O5 124.8(2) . . ?
O1 Yb1 O1 110.5(3) . 2_656 ?
O1 Yb1 O3 67.6(3) . 2_656 ?
O1 Yb1 O2 69.4(3) . 3_656 ?
O1 Yb1 O4 132.0(3) . 3_657 ?
O1 Yb1 O4 73.5(3) . 4_554 ?
O1 Yb1 O2 135.8(3) . 4_555 ?
O3 Yb1 O5 131.1(2) . . ?
O1 Yb1 O3 67.6(3) 2_656 . ?
O3 Yb1 O3 97.7(3) . 2_656 ?
O2 Yb1 O3 72.4(3) 3_656 . ?
O3 Yb1 O4 70.1(3) . 3_657 ?
O3 Yb1 O4 141.7(3) . 4_554 ?
O2 Yb1 O3 136.4(3) 4_555 . ?
O1 Yb1 O5 124.8(2) 2_656 . ?
O3 Yb1 O5 131.1(2) 2_656 . ?
O2 Yb1 O5 71.32(19) 3_656 . ?
O4 Yb1 O5 70.3(2) 3_657 . ?
O4 Yb1 O5 70.3(2) 4_554 . ?
O2 Yb1 O5 71.32(19) 4_555 . ?
O1 Yb1 O3 68.4(3) 2_656 2_656 ?
O1 Yb1 O2 135.8(3) 2_656 3_656 ?
O1 Yb1 O4 73.5(3) 2_656 3_657 ?
O1 Yb1 O4 132.0(3) 2_656 4_554 ?
O1 Yb1 O2 69.4(3) 2_656 4_555 ?
O2 Yb1 O3 136.4(3) 3_656 2_656 ?
O3 Yb1 O4 141.7(3) 2_656 3_657 ?
O3 Yb1 O4 70.1(3) 2_656 4_554 ?
O2 Yb1 O3 72.4(3) 4_555 2_656 ?
O2 Yb1 O4 76.0(3) 3_656 3_657 ?
O2 Yb1 O4 91.5(3) 3_656 4_554 ?
O2 Yb1 O2 142.6(3) 3_656 4_555 ?
O4 Yb1 O4 140.6(3) 3_657 4_554 ?
O2 Yb1 O4 91.5(3) 4_555 3_657 ?
O2 Yb1 O4 76.0(3) 4_555 4_554 ?
Yb1 O1 C1 114.6(10) . . ?
Yb1 O2 C1 115.8(10) 3_656 . ?
Yb1 O3 C2 120.6(9) . . ?
Yb1 O4 C2 112.0(9) 3_657 . ?
O1 C1 O2 122.5(17) . . ?
O1 C1 C1 113.8(16) . 3_656 ?
O2 C1 C1 122.6(13) . 3_656 ?
O3 C2 O4 122.6(15) . . ?
O3 C2 C2 107.1(13) . 3_657 ?
O4 C2 C2 129.7(14) . 3_657 ?
####################################################################### 
# 
# 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_Eu_K3_ox3
_database_code_depnum_ccdc_archive 'CCDC 1963551'
loop_
_audit_author_name
_audit_author_address
'Igor Huskic'
;McGill University
Canada
;
_audit_update_record             
;
2019-11-04 deposited with the CCDC.	2020-05-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT699_Eu_K3_ox3           
;
PROBLEM: Missing _exptl_crystal_description Value .......     Please Do !
RESPONSE: Structure solved from powder data
;
# Added during the CSD deposition process: Monday 04 November 2019 03:30 PM
# end Validation Reply Form


_chemical_name_systematic        
; ?
;
_chemical_name_common            
'catena-(potassium bis(m2-oxalato)-europium hydrate)'
_chemical_formula_moiety         'C6 Eu O13, 2(O), 3(K)'
_chemical_formula_analytical     ?
_chemical_formula_sum            'C6 Eu K3 O15'
_chemical_formula_weight         581.33


#==============================================================================

# POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      triclinic
_symmetry_space_group_name_H-M   P-1
_space_group_name_Hall           '-p 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z '
'-x, -y, -z '

_cell_length_a                   8.4883(2)
_cell_length_b                   9.3894(3)
_cell_length_c                   9.7552(2)
_cell_angle_alpha                98.255(2)
_cell_angle_beta                 91.154(2)
_cell_angle_gamma                96.544(3)
_cell_volume                     763.90(4)

_cell_formula_units_Z            2
_cell_measurement_temperature    293
_cell_measurement_theta_min      3
_cell_measurement_theta_max      90
_cell_measurement_reflns_used    20
_exptl_crystal_density_diffrn    2.5273(1)
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             552

_cell_special_details            
; ?
;



# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
; 'packed powder pellet'
;
_pd_spec_mount_mode              resflection

_pd_spec_shape                   flat_sheet

_pd_char_particle_morphology     ?
_pd_char_colour                  white # use ICDD colour descriptions



_pd_prep_temperature             293


#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      293
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              ?
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_source_voltage           40
_diffrn_source_current           30
_diffrn_measurement_device_type  'Bruker D2 PHASER'
_diffrn_detector                 'Position Sensitive Detector'
_diffrn_detector_type            LYNXEYE
_pd_meas_scan_method             cont

_pd_meas_special_details         
;  ?
;

# The following six items are used for angular dispersive measurements only.

_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_monochromator  none

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        4264
_pd_meas_2theta_range_min        3.010
_pd_meas_2theta_range_max        90.000
_pd_meas_2theta_range_inc        0.0199




#==============================================================================

# REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.


# The next three items are given as text.

_pd_proc_ls_profile_function     pseudo-Voigt
_pd_proc_ls_background_function  'Chebyshev polynomial'


_pd_proc_ls_prof_R_factor        0.031
_pd_proc_ls_prof_wR_factor       0.039
_pd_proc_ls_prof_wR_expected     0.017
_refine_ls_R_I_factor            0.023


_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_parameters     81
_refine_ls_number_restraints     11
_refine_ls_number_constraints    42

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   2.282


# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        8
_pd_proc_2theta_range_max        90
_pd_proc_2theta_range_inc        0.0199
_pd_proc_wavelength              1.5418

#


# The following items are used to identify the programs used.

_computing_data_collection       'Bruker DIFFRAC.SUITE'
_computing_cell_refinement       'TOPAS Academic v. 6'
_computing_structure_solution    'TOPAS Academic v. 6'
_computing_structure_refinement  'TOPAS Academic v. 6'
_computing_molecular_graphics    ?
_computing_publication_material  ?


#==============================================================================


# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Eu1 Eu 2 0.2289(5) 0.3583(5) -0.2200(4) 1 0.87(10)
O1 O 2 0.498(3) 0.475(3) -0.290(3) 1 0.87(10)
O2 O 2 0.038(3) -0.1006(18) -0.1873(19) 1 0.87(10)
O3 O 2 -0.144(3) -0.015(4) -0.383(3) 1 0.87(10)
O4 O 2 0.324(2) 0.743(2) -0.4302(19) 1 0.87(10)
O5 O 2 0.351(6) 0.579(11) -0.068(8) 1 0.87(10)
O6 O 2 0.6158(18) 0.683(4) -0.341(3) 1 0.87(10)
O7 O 2 0.552(10) 0.687(7) 0.071(10) 1 0.87(10)
O8 O 2 0.344(4) 0.184(3) -0.405(3) 1 0.87(10)
O9 O 2 -0.008(13) 0.494(9) -0.190(3) 1 0.87(10)
O10 O 2 -0.113(13) 0.627(10) -0.014(8) 1 0.87(10)
O11 O 2 0.197(2) 0.107(2) -0.1745(19) 1 0.87(10)
O12 O 2 -0.002(4) 0.205(3) -0.345(3) 1 0.87(10)
O13 O 2 0.219(2) 0.526(2) -0.388(2) 1 0.87(10)
C1 C 2 0.476(4) 0.579(3) -0.000(5) 1 0.87(10)
C2 C 2 -0.030(6) 0.531(5) -0.063(2) 1 0.87(10)
C3 C 2 0.0768(18) 0.0283(18) -0.2009(13) 1 0.87(10)
C4 C 2 -0.031(2) 0.078(3) -0.3121(18) 1 0.87(10)
C5 C 2 0.3287(18) 0.630(2) -0.3880(12) 1 0.87(10)
C6 C 2 0.4956(19) 0.595(3) -0.3372(19) 1 0.87(10)
O15 O 2 0.191(3) 0.861(3) -0.962(3) 1 0.87(10)
K2 K 2 0.0474(13) 0.3216(12) -0.6109(10) 1 0.87(10)
K3 K 2 0.3501(13) 0.7773(12) -0.7022(10) 1 0.87(10)
O14 O 2 0.552(4) 1.045(3) -0.769(3) 1 0.87(10)
K1 K 2 -0.2871(15) -0.1501(12) -0.1121(10) 1 0.87(10)
#==============================================================================

