# Supplementary Information (SI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2024

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

data_mo_ErCOB_100K_0m_b
_database_code_depnum_ccdc_archive 'CCDC 2372139'
loop_
_audit_author_name
_audit_author_address

'fatiha azrour romain viennois jerome long dominique granier fapeng yu shujun zhang frederico alabarse mickael beaudhuin jerome rouquette'
;ICGM Univ Montpellier CNRS ENSCM  Montpellier France
France
;
_audit_update_record             
;
2024-07-19 deposited with the CCDC.	2024-11-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        'Calcium lanthanide oxyborates'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'B3 Ca4 Er O10'
_chemical_formula_sum            'B3 Ca4 Er O10'

_chemical_formula_weight         520.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source



B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.1943 3.0179 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_H-M_alt        'C m'
_space_group_name_Hall           'C -2y'

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

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

_cell_length_a                   8.0678(10)
_cell_length_b                   15.998(2)
_cell_length_c                   3.5172(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.097(4)
_cell_angle_gamma                90
_cell_volume                     445.48(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9698
_cell_measurement_theta_min      5.741
_cell_measurement_theta_max      144.2

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      3.877
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.877
_exptl_crystal_F_000             486
_exptl_transmission_factor_min   0.586
_exptl_transmission_factor_max   1
_exptl_crystal_size_max          0.113
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.049
_exptl_absorpt_coefficient_mu    11.765
_shelx_estimated_absorpt_T_min   0.586
_shelx_estimated_absorpt_T_max   1
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.586
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'D8 VENTURE  '
_diffrn_measurement_method       'profile data from θ/2θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15618
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.871
_diffrn_reflns_theta_max         45.280
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measured_fraction_theta_full 0.780
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_Laue_measured_fraction_full 0.780
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_point_group_measured_fraction_full 0.659
_reflns_number_total             3200
_reflns_number_gt                3200
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_max     0.738
_reflns_Friedel_fraction_full    0.536

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_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)+(0.0170P)²+0.2516P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.0050(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1390 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.129(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3200
_refine_ls_number_parameters     91
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0189
_refine_ls_wR_factor_ref         0.0395
_refine_ls_wR_factor_gt          0.0395
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.125
_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
Er1 Er 0.56245(2) 0.500000 0.47182(2) 0.00192(3) Uani 0.8029(14) 2 d S T P . .
Ca2 Ca 0.70233(3) 0.11237(2) 0.79554(7) 0.00308(7) Uani 0.9014(7) 1 d . . P . .
Ca3 Ca 0.31821(4) 0.18108(2) 1.11825(10) 0.00509(6) Uani 1 1 d . . . . .
Ca1 Ca 0.56245(2) 0.500000 0.47182(2) 0.00192(3) Uani 0.1971(14) 2 d S T P . .
Er2 Er 0.70233(3) 0.11237(2) 0.79554(7) 0.00308(7) Uani 0.0986(7) 1 d . . P . .
O1 O 0.5197(2) 0.07456(9) 1.2160(5) 0.00655(19) Uani 1 1 d . . . . .
O2 O 0.34647(18) 0.32523(9) 0.3496(5) 0.00604(18) Uani 1 1 d . . . . .
O3 O 0.3879(3) 0.500000 -0.1092(8) 0.0063(3) Uani 1 2 d S T P . .
O4 O 0.64076(19) 0.35850(9) 0.5417(4) 0.00526(17) Uani 1 1 d . . . . .
O5 O 0.5277(2) 0.23045(9) 0.7437(5) 0.00688(19) Uani 1 1 d . . . . .
O6 O 0.2587(3) 0.000000 1.0711(9) 0.0095(4) Uani 1 2 d S T P . .
B1 B 0.5059(2) 0.30497(12) 0.5459(6) 0.0045(2) Uani 1 1 d . . . . .
B2 B 0.4331(4) 0.000000 1.1683(8) 0.0035(3) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O3 2.226(3) 1_556 ?
Er1 O3 2.247(3) . ?
Er1 O6 2.313(3) 3_554 ?
Er1 O4 2.3503(15) 2_565 ?
Er1 O4 2.3503(15) . ?
Er1 O6 2.380(3) 3 ?
Er1 Er1 3.5172(4) 1_556 ?
Er1 Er1 3.5172(4) 1_554 ?
Er1 Ca2 3.7740(4) 4_455 ?
Er1 Ca2 3.7740(4) 3_455 ?
Er1 Ca2 3.8302(4) 4_454 ?
Er1 Ca2 3.8302(4) 3_454 ?
Ca3 O4 2.3335(16) 4_455 ?
Ca3 O1 2.3343(17) . ?
Ca3 O4 2.3429(15) 4_456 ?
Ca3 O2 2.4415(16) 1_556 ?
Ca3 O5 