# BOND LENGTHS AND ANGLES

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
Eu1 O1 2.57(3) . ?
Eu1 O5 2.48(9) . ?
Eu1 O8 2.55(3) . ?
Eu1 O9 2.50(10) . ?
Eu1 O11 2.449(19) . ?
Eu1 O12 2.48(3) . ?
Eu1 O13 2.44(2) . ?
Eu1 O10 2.50(8) 2_565 ?
Eu1 O7 2.45(9) 2_665 ?
O1 C6 1.28(4) . ?
O2 C3 1.24(2) . ?
O3 C4 1.33(4) . ?
O4 C5 1.20(3) . ?
O5 C1 1.24(7) . ?
O6 C6 1.24(4) . ?
O7 C1 1.25(9) . ?
O9 C2 1.26(5) . ?
O10 C2 1.25(11) . ?
O11 C3 1.19(2) . ?
O12 C4 1.28(4) . ?
O13 C5 1.27(3) . ?
C1 C1 1.58(4) 2_665 ?
C2 C2 1.54(5) 2_565 ?
C3 C4 1.56(2) . ?
C5 C6 1.58(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
O1 Eu1 O5 63.1(16) . . ?
O1 Eu1 O8 70.4(10) . . ?
O1 Eu1 O9 122(2) . . ?
O1 Eu1 O11 120.4(8) . . ?
O1 Eu1 O12 135.2(10) . . ?
O1 Eu1 O13 64.0(7) . . ?
O1 Eu1 O10 129(2) . 2_565 ?
O1 Eu1 O7 68(2) . 2_665 ?
O5 Eu1 O8 131.8(15) . . ?
O5 Eu1 O9 81(2) . . ?
O5 Eu1 O11 129(2) . . ?
O5 Eu1 O12 152.2(16) . . ?
O5 Eu1 O13 83(2) . . ?
O5 Eu1 O10 70(3) . 2_565 ?
O5 Eu1 O7 67(2) . 2_665 ?
O8 Eu1 O9 138.6(13) . . ?
O8 Eu1 O11 66.5(8) . . ?
O8 Eu1 O12 74.1(10) . . ?
O8 Eu1 O13 88.5(8) . . ?
O8 Eu1 O10 142(2) . 2_565 ?
O7 Eu1 O8 85(2) 2_665 . ?
O9 Eu1 O11 117(2) . . ?
O9 Eu1 O12 72(2) . . ?
O9 Eu1 O13 68.5(15) . . ?
O9 Eu1 O10 65(3) . 2_565 ?
O7 Eu1 O9 136(2) 2_665 . ?
O11 Eu1 O12 65.7(8) . . ?
O11 Eu1 O13 147.9(6) . . ?
O10 Eu1 O11 76(2) 2_565 . ?
O7 Eu1 O11 69.1(17) 2_665 . ?
O12 Eu1 O13 89.0(8) . . ?
O10 Eu1 O12 96(2) 2_565 . ?
O7 Eu1 O12 134.6(18) 2_665 . ?
O10 Eu1 O13 128(2) 2_565 . ?
O7 Eu1 O13 130.9(18) 2_665 . ?
O7 Eu1 O10 77(3) 2_665 2_565 ?
Eu1 O1 C6 115.5(17) . . ?
Eu1 O5 C1 121(6) . . ?
Eu1 O7 C1 117(4) 2_665 . ?
Eu1 O9 C2 110(5) . . ?
Eu1 O10 C2 124(5) 2_565 . ?
Eu1 O11 C3 122.7(14) . . ?
Eu1 O12 C4 116(2) . . ?
Eu1 O13 C5 120.3(13) . . ?
O5 C1 O7 126(6) . . ?
O5 C1 C1 112(5) . 2_665 ?
O7 C1 C1 122(5) . 2_665 ?
O9 C2 O10 126(6) . . ?
O9 C2 C2 129(6) . 2_565 ?
O10 C2 C2 105(4) . 2_565 ?
O2 C3 O11 132(2) . . ?
O2 C3 C4 111.7(17) . . ?
O11 C3 C4 112.8(17) . . ?
O3 C4 O12 119(3) . . ?
O3 C4 C3 121(3) . . ?
O12 C4 C3 120(2) . . ?
O4 C5 O13 129.0(17) . . ?
O4 C5 C6 117.3(18) . . ?
O13 C5 C6 113.5(18) . . ?
O1 C6 O6 123(2) . . ?
O1 C6 C5 117(2) . . ?
O6 C6 C5 120(2) . . ?
_exptl_crystal_description       powder
####################################################################### 
# 
# 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_K3GdOx3
_database_code_depnum_ccdc_archive 'CCDC 1963556'
loop_
_audit_author_name
_audit_author_address
'Igor Huskic'
;McGill University
Canada
;
_audit_update_record             
;
2019-11-04 deposited with the CCDC.	2020-05-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_K3GdOx3             
;
PROBLEM: Short Inter D...A Contact  O6       ..O8       .       2.84 Ang.
RESPONSE: O6 and O8 are involved in hydrogen bonding
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        'Tripotassium gadolinium oxalate trihydrate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H6 Gd K3 O15'
_chemical_compound_source        synthetic
_exptl_crystal_recrystallization_method water


_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      100
_chemical_formula_weight         592.66

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   8.4795(8)
_cell_length_b                   9.3708(9)
_cell_length_c                   9.7323(9)
_cell_angle_alpha                98.377(4)
_cell_angle_beta                 91.097(4)
_cell_angle_gamma                96.629(4)
_cell_volume                     759.45(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    45874
_cell_measurement_theta_min      4.830
_cell_measurement_theta_max      66.508


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.592
_exptl_crystal_F_000             566
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    5.270
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7041
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_absorpt_special_details   ?
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed x-ray tube'
_diffrn_measurement_device_type  'Bruker PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            45705
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.078
_diffrn_reflns_theta_max         33.379
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5886
_reflns_number_gt                5474
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX 2, Bruker-AXS'
_computing_cell_refinement       'SAINT V8.35A, Bruker-AXS'
_computing_data_reduction        'SAINT V8.35A, Bruker-AXS'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0178P)²+0.2778P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refU
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5886
_refine_ls_number_parameters     250
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0174
_refine_ls_wR_factor_ref         0.0379
_refine_ls_wR_factor_gt          0.0369
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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
Gd1 Gd 0.27254(2) 0.14227(2) 0.21742(2) 0.01096(2) Uani 1 1 d . . . . .
K1 K 0.78851(5) 0.64177(4) 0.11349(4) 0.02422(7) Uani 1 1 d . . . . .
O1 O 0.64854(16) 0.50408(15) 0.37825(15) 0.0288(3) Uani 1 1 d . . . . .
C1 C 0.53650(18) 0.41830(18) 0.32127(17) 0.0171(3) Uani 1 1 d . . . . .
H1 H 0.135(3) 0.256(3) 0.482(3) 0.049(8) Uiso 1 1 d . . . . .
O2 O 0.47014(16) 0.59343(14) 0.17866(15) 0.0269(3) Uani 1 1 d . . . . .
C2 C 0.42924(18) 0.47309(17) 0.21335(17) 0.0160(3) Uani 1 1 d . . . . .
H2 H 0.226(3) 0.371(3) 0.460(3) 0.040(7) Uiso 1 1 d . . . . .
K2 K 0.54302(5) 0.81727(4) 0.38963(4) 0.02564(8) Uani 1 1 d . . . . .
O3 O 0.50123(14) 0.28703(13) 0.33830(13) 0.0201(2) Uani 1 1 d . . . . .
C3 C 0.53193(18) -0.04233(17) 0.05546(16) 0.0151(3) Uani 1 1 d . . . . .
K3 K 0.15656(5) -0.28067(5) 0.70254(5) 0.02958(9) Uani 1 1 d . . . . .
O4 O 0.30633(14) 0.38813(12) 0.16894(12) 0.0180(2) Uani 1 1 d . . . . .
C4 C -0.02868(17) 0.07543(16) 0.00080(16) 0.0131(3) Uani 1 1 d . . . . .
O5 O 0.48810(15) -0.00936(14) 0.17663(12) 0.0222(2) Uani 1 1 d . . . . .
C5 C 0.00924(18) -0.07462(17) 0.34671(16) 0.0156(3) Uani 1 1 d . . . . .
C6 C 0.17483(19) -0.10782(17) 0.39904(16) 0.0158(3) Uani 1 1 d . . . . .
O6 O 0.62131(15) -0.13551(13) 0.01501(13) 0.0210(2) Uani 1 1 d . . . . .
O7 O 0.05362(13) 0.18258(12) 0.07023(12) 0.0166(2) Uani 1 1 d . . . . .
O8 O -0.15358(14) 0.08138(13) -0.06763(13) 0.0209(2) Uani 1 1 d . . . . .
O9 O 0.28901(14) -0.00830(13) 0.39469(12) 0.0184(2) Uani 1 1 d . . . . .
O10 O 0.01088(14) 0.04303(13) 0.29974(13) 0.0210(2) Uani 1 1 d . . . . .
O11 O 0.18625(17) -0.22536(15) 0.43886(15) 0.0282(3) Uani 1 1 d . . . . .
O12 O -0.10893(15) -0.16442(14) 0.35453(14) 0.0239(3) Uani 1 1 d . . . . .
O13 O 0.16954(16) 0.29991(14) 0.41876(13) 0.0218(2) Uani 1 1 d . . . . .
O14 O 0.7231(2) 0.34363(17) 0.03952(17) 0.0367(4) Uani 1 1 d . . . . .
H4 H 0.769573 0.277193 -0.002335 0.055(9) Uiso 1 1 d G . . . .
H3 H 0.662681 0.348379 -0.017462 0.049(9) Uiso 1 1 d G . . . .
O15 O 1.02824(19) 0.53732(19) 0.2456(2) 0.0391(4) Uani 1 1 d . . . . .
H6 H 1.065788 0.603374 0.310701 0.063(10) Uiso 1 1 d G . . . .
H5 H 1.103374 0.503561 0.215551 0.053(9) Uiso 1 1 d G . . . .


_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
Gd1 O9 2.3943(12) . ?
Gd1 O4 2.4045(12) . ?
Gd1 O3 2.4134(12) . ?
Gd1 O7 2.4204(11) . ?
Gd1 O6 2.4455(12) 2_655 ?
Gd1 O5 2.4455(12) . ?
Gd1 O8 2.4699(12) 2 ?
Gd1 O10 2.4976(12) . ?
Gd1 O13 2.5108(13) . ?
Gd1 K2 4.0530(5) 2_666 ?
Gd1 K3 4.0535(5) 2_556 ?
Gd1 K1 4.1003(5) 2_665 ?
K1 O15 2.7329(16) . ?
K1 O14 2.7698(17) . ?
K1 O2 2.7861(15) . ?
K1 O12 2.8061(14) 1_665 ?
K1 O4 2.8141(12) 2_665 ?
K1 O7 2.8528(12) 2_665 ?
K1 O6 2.9152(12) 1_565 ?
K1 O1 3.2319(16) . ?
K1 C4 3.4796(15) 2_665 ?
K1 C2 3.4890(16) . ?
K1 K2 3.7386(6) . ?
K1 H3 2.9276 . ?
O1 C1 1.2369(19) . ?
O1 K3 2.8463(15) 2_656 ?
O1 K2 3.1530(15) . ?
C1 O3 1.268(2) . ?
C1 C2 1.556(2) . ?
C1 K3 3.0336(16) 2_656 ?
O2 C2 1.237(2) . ?
O2 K2 2.7193(14) . ?
C2 O4 1.2640(18) . ?
C2 K2 3.4471(16) . ?
K2 O9 2.8002(13) 2_666 ?
K2 O9 2.8472(13) 1_565 ?
K2 O5 2.8762(13) 1_565 ?
K2 O12 2.9656(13) 1_665 ?
K2 O3 2.9689(13) 2_666 ?
K2 O11 3.0616(15) 1_565 ?
K2 C6 3.2782(16) 1_565 ?
K2 O13 3.4153(15) 2_666 ?
O3 K3 2.9427(13) 2_656 ?
C3 O6 1.2474(19) . ?
C3 O5 1.2496(19) . ?
C3 C3 1.554(3) 2_655 ?
K3 O11 2.7018(14) . ?
K3 O10 2.7781(13) 2_556 ?
K3 O15 2.8299(18) 2_656 ?
K3 O14 2.8571(17) 2_656 ?
K3 O13 2.9615(15) 2_556 ?
K3 O7 2.9746(13) 2_556 ?
K3 C4 3.4920(16) 2_556 ?
C4 O8 1.2512(18) . ?
C4 O7 1.2547(18) . ?
C4 C4 1.545(3) 2 ?
C5 O12 1.2429(19) . ?
C5 O10 1.252(2) . ?
C5 C6 1.564(2) . ?
C6 O11 1.233(2) . ?
C6 O9 1.2702(19) . ?
O13 H1 0.83(3) . ?
O13 H2 0.82(3) . ?
O14 H4 0.84 . ?
O14 H3 0.7576 . ?
O15 H6 0.85 . ?
O15 H5 0.7863 . ?

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
O9 Gd1 O4 144.71(4) . . ?
O9 Gd1 O3 84.89(4) . . ?
O4 Gd1 O3 66.93(4) . . ?
O9 Gd1 O7 132.25(4) . . ?
O4 Gd1 O7 69.97(4) . . ?
O3 Gd1 O7 136.73(4) . . ?
O9 Gd1 O6 133.26(4) . 2_655 ?
O4 Gd1 O6 73.02(4) . 2_655 ?
O3 Gd1 O6 95.90(4) . 2_655 ?
O7 Gd1 O6 74.84(4) . 2_655 ?
O9 Gd1 O5 68.86(4) . . ?
O4 Gd1 O5 120.08(4) . . ?
O3 Gd1 O5 75.50(4) . . ?
O7 Gd1 O5 132.30(4) . . ?
O6 Gd1 O5 66.25(4) 2_655 . ?
O9 Gd1 O8 85.78(4) . 2 ?
O4 Gd1 O8 129.13(4) . 2 ?
O3 Gd1 O8 150.01(4) . 2 ?
O7 Gd1 O8 67.09(4) . 2 ?
O6 Gd1 O8 70.56(4) 2_655 2 ?
O5 Gd1 O8 74.54(4) . 2 ?
O9 Gd1 O10 65.21(4) . . ?
O4 Gd1 O10 118.79(4) . . ?
O3 Gd1 O10 132.14(4) . . ?
O7 Gd1 O10 68.18(4) . . ?
O6 Gd1 O10 131.90(4) 2_655 . ?
O5 Gd1 O10 121.07(4) . . ?
O8 Gd1 O10 67.36(4) 2 . ?
O9 Gd1 O13 79.81(4) . . ?
O4 Gd1 O13 72.29(4) . . ?
O3 Gd1 O13 73.43(4) . . ?
O7 Gd1 O13 90.26(4) . . ?
O6 Gd1 O13 145.15(4) 2_655 . ?
O5 Gd1 O13 137.29(4) . . ?
O8 Gd1 O13 132.44(4) 2 . ?
O10 Gd1 O13 65.42(4) . . ?
O9 Gd1 K2 42.46(3) . 2_666 ?
O4 Gd1 K2 102.90(3) . 2_666 ?
O3 Gd1 K2 46.62(3) . 2_666 ?
O7 Gd1 K2 146.47(3) . 2_666 ?
O6 Gd1 K2 136.03(3) 2_655 2_666 ?
O5 Gd1 K2 80.30(3) . 2_666 ?
O8 Gd1 K2 127.97(3) 2 2_666 ?
O10 Gd1 K2 89.33(3) . 2_666 ?
O13 Gd1 K2 57.06(3) . 2_666 ?
O9 Gd1 K3 99.82(3) . 2_556 ?
O4 Gd1 K3 76.39(3) . 2_556 ?
O3 Gd1 K3 116.89(3) . 2_556 ?
O7 Gd1 K3 46.77(3) . 2_556 ?
O6 Gd1 K3 120.40(3) 2_655 2_556 ?
O5 Gd1 K3 163.24(3) . 2_556 ?
O8 Gd1 K3 92.78(3) 2 2_556 ?
O10 Gd1 K3 42.41(3) . 2_556 ?
O13 Gd1 K3 46.68(3) . 2_556 ?
K2 Gd1 K3 99.875(10) 2_666 2_556 ?
O9 Gd1 K1 173.09(3) . 2_665 ?
O4 Gd1 K1 41.91(3) . 2_665 ?
O3 Gd1 K1 101.65(3) . 2_665 ?
O7 Gd1 K1 42.93(3) . 2_665 ?
O6 Gd1 K1 44.54(3) 2_655 2_665 ?
O5 Gd1 K1 110.40(3) . 2_665 ?
O8 Gd1 K1 87.42(3) 2 2_665 ?
O10 Gd1 K1 110.89(3) . 2_665 ?
O13 Gd1 K1 104.03(3) . 2_665 ?
K2 Gd1 K1 144.426(9) 2_666 2_665 ?
K3 Gd1 K1 79.287(9) 2_556 2_665 ?
O15 K1 O14 76.73(5) . . ?
O15 K1 O2 123.57(5) . . ?
O14 K1 O2 78.14(5) . . ?
O15 K1 O12 70.50(5) . 1_665 ?
O14 K1 O12 136.80(5) . 1_665 ?
O2 K1 O12 97.15(4) . 1_665 ?
O15 K1 O4 131.86(5) . 2_665 ?
O14 K1 O4 77.09(4) . 2_665 ?
O2 K1 O4 89.00(4) . 2_665 ?
O12 K1 O4 146.10(4) 1_665 2_665 ?
O15 K1 O7 104.49(5) . 2_665 ?
O14 K1 O7 121.02(5) . 2_665 ?
O2 K1 O7 131.72(4) . 2_665 ?
O12 K1 O7 94.35(4) 1_665 2_665 ?
O4 K1 O7 58.44(3) 2_665 2_665 ?
O15 K1 O6 155.72(5) . 1_565 ?
O14 K1 O6 127.18(5) . 1_565 ?
O2 K1 O6 71.61(4) . 1_565 ?
O12 K1 O6 89.88(4) 1_665 1_565 ?
O4 K1 O6 60.46(4) 2_665 1_565 ?
O7 K1 O6 61.66(3) 2_665 1_565 ?
O15 K1 O1 71.04(5) . . ?
O14 K1 O1 71.32(4) . . ?
O2 K1 O1 53.19(4) . . ?
O12 K1 O1 71.90(4) 1_665 . ?
O4 K1 O1 134.36(3) 2_665 . ?
O7 K1 O1 166.24(3) 2_665 . ?
O6 K1 O1 117.29(4) 1_565 . ?
O15 K1 C4 95.66(5) . 2_665 ?
O14 K1 C4 137.14(5) . 2_665 ?
O2 K1 C4 135.14(4) . 2_665 ?
O12 K1 C4 74.57(4) 1_665 2_665 ?
O4 K1 C4 77.65(4) 2_665 2_665 ?
O7 K1 C4 19.87(3) 2_665 2_665 ?
O6 K1 C4 64.49(4) 1_565 2_665 ?
O1 K1 C4 146.39(4) . 2_665 ?
O15 K1 C2 107.69(5) . . ?
O14 K1 C2 62.12(5) . . ?
O2 K1 C2 18.80(4) . . ?
O12 K1 C2 102.02(4) 1_665 . ?
O4 K1 C2 94.45(4) 2_665 . ?
O7 K1 C2 147.22(4) 2_665 . ?
O6 K1 C2 89.90(4) 1_565 . ?
O1 K1 C2 41.56(3) . . ?
C4 K1 C2 153.93(4) 2_665 . ?
O15 K1 K2 106.99(4) . . ?
O14 K1 K2 116.84(4) . . ?
O2 K1 K2 46.48(3) . . ?
O12 K1 K2 51.52(3) 1_665 . ?
O4 K1 K2 120.81(3) 2_665 . ?
O7 K1 K2 118.56(3) 2_665 . ?
O6 K1 K2 68.32(3) 1_565 . ?
O1 K1 K2 53.18(3) . . ?
C4 K1 K2 105.79(3) 2_665 . ?
C2 K1 K2 56.84(3) . . ?
O15 K1 Gd1 138.61(4) . 2_665 ?
O14 K1 Gd1 111.85(4) . 2_665 ?
O2 K1 Gd1 97.64(3) . 2_665 ?
O12 K1 Gd1 111.34(3) 1_665 2_665 ?
O4 K1 Gd1 34.80(2) 2_665 2_665 ?
O7 K1 Gd1 35.30(2) 2_665 2_665 ?
O6 K1 Gd1 36.04(2) 1_565 2_665 ?
O1 K1 Gd1 150.27(3) . 2_665 ?
C4 K1 Gd1 49.53(3) 2_665 2_665 ?
C2 K1 Gd1 111.92(3) . 2_665 ?
K2 K1 Gd1 104.304(13) . 2_665 ?
O15 K1 H3 91.3 . . ?
O14 K1 H3 15.0 . . ?
O2 K1 H3 72.0 . . ?
O12 K1 H3 149.3 1_665 . ?
O4 K1 H3 64.0 2_665 . ?
O7 K1 H3 114.5 2_665 . ?
O6 K1 H3 112.4 1_565 . ?
O1 K1 H3 79.0 . . ?
C4 K1 H3 133.4 2_665 . ?
C2 K1 H3 59.2 . . ?
K2 K1 H3 116.0 . . ?
Gd1 K1 H3 98.7 2_665 . ?
C1 O1 K3 86.51(10) . 2_656 ?
C1 O1 K2 106.21(11) . . ?
K3 O1 K2 154.99(6) 2_656 . ?
C1 O1 K1 100.32(11) . . ?
K3 O1 K1 85.08(4) 2_656 . ?
K2 O1 K1 71.67(3) . . ?
O1 C1 O3 126.76(16) . . ?
O1 C1 C2 117.72(15) . . ?
O3 C1 C2 115.48(13) . . ?
O1 C1 K3 69.48(10) . 2_656 ?
O3 C1 K3 73.77(9) . 2_656 ?
C2 C1 K3 132.79(10) . 2_656 ?
C2 O2 K2 116.07(11) . . ?
C2 O2 K1 114.69(11) . . ?
K2 O2 K1 85.53(4) . . ?
O2 C2 O4 125.93(15) . . ?
O2 C2 C1 118.36(14) . . ?
O4 C2 C1 115.71(14) . . ?
O2 C2 K2 45.12(9) . . ?
O4 C2 K2 141.16(11) . . ?
C1 C2 K2 86.50(8) . . ?
O2 C2 K1 46.52(9) . . ?
O4 C2 K1 143.62(11) . . ?
C1 C2 K1 83.72(8) . . ?
K2 C2 K1 65.23(3) . . ?
O2 K2 O9 161.35(4) . 2_666 ?
O2 K2 O9 106.38(4) . 1_565 ?
O9 K2 O9 92.08(3) 2_666 1_565 ?
O2 K2 O5 83.03(4) . 1_565 ?
O9 K2 O5 105.54(4) 2_666 1_565 ?
O9 K2 O5 57.12(3) 1_565 1_565 ?
O2 K2 O12 94.96(4) . 1_665 ?
O9 K2 O12 68.21(4) 2_666 1_665 ?
O9 K2 O12 140.81(4) 1_565 1_665 ?
O5 K2 O12 94.61(4) 1_565 1_665 ?
O2 K2 O3 110.16(4) . 2_666 ?
O9 K2 O3 68.38(3) 2_666 2_666 ?
O9 K2 O3 99.15(4) 1_565 2_666 ?
O5 K2 O3 155.94(4) 1_565 2_666 ?
O12 K2 O3 103.84(4) 1_665 2_666 ?
O2 K2 O11 83.96(4) . 1_565 ?
O9 K2 O11 112.07(4) 2_666 1_565 ?
O9 K2 O11 44.01(3) 1_565 1_565 ?
O5 K2 O11 90.24(4) 1_565 1_565 ?
O12 K2 O11 174.87(4) 1_665 1_565 ?
O3 K2 O11 71.96(4) 2_666 1_565 ?
O2 K2 O1 54.66(4) . . ?
O9 K2 O1 110.01(4) 2_666 . ?
O9 K2 O1 147.68(4) 1_565 . ?
O5 K2 O1 132.33(4) 1_565 . ?
O12 K2 O1 71.12(4) 1_665 . ?
O3 K2 O1 69.47(4) 2_666 . ?
O11 K2 O1 104.32(4) 1_565 . ?
O2 K2 C6 92.06(4) . 1_565 ?
O9 K2 C6 106.34(4) 2_666 1_565 ?
O9 K2 C6 22.55(4) 1_565 1_565 ?
O5 K2 C6 70.84(4) 1_565 1_565 ?
O12 K2 C6 162.96(4) 1_665 1_565 ?
O3 K2 C6 88.19(4) 2_666 1_565 ?
O11 K2 C6 22.09(4) 1_565 1_565 ?
O1 K2 C6 125.16(4) . 1_565 ?
O2 K2 O13 103.45(4) . 2_666 ?
O9 K2 O13 59.89(3) 2_666 2_666 ?
O9 K2 O13 145.85(4) 1_565 2_666 ?
O5 K2 O13 144.13(4) 1_565 2_666 ?
O12 K2 O13 50.06(3) 1_665 2_666 ?
O3 K2 O13 54.40(3) 2_666 2_666 ?
O11 K2 O13 125.30(4) 1_565 2_666 ?
O1 K2 O13 50.23(3) . 2_666 ?
C6 K2 O13 142.41(4) 1_565 2_666 ?
O2 K2 C2 18.81(4) . . ?
O9 K2 C2 151.71(4) 2_666 . ?
O9 K2 C2 111.12(4) 1_565 . ?
O5 K2 C2 100.74(4) 1_565 . ?
O12 K2 C2 99.71(4) 1_665 . ?
O3 K2 C2 91.35(4) 2_666 . ?
O11 K2 C2 77.70(4) 1_565 . ?
O1 K2 C2 42.29(4) . . ?
C6 K2 C2 91.91(4) 1_565 . ?
O13 K2 C2 92.47(4) 2_666 . ?
O2 K2 K1 47.99(3) . . ?
O9 K2 K1 115.99(3) 2_666 . ?
O9 K2 K1 135.30(3) 1_565 . ?
O5 K2 K1 81.18(3) 1_565 . ?
O12 K2 K1 47.79(3) 1_665 . ?
O3 K2 K1 122.72(3) 2_666 . ?
O11 K2 K1 131.76(3) 1_565 . ?
O1 K2 K1 55.15(3) . . ?
C6 K2 K1 134.10(3) 1_565 . ?
O13 K2 K1 77.97(2) 2_666 . ?
C2 K2 K1 57.93(3) . . ?
C1 O3 Gd1 120.50(10) . . ?
C1 O3 K3 81.80(9) . 2_656 ?
Gd1 O3 K3 131.18(5) . 2_656 ?
C1 O3 K2 125.42(10) . 2_666 ?
Gd1 O3 K2 97.16(4) . 2_666 ?
K3 O3 K2 102.84(4) 2_656 2_666 ?
O6 C3 O5 126.74(15) . . ?
O6 C3 C3 117.09(17) . 2_655 ?
O5 C3 C3 116.18(17) . 2_655 ?
O11 K3 O10 77.39(4) . 2_556 ?
O11 K3 O15 119.71(5) . 2_656 ?
O10 K3 O15 114.75(4) 2_556 2_656 ?
O11 K3 O1 84.98(4) . 2_656 ?
O10 K3 O1 162.25(4) 2_556 2_656 ?
O15 K3 O1 75.86(5) 2_656 2_656 ?
O11 K3 O14 153.48(5) . 2_656 ?
O10 K3 O14 119.63(4) 2_556 2_656 ?
O15 K3 O14 73.82(5) 2_656 2_656 ?
O1 K3 O14 76.20(4) 2_656 2_656 ?
O11 K3 O3 77.65(4) . 2_656 ?
O10 K3 O3 126.65(4) 2_556 2_656 ?
O15 K3 O3 118.59(4) 2_656 2_656 ?
O1 K3 O3 45.47(4) 2_656 2_656 ?
O14 K3 O3 75.83(5) 2_656 2_656 ?
O11 K3 O13 73.28(4) . 2_556 ?
O10 K3 O13 56.16(4) 2_556 2_556 ?
O15 K3 O13 69.31(4) 2_656 2_556 ?
O1 K3 O13 120.54(4) 2_656 2_556 ?
O14 K3 O13 132.58(5) 2_656 2_556 ?
O3 K3 O13 149.11(4) 2_656 2_556 ?
O11 K3 O7 133.08(4) . 2_556 ?
O10 K3 O7 57.16(3) 2_556 2_556 ?
O15 K3 O7 75.13(5) 2_656 2_556 ?
O1 K3 O7 140.48(4) 2_656 2_556 ?
O14 K3 O7 70.35(4) 2_656 2_556 ?
O3 K3 O7 137.85(4) 2_656 2_556 ?
O13 K3 O7 72.15(3) 2_556 2_556 ?
O11 K3 C1 89.11(4) . 2_656 ?
O10 K3 C1 151.08(4) 2_556 2_656 ?
O15 K3 C1 94.16(5) 2_656 2_656 ?
O1 K3 C1 24.02(4) 2_656 2_656 ?
O14 K3 C1 66.22(5) 2_656 2_656 ?
O3 K3 C1 24.43(4) 2_656 2_656 ?
O13 K3 C1 143.59(4) 2_556 2_656 ?
O7 K3 C1 136.54(4) 2_556 2_656 ?
O11 K3 C4 131.42(4) . 2_556 ?
O10 K3 C4 55.46(4) 2_556 2_556 ?
O15 K3 C4 92.64(5) 2_656 2_556 ?
O1 K3 C4 141.00(4) 2_656 2_556 ?
O14 K3 C4 64.81(4) 2_656 2_556 ?
O3 K3 C4 119.71(4) 2_656 2_556 ?
O13 K3 C4 87.95(4) 2_556 2_556 ?
O7 K3 C4 20.43(3) 2_556 2_556 ?
C1 K3 C4 126.18(4) 2_656 2_556 ?
O11 K3 Gd1 99.56(3) . 2_556 ?
O10 K3 Gd1 37.32(3) 2_556 2_556 ?
O15 K3 Gd1 77.74(4) 2_656 2_556 ?
O1 K3 Gd1 151.72(3) 2_656 2_556 ?
O14 K3 Gd1 105.88(4) 2_656 2_556 ?
O3 K3 Gd1 162.78(3) 2_656 2_556 ?
O13 K3 Gd1 38.09(3) 2_556 2_556 ?
O7 K3 Gd1 36.36(2) 2_556 2_556 ?
C1 K3 Gd1 170.26(3) 2_656 2_556 ?
C4 K3 Gd1 49.93(2) 2_556 2_556 ?
O11 K3 K1 132.69(3) . 2_656 ?
O10 K3 K1 145.69(3) 2_556 2_656 ?
O15 K3 K1 41.32(3) 2_656 2_656 ?
O1 K3 K1 51.41(3) 2_656 2_656 ?
O14 K3 K1 42.12(3) 2_656 2_656 ?
O3 K3 K1 81.93(3) 2_656 2_656 ?
O13 K3 K1 110.60(3) 2_556 2_656 ?
O7 K3 K1 89.23(2) 2_556 2_656 ?
C1 K3 K1 59.29(3) 2_656 2_656 ?
C4 K3 K1 95.74(3) 2_556 2_656 ?
Gd1 K3 K1 111.118(12) 2_556 2_656 ?
C2 O4 Gd1 120.49(10) . . ?
C2 O4 K1 119.35(10) . 2_665 ?
Gd1 O4 K1 103.29(4) . 2_665 ?
O8 C4 O7 124.99(14) . . ?
O8 C4 C4 117.43(16) . 2 ?
O7 C4 C4 117.58(16) . 2 ?
O8 C4 K1 99.09(10) . 2_665 ?
O7 C4 K1 50.59(8) . 2_665 ?
C4 C4 K1 120.97(12) 2 2_665 ?
O8 C4 K3 92.85(9) . 2_556 ?
O7 C4 K3 55.84(8) . 2_556 ?
C4 C4 K3 123.83(13) 2 2_556 ?
K1 C4 K3 96.53(4) 2_665 2_556 ?
C3 O5 Gd1 119.28(10) . . ?
C3 O5 K2 121.42(10) . 1_545 ?
Gd1 O5 K2 115.45(4) . 1_545 ?
O12 C5 O10 126.45(15) . . ?
O12 C5 C6 118.65(14) . . ?
O10 C5 C6 114.90(13) . . ?
O11 C6 O9 125.24(15) . . ?
O11 C6 C5 119.37(14) . . ?
O9 C6 C5 115.39(14) . . ?
O11 C6 K2 69.03(10) . 1_545 ?
O9 C6 K2 59.29(8) . 1_545 ?
C5 C6 K2 159.42(10) . 1_545 ?
C3 O6 Gd1 118.86(10) . 2_655 ?
C3 O6 K1 141.46(10) . 1_545 ?
Gd1 O6 K1 99.42(4) 2_655 1_545 ?
C4 O7 Gd1 119.25(10) . . ?
C4 O7 K1 109.54(10) . 2_665 ?
Gd1 O7 K1 101.76(4) . 2_665 ?
C4 O7 K3 103.73(9) . 2_556 ?
Gd1 O7 K3 96.88(4) . 2_556 ?
K1 O7 K3 126.43(4) 2_665 2_556 ?
C4 O8 Gd1 117.74(10) . 2 ?
C6 O9 Gd1 117.11(10) . . ?
C6 O9 K2 130.17(10) . 2_666 ?
Gd1 O9 K2 102.29(4) . 2_666 ?
C6 O9 K2 98.16(10) . 1_545 ?
Gd1 O9 K2 118.27(5) . 1_545 ?
K2 O9 K2 87.92(3) 2_666 1_545 ?
C5 O10 Gd1 115.55(10) . . ?
C5 O10 K3 142.55(11) . 2_556 ?
Gd1 O10 K3 100.27(4) . 2_556 ?
C6 O11 K3 125.89(12) . . ?
C6 O11 K2 88.88(10) . 1_545 ?
K3 O11 K2 106.45(5) . 1_545 ?
C5 O12 K1 117.59(10) . 1_445 ?
C5 O12 K2 141.27(11) . 1_445 ?
K1 O12 K2 80.69(3) 1_445 1_445 ?
Gd1 O13 K3 95.23(4) . 2_556 ?
Gd1 O13 K2 84.84(4) . 2_666 ?
K3 O13 K2 153.22(5) 2_556 2_666 ?
Gd1 O13 H1 115(2) . . ?
K3 O13 H1 90(2) 2_556 . ?
K2 O13 H1 66(2) 2_666 . ?
Gd1 O13 H2 120.7(19) . . ?
K3 O13 H2 129.0(19) 2_556 . ?
K2 O13 H2 71.4(19) 2_666 . ?
H1 O13 H2 104(3) . . ?
K1 O14 K3 94.11(5) . 2_656 ?
K1 O14 H4 136 . . ?
K3 O14 H4 89(2) 2_656 . ?
K1 O14 H3 94.4 . . ?
K3 O14 H3 158.2 2_656 . ?
H4 O14 H3 98.2 . . ?
K1 O15 K3 95.54(5) . 2_656 ?
K1 O15 H6 107 . . ?
K3 O15 H6 122(2) 2_656 . ?
K1 O15 H5 130.2 . . ?
K3 O15 H5 99.3 2_656 . ?
H6 O15 H5 104.1 . . ?

_refine_diff_density_max         0.748
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.107

####################################################################### 
# 
# 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_Lu_ox
_database_code_depnum_ccdc_archive 'CCDC 1963552'
loop_
_audit_author_name
_audit_author_address
'Igor Huskic'
;McGill University
Canada
;
_audit_update_record             
;
2019-11-04 deposited with the CCDC.	2020-05-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT699_Lu_ox               
;
PROBLEM: Missing _exptl_crystal_description Value .......     Please Do !
RESPONSE: Structure solved from powder data
;
# Added during the CSD deposition process: Monday 04 November 2019 03:30 PM
# end Validation Reply Form


_chemical_name_systematic        
; ?
;
_chemical_name_common            
"catena-(tetra-aqua-tris(m2-oxalato-O,O',O'',O''')-di-lutecium(iii)) dihydrate"
_chemical_formula_moiety         'C3 Lu O8, O'
_chemical_formula_analytical     ?
_chemical_formula_sum            'C3 Lu O9'
_chemical_formula_weight         355.00


#==============================================================================

# POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      triclinic
_symmetry_space_group_name_H-M   P-1
_space_group_name_Hall           '-p 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z '
'-x, -y, -z '
_cell_length_a                   9.5867(2)
_cell_length_b                   6.64358(16)
_cell_length_c                   6.25859(16)
_cell_angle_alpha                98.1966(17)
_cell_angle_beta                 99.4509(19)
_cell_angle_gamma                75.113(2)
_cell_volume                     377.890(16)

_cell_formula_units_Z            2
_cell_measurement_temperature    293
_cell_measurement_theta_min      4
_cell_measurement_theta_max      100
_cell_measurement_reflns_used    20
_exptl_crystal_density_diffrn    3.1199(1)
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             322
_cell_special_details            
; ?
;



# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
; 'packed powder pellet'
;
_pd_spec_mount_mode              resflection

_pd_spec_shape                   flat_sheet

_pd_char_particle_morphology     ?
_pd_char_colour                  white # use ICDD colour descriptions



_pd_prep_temperature             293


#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      293
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              ?
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_source_voltage           40
_diffrn_source_current           30
_diffrn_measurement_device_type  'Bruker D2 PHASER'
_diffrn_detector                 'Position Sensitive Detector'
_diffrn_detector_type            LYNXEYE
_pd_meas_scan_method             cont

_pd_meas_special_details         
;  ?
;

# The following six items are used for angular dispersive measurements only.

_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_monochromator  none

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        4264
_pd_meas_2theta_range_min        3.010
_pd_meas_2theta_range_max        90.000
_pd_meas_2theta_range_inc        0.0199




#==============================================================================

# REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.


# The next three items are given as text.

_pd_proc_ls_profile_function     pseudo-Voigt
_pd_proc_ls_background_function  'Chebyshev polynomial'


_pd_proc_ls_prof_R_factor        0.011
_pd_proc_ls_prof_wR_factor       0.052
_pd_proc_ls_prof_wR_expected     0.010
_refine_ls_R_I_factor            0.027


_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_parameters     53
_refine_ls_number_restraints     12
_refine_ls_number_constraints    18

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   5.391


# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        8
_pd_proc_2theta_range_max        90
_pd_proc_2theta_range_inc        0.0199
_pd_proc_wavelength              1.5418

#


# The following items are used to identify the programs used.

_computing_data_collection       'Bruker DIFFRAC.SUITE'
_computing_cell_refinement       'TOPAS Academic v. 6'
_computing_structure_solution    'TOPAS Academic v. 6'
_computing_structure_refinement  'TOPAS Academic v. 6'
_computing_molecular_graphics    ?
_computing_publication_material  ?


#==============================================================================


# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Lu1 Lu 2 0.80625(17) 0.3105(3) -0.8006(3) 1 0.36(5)
C1a C 2 0.0708(10) 1.025(4) -0.530(4) 1 1.80(14)
O1a O 2 0.046(6) 1.160(7) -0.662(8) 1 1.80(14)
O2a O 2 0.190(3) 0.926(9) -0.438(10) 1 1.80(14)
C1b C 2 0.021(2) -0.600(2) 0.914(3) 1 1.80(14)
O1b O 2 -0.035(4) -0.748(4) 0.930(7) 1 1.80(14)
O2b O 2 0.104(4) -0.586(6) 0.785(5) 1 1.80(14)
C1c C 2 0.4712(14) 0.455(4) -0.912(3) 1 1.80(14)
O1c O 2 0.3358(16) 0.510(6) -0.911(9) 1 1.80(14)
O2c O 2 0.568(3) 0.341(9) -0.792(10) 1 1.80(14)
Ow O 2 0.2458(17) -0.030(2) -0.938(2) 1 1.80(14)
Ow2 O 2 0.5304(15) -0.080(2) -0.736(2) 1 1.80(14)
Ow3 O 2 0.7580(17) -0.448(2) -0.470(2) 1 1.80(14)
#==============================================================================

# BOND LENGTHS AND ANGLES

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
Lu1 O2C 2.25(3) . ?
Lu1 Ow3 2.461(13) 1_565 ?
Lu1 O1A 2.33(6) 1_645 ?
Lu1 O1B 2.38(4) 1_663 ?
Lu1 Ow 2.396(13) 2_653 ?
Lu1 O2B 2.20(4) 2_655 ?
Lu1 O1C 2.35(5) 2_663 ?
Lu1 O2A 2.31(6) 2_664 ?
O1A C1A 1.26(5) . ?
O1B C1B 1.26(4) . ?
O1C C1C 1.26(3) . ?
O2A C1A 1.26(5) . ?
O2B C1B 1.25(4) . ?
O2C C1C 1.25(6) . ?
C1A C1A 1.59(2) 2_574 ?
C1B C1B 1.60(2) 2_547 ?
C1C C1C 1.56(3) 2_663 ?



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
O2C Lu1 Ow3 77.1(16) . 1_565 ?
O1A Lu1 O2C 147(2) 1_645 . ?
O1B Lu1 O2C 137.3(19) 1_663 . ?
Ow Lu1 O2C 77.2(16) 2_653 . ?
O2B Lu1 O2C 121.8(18) 2_655 . ?
O1C Lu1 O2C 69.3(17) 2_663 . ?
O2A Lu1 O2C 77.4(18) 2_664 . ?
O1A Lu1 Ow3 94.2(12) 1_645 1_565 ?
O1B Lu1 Ow3 137.1(9) 1_663 1_565 ?
Ow Lu1 Ow3 151.1(5) 2_653 1_565 ?
O2B Lu1 Ow3 68.0(9) 2_655 1_565 ?
O1C Lu1 Ow3 105.1(12) 2_663 1_565 ?
O2A Lu1 Ow3 80.1(15) 2_664 1_565 ?
O1A Lu1 O1B 68.6(16) 1_645 1_663 ?
Ow Lu1 O1A 100.2(12) 2_653 1_645 ?
O1A Lu1 O2B 81.9(16) 1_645 2_655 ?
O1A Lu1 O1C 142.8(14) 1_645 2_663 ?
O1A Lu1 O2A 69.9(16) 1_645 2_664 ?
Ow Lu1 O1B 71.8(9) 2_653 1_663 ?
O1B Lu1 O2B 70.8(12) 1_663 2_655 ?
O1B Lu1 O1C 75.8(12) 1_663 2_663 ?
O1B Lu1 O2A 124.7(14) 1_663 2_664 ?
Ow Lu1 O2B 138.7(9) 2_653 2_655 ?
Ow Lu1 O1C 77.7(11) 2_653 2_663 ?
Ow Lu1 O2A 81.5(15) 2_653 2_664 ?
O1C Lu1 O2B 76.7(12) 2_663 2_655 ?
O2A Lu1 O2B 135.4(16) 2_664 2_655 ?
O1C Lu1 O2A 143.8(12) 2_663 2_664 ?
Lu1 O1A C1A 120(4) 1_465 . ?
Lu1 O1B C1B 117(2) 1_447 . ?
Lu1 O1C C1C 118(3) 2_663 . ?
Lu1 O2A C1A 120(3) 2_664 . ?
Lu1 O2B C1B 123(2) 2_655 . ?
Lu1 O2C C1C 122(3) . . ?
O1A C1A O2A 130(4) . . ?
O1A C1A C1A 115(3) . 2_574 ?
O2A C1A C1A 116(3) . 2_574 ?
O1B C1B O2B 130(3) . . ?
O1B C1B C1B 114(2) . 2_547 ?
O2B C1B C1B 116(2) . 2_547 ?
O1C C1C O2C 130(3) . . ?
O1C C1C C1C 115(3) . 2_663 ?
O2C C1C C1C 115(2) . 2_663 ?
####################################################################### 
# 
# 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_K3ScOx3
_database_code_depnum_ccdc_archive 'CCDC 1963555'
loop_
_audit_author_name
_audit_author_address
'Igor Huskic'
;McGill University
Canada
;
_audit_update_record             
;
2019-11-04 deposited with the CCDC.	2020-05-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_K3ScOx3             
;
PROBLEM: Short Inter D-H..H-D       H2       ..H4       .       2.09 Ang.
RESPONSE: H2 and H4 are involved in hydrogen bonding
;
# Added during the CSD deposition process: Monday 04 November 2019 03:30 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        'Potassium scandium oxalate'
_chemical_name_common            ?
_chemical_formula_moiety         '3K+, [ScC6O12]3-, 2[H2O]'
_chemical_formula_sum            'C6 H8 K3 O16 Sc'
_chemical_compound_source        synthetic
_exptl_crystal_recrystallization_method water
_chemical_melting_point          ?

_exptl_crystal_description       'monoclinic block'
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      100
_chemical_formula_weight         498.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.2519 0.3716 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yn'
_chemical_absolute_configuration .

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

_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.
;

_cell_length_a                   11.4151(8)
_cell_length_b                   12.6781(9)
_cell_length_c                   11.4093(8)
_cell_angle_alpha                90
_cell_angle_beta                 111.900(2)
_cell_angle_gamma                90
_cell_volume                     1532.02(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19621
_cell_measurement_theta_min      5.005
_cell_measurement_theta_max      55.006
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.161
_exptl_crystal_F_000             1000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    1.385
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6898
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS-2012/1, G. Sheldrick'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed x-ray tube'
_diffrn_measurement_device_type  'Bruker PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18855
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.687
_diffrn_reflns_theta_max         27.534
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             1741
_reflns_number_gt                1719
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX 2, Bruker-AXS'
_computing_cell_refinement       'SAINT V8.35A, Bruker-AXS'
_computing_data_reduction        'SAINT V8.35A, Bruker-AXS'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0254P)²+1.5421P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1741
_refine_ls_number_parameters     135
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0180
_refine_ls_wR_factor_ref         0.0478
_refine_ls_wR_factor_gt          0.0474
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_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
Sc1 Sc 0.500000 0.56058(2) 0.750000 0.00465(8) Uani 1 2 d S T P . .
K1 K 0.500000 0.23448(2) 0.750000 0.00878(9) Uani 1 2 d S T P . .
O1 O 0.46675(7) 0.42628(6) 0.61277(7) 0.00731(15) Uani 1 1 d . . . . .
C1 C 0.48083(9) 0.44380(7) 0.51031(10) 0.0057(2) Uani 1 1 d . . . . .
O2 O 0.46548(7) 0.38015(6) 0.42208(7) 0.00771(15) Uani 1 1 d . . . . .
C2 C 0.25800(10) 0.68673(9) 0.65758(9) 0.0079(2) Uani 1 1 d . . . . .
O3 O 0.30588(7) 0.50597(6) 0.70645(7) 0.00931(16) Uani 1 1 d . . . . .
C3 C 0.21698(10) 0.57230(9) 0.67231(10) 0.0084(2) Uani 1 1 d . . . . .
H3 H 0.7303(19) 0.1081(15) 0.3853(19) 0.029(5) Uiso 1 1 d . . . . .
H4 H 0.663(2) 0.0376(17) 0.317(2) 0.041(6) Uiso 1 1 d . . . . .
O4 O 0.37563(7) 0.69729(6) 0.68176(7) 0.00811(15) Uani 1 1 d . . . . .
O5 O 0.17768(8) 0.75776(7) 0.62596(8) 0.01306(17) Uani 1 1 d . . . . .
O7 O 0.31270(9) 0.14710(7) 0.53583(9) 0.01461(17) Uani 1 1 d . . . . .
O6 O 0.10405(8) 0.55406(6) 0.65353(8) 0.01293(17) Uani 1 1 d . . . . .
H2 H 0.314(2) 0.0813(18) 0.549(2) 0.042(6) Uiso 1 1 d . . . . .
K2 K 0.47908(2) 0.16527(2) 0.41175(2) 0.01028(8) Uani 1 1 d . . . . .
H1 H 0.244(3) 0.159(2) 0.494(3) 0.060(8) Uiso 1 1 d . . . . .
O8 O 0.68034(10) 0.06552(7) 0.38664(10) 0.0198(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sc1 O4 2.1911(8) . ?
Sc1 O4 2.1911(8) 2_656 ?
Sc1 O3 2.1943(8) 2_656 ?
Sc1 O3 2.1943(8) . ?
Sc1 O1 2.2475(8) 2_656 ?
Sc1 O1 2.2475(8) . ?
Sc1 O2 2.2697(8) 6_566 ?
Sc1 O2 2.2697(8) 5_666 ?
Sc1 K2 3.9838(4) 6_566 ?
Sc1 K2 3.9838(4) 5_666 ?
Sc1 K1 4.1344(5) . ?
K1 O7 2.8057(9) . ?
K1 O7 2.8057(9) 2_656 ?
K1 O1 2.8400(8) . ?
K1 O1 2.8400(8) 2_656 ?
K1 O5 2.8888(8) 3_545 ?
K1 O5 2.8888(8) 4_546 ?
K1 O6 2.9715(9) 4_546 ?
K1 O6 2.9715(9) 3_545 ?
K1 C2 3.5310(11) 4_546 ?
K1 C2 3.5310(11) 3_545 ?
K1 K2 3.8773(4) . ?
K1 K2 3.8773(4) 2_656 ?
O1 C1 1.2577(13) . ?
C1 O2 1.2505(13) . ?
C1 C1 1.5345(19) 5_666 ?
O2 K2 2.7336(8) . ?
C2 O5 1.2388(14) . ?
C2 O4 1.2731(13) . ?
C2 C3 1.5527(15) . ?
C2 K2 3.3788(11) 3_455 ?
O3 C3 1.2624(14) . ?
C3 O6 1.2471(14) . ?
C3 K2 3.4029(11) 3_455 ?
O4 K2 2.8714(8) 5_666 ?
O4 K2 3.0007(8) 6_566 ?
O5 K2 2.8904(9) 3_455 ?
O7 K2 2.7695(9) . ?
O7 H2 0.85(2) . ?
O7 H1 0.76(3) . ?
O6 K2 2.9429(9) 7_556 ?
O6 K2 2.9492(9) 3_455 ?
K2 O8 2.7296(10) . ?
K2 K2 3.8942(5) 2_655 ?
K2 H3 3.08(2) . ?
K2 H2 3.05(2) . ?
O8 H3 0.79(2) . ?
O8 H4 0.83(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
O4 Sc1 O4 75.44(4) . 2_656 ?
O4 Sc1 O3 142.73(3) . 2_656 ?
O4 Sc1 O3 72.75(3) 2_656 2_656 ?
O4 Sc1 O3 72.75(3) . . ?
O4 Sc1 O3 142.73(3) 2_656 . ?
O3 Sc1 O3 143.21(4) 2_656 . ?
O4 Sc1 O1 139.95(3) . 2_656 ?
O4 Sc1 O1 115.66(3) 2_656 2_656 ?
O3 Sc1 O1 73.10(3) 2_656 2_656 ?
O3 Sc1 O1 79.20(3) . 2_656 ?
O4 Sc1 O1 115.66(3) . . ?
O4 Sc1 O1 139.95(3) 2_656 . ?
O3 Sc1 O1 79.20(3) 2_656 . ?
O3 Sc1 O1 73.10(3) . . ?
O1 Sc1 O1 81.50(4) 2_656 . ?
O4 Sc1 O2 75.34(3) . 6_566 ?
O4 Sc1 O2 74.29(3) 2_656 6_566 ?
O3 Sc1 O2 113.27(3) 2_656 6_566 ?
O3 Sc1 O2 79.27(3) . 6_566 ?
O1 Sc1 O2 71.76(3) 2_656 6_566 ?
O1 Sc1 O2 144.56(3) . 6_566 ?
O4 Sc1 O2 74.29(3) . 5_666 ?
O4 Sc1 O2 75.34(3) 2_656 5_666 ?
O3 Sc1 O2 79.28(3) 2_656 5_666 ?
O3 Sc1 O2 113.27(3) . 5_666 ?
O1 Sc1 O2 144.56(3) 2_656 5_666 ?
O1 Sc1 O2 71.76(3) . 5_666 ?
O2 Sc1 O2 141.33(4) 6_566 5_666 ?
O4 Sc1 K2 48.06(2) . 6_566 ?
O4 Sc1 K2 44.62(2) 2_656 6_566 ?
O3 Sc1 K2 113.60(2) 2_656 6_566 ?
O3 Sc1 K2 98.64(2) . 6_566 ?
O1 Sc1 K2 111.22(2) 2_656 6_566 ?
O1 Sc1 K2 163.72(2) . 6_566 ?
O2 Sc1 K2 41.47(2) 6_566 6_566 ?
O2 Sc1 K2 99.88(2) 5_666 6_566 ?
O4 Sc1 K2 44.62(2) . 5_666 ?
O4 Sc1 K2 48.06(2) 2_656 5_666 ?
O3 Sc1 K2 98.64(2) 2_656 5_666 ?
O3 Sc1 K2 113.60(2) . 5_666 ?
O1 Sc1 K2 163.72(2) 2_656 5_666 ?
O1 Sc1 K2 111.22(2) . 5_666 ?
O2 Sc1 K2 99.88(2) 6_566 5_666 ?
O2 Sc1 K2 41.47(2) 5_666 5_666 ?
K2 Sc1 K2 58.517(9) 6_566 5_666 ?
O4 Sc1 K1 142.28(2) . . ?
O4 Sc1 K1 142.28(2) 2_656 . ?
O3 Sc1 K1 71.60(2) 2_656 . ?
O3 Sc1 K1 71.61(2) . . ?
O1 Sc1 K1 40.75(2) 2_656 . ?
O1 Sc1 K1 40.75(2) . . ?
O2 Sc1 K1 109.33(2) 6_566 . ?
O2 Sc1 K1 109.33(2) 5_666 . ?
K2 Sc1 K1 150.742(4) 6_566 . ?
K2 Sc1 K1 150.742(4) 5_666 . ?
O7 K1 O7 133.49(4) . 2_656 ?
O7 K1 O1 87.49(2) . . ?
O7 K1 O1 136.05(3) 2_656 . ?
O7 K1 O1 136.05(3) . 2_656 ?
O7 K1 O1 87.49(2) 2_656 2_656 ?
O1 K1 O1 62.20(3) . 2_656 ?
O7 K1 O5 93.43(3) . 3_545 ?
O7 K1 O5 91.19(3) 2_656 3_545 ?
O1 K1 O5 67.44(2) . 3_545 ?
O1 K1 O5 102.05(2) 2_656 3_545 ?
O7 K1 O5 91.19(3) . 4_546 ?
O7 K1 O5 93.43(3) 2_656 4_546 ?
O1 K1 O5 102.05(2) . 4_546 ?
O1 K1 O5 67.44(2) 2_656 4_546 ?
O5 K1 O5 168.27(4) 3_545 4_546 ?
O7 K1 O6 74.85(3) . 4_546 ?
O7 K1 O6 69.73(3) 2_656 4_546 ?
O1 K1 O6 150.88(2) . 4_546 ?
O1 K1 O6 116.40(2) 2_656 4_546 ?
O5 K1 O6 135.30(3) 3_545 4_546 ?
O5 K1 O6 56.39(2) 4_546 4_546 ?
O7 K1 O6 69.73(3) . 3_545 ?
O7 K1 O6 74.85(3) 2_656 3_545 ?
O1 K1 O6 116.40(2) . 3_545 ?
O1 K1 O6 150.88(2) 2_656 3_545 ?
O5 K1 O6 56.39(2) 3_545 3_545 ?
O5 K1 O6 135.30(3) 4_546 3_545 ?
O6 K1 O6 79.33(3) 4_546 3_545 ?
O7 K1 C2 75.10(3) . 4_546 ?
O7 K1 C2 96.99(3) 2_656 4_546 ?
O1 K1 C2 110.89(2) . 4_546 ?
O1 K1 C2 86.39(2) 2_656 4_546 ?
O5 K1 C2 168.53(2) 3_545 4_546 ?
O5 K1 C2 19.09(2) 4_546 4_546 ?
O6 K1 C2 42.63(2) 4_546 4_546 ?
O6 K1 C2 118.15(3) 3_545 4_546 ?
O7 K1 C2 96.99(3) . 3_545 ?
O7 K1 C2 75.10(3) 2_656 3_545 ?
O1 K1 C2 86.39(2) . 3_545 ?
O1 K1 C2 110.89(2) 2_656 3_545 ?
O5 K1 C2 19.09(2) 3_545 3_545 ?
O5 K1 C2 168.53(2) 4_546 3_545 ?
O6 K1 C2 118.15(3) 4_546 3_545 ?
O6 K1 C2 42.63(2) 3_545 3_545 ?
C2 K1 C2 160.26(4) 4_546 3_545 ?
O7 K1 K2 45.554(19) . . ?
O7 K1 K2 121.44(2) 2_656 . ?
O1 K1 K2 72.486(16) . . ?
O1 K1 K2 133.508(17) 2_656 . ?
O5 K1 K2 47.881(18) 3_545 . ?
O5 K1 K2 135.801(17) 4_546 . ?
O6 K1 K2 108.044(19) 4_546 . ?
O6 K1 K2 48.842(17) 3_545 . ?
C2 K1 K2 120.654(17) 4_546 . ?
C2 K1 K2 54.024(17) 3_545 . ?
O7 K1 K2 121.44(2) . 2_656 ?
O7 K1 K2 45.553(19) 2_656 2_656 ?
O1 K1 K2 133.508(17) . 2_656 ?
O1 K1 K2 72.486(16) 2_656 2_656 ?
O5 K1 K2 135.800(17) 3_545 2_656 ?
O5 K1 K2 47.881(18) 4_546 2_656 ?
O6 K1 K2 48.842(17) 4_546 2_656 ?
O6 K1 K2 108.044(18) 3_545 2_656 ?
C2 K1 K2 54.025(17) 4_546 2_656 ?
C2 K1 K2 120.654(17) 3_545 2_656 ?
K2 K1 K2 153.843(12) . 2_656 ?
C1 O1 Sc1 117.83(6) . . ?
C1 O1 K1 128.79(6) . . ?
Sc1 O1 K1 108.15(3) . . ?
O2 C1 O1 127.32(9) . . ?
O2 C1 C1 115.99(11) . 5_666 ?
O1 C1 C1 116.69(11) . 5_666 ?
C1 O2 Sc1 117.73(7) . 5_666 ?
C1 O2 K2 133.21(7) . . ?
Sc1 O2 K2 105.17(3) 5_666 . ?
O5 C2 O4 126.36(10) . . ?
O5 C2 C3 119.37(9) . . ?
O4 C2 C3 114.27(9) . . ?
O5 C2 K2 56.70(6) . 3_455 ?
O4 C2 K2 141.22(7) . 3_455 ?
C3 C2 K2 77.63(5) . 3_455 ?
O5 C2 K1 49.71(5) . 3_455 ?
O4 C2 K1 147.89(7) . 3_455 ?
C3 C2 K1 79.00(5) . 3_455 ?
K2 C2 K1 68.23(2) 3_455 3_455 ?
C3 O3 Sc1 119.16(7) . . ?
O6 C3 O3 126.15(10) . . ?
O6 C3 C2 119.26(10) . . ?
O3 C3 C2 114.56(9) . . ?
O6 C3 K2 58.48(6) . 3_455 ?
O3 C3 K2 142.00(7) . 3_455 ?
C2 C3 K2 75.90(5) . 3_455 ?
C2 O4 Sc1 119.02(7) . . ?
C2 O4 K2 133.79(7) . 5_666 ?
Sc1 O4 K2 102.97(3) . 5_666 ?
C2 O4 K2 106.85(6) . 6_566 ?
Sc1 O4 K2 99.04(3) . 6_566 ?
K2 O4 K2 83.05(2) 5_666 6_566 ?
C2 O5 K1 111.20(7) . 3_455 ?
C2 O5 K2 102.31(7) . 3_455 ?
K1 O5 K2 84.27(2) 3_455 3_455 ?
K2 O7 K1 88.12(3) . . ?
K2 O7 H2 101.5(15) . . ?
K1 O7 H2 105.9(15) . . ?
K2 O7 H1 113(2) . . ?
K1 O7 H1 137.9(19) . . ?
H2 O7 H1 105(2) . . ?
C3 O6 K2 115.71(7) . 7_556 ?
C3 O6 K2 100.39(7) . 3_455 ?
K2 O6 K2 102.55(3) 7_556 3_455 ?
C3 O6 K1 108.91(7) . 3_455 ?
K2 O6 K1 133.27(3) 7_556 3_455 ?
K2 O6 K1 81.82(2) 3_455 3_455 ?
O8 K2 O2 122.00(3) . . ?
O8 K2 O7 141.22(3) . . ?
O2 K2 O7 90.00(3) . . ?
O8 K2 O4 67.47(3) . 5_666 ?
O2 K2 O4 57.40(2) . 5_666 ?
O7 K2 O4 147.32(3) . 5_666 ?
O8 K2 O5 81.45(3) . 3_545 ?
O2 K2 O5 66.33(2) . 3_545 ?
O7 K2 O5 94.17(3) . 3_545 ?
O4 K2 O5 71.85(2) 5_666 3_545 ?
O8 K2 O6 74.94(3) . 7_556 ?
O2 K2 O6 159.13(3) . 7_556 ?
O7 K2 O6 80.38(3) . 7_556 ?
O4 K2 O6 130.98(2) 5_666 7_556 ?
O5 K2 O6 132.42(2) 3_545 7_556 ?
O8 K2 O6 75.18(3) . 3_545 ?
O2 K2 O6 116.85(2) . 3_545 ?
O7 K2 O6 70.53(3) . 3_545 ?
O4 K2 O6 119.52(2) 5_666 3_545 ?
O5 K2 O6 56.62(2) 3_545 3_545 ?
O6 K2 O6 77.45(3) 7_556 3_545 ?
O8 K2 O4 104.44(3) . 6_565 ?
O2 K2 O4 56.56(2) . 6_565 ?
O7 K2 O4 111.97(3) . 6_565 ?
O4 K2 O4 54.28(3) 5_666 6_565 ?
O5 K2 O4 115.63(2) 3_545 6_565 ?
O6 K2 O4 110.05(2) 7_556 6_565 ?
O6 K2 O4 172.25(2) 3_545 6_565 ?
O8 K2 C2 63.58(3) . 3_545 ?
O2 K2 C2 86.28(3) . 3_545 ?
O7 K2 C2 101.30(3) . 3_545 ?
O4 K2 C2 76.32(2) 5_666 3_545 ?
O5 K2 C2 20.99(2) 3_545 3_545 ?
O6 K2 C2 113.66(3) 7_556 3_545 ?
O6 K2 C2 44.33(2) 3_545 3_545 ?
O4 K2 C2 128.38(2) 6_565 3_545 ?
O8 K2 C3 60.17(3) . 3_545 ?
O2 K2 C3 110.32(3) . 3_545 ?
O7 K2 C3 90.03(3) . 3_545 ?
O4 K2 C3 98.71(2) 5_666 3_545 ?
O5 K2 C3 44.21(2) 3_545 3_545 ?
O6 K2 C3 88.32(3) 7_556 3_545 ?
O6 K2 C3 21.13(2) 3_545 3_545 ?
O4 K2 C3 152.95(2) 6_565 3_545 ?
C2 K2 C3 26.47(2) 3_545 3_545 ?
O8 K2 K1 117.88(2) . . ?
O2 K2 K1 73.440(17) . . ?
O7 K2 K1 46.323(19) . . ?
O4 K2 K1 113.756(17) 5_666 . ?
O5 K2 K1 47.845(17) 3_545 . ?
O6 K2 K1 111.103(18) 7_556 . ?
O6 K2 K1 49.340(17) 3_545 . ?
O4 K2 K1 126.656(17) 6_565 . ?
C2 K2 K1 57.750(18) 3_545 . ?
C3 K2 K1 58.401(19) 3_545 . ?
O8 K2 K2 59.67(2) . 2_655 ?
O2 K2 K2 94.007(16) . 2_655 ?
O7 K2 K2 146.55(2) . 2_655 ?
O4 K2 K2 49.898(16) 5_666 2_655 ?
O5 K2 K2 117.816(19) 3_545 2_655 ?
O6 K2 K2 84.382(17) 7_556 2_655 ?
O6 K2 K2 134.346(18) 3_545 2_655 ?
O4 K2 K2 47.049(15) 6_565 2_655 ?
C2 K2 K2 112.09(2) 3_545 2_655 ?
C3 K2 K2 119.21(2) 3_545 2_655 ?
K1 K2 K2 163.651(8) . 2_655 ?
O8 K2 H3 14.0(4) . . ?
O2 K2 H3 108.0(4) . . ?
O7 K2 H3 150.6(4) . . ?
O4 K2 H3 54.4(4) 5_666 . ?
O5 K2 H3 73.3(4) 3_545 . ?
O6 K2 H3 88.7(4) 7_556 . ?
O6 K2 H3 80.6(4) 3_545 . ?
O4 K2 H3 97.4(4) 6_565 . ?
C2 K2 H3 58.5(4) 3_545 . ?
C3 K2 H3 62.3(4) 3_545 . ?
K1 K2 H3 115.9(4) . . ?
K2 K2 H3 57.3(4) 2_655 . ?
O8 K2 H2 126.6(4) . . ?
O2 K2 H2 105.7(4) . . ?
O7 K2 H2 15.8(4) . . ?
O4 K2 H2 162.5(4) 5_666 . ?
O5 K2 H2 98.4(4) 3_545 . ?
O6 K2 H2 66.3(4) 7_556 . ?
O6 K2 H2 61.9(4) 3_545 . ?
O4 K2 H2 122.3(4) 6_565 . ?
C2 K2 H2 99.9(4) 3_545 . ?
C3 K2 H2 82.8(4) 3_545 . ?
K1 K2 H2 52.3(4) . . ?
K2 K2 H2 143.4(4) 2_655 . ?
H3 K2 H2 137.9(6) . . ?
K2 O8 H3 109.1(14) . . ?
K2 O8 H4 112.9(15) . . ?
H3 O8 H4 101(2) . . ?

_refine_diff_density_max         0.626
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.059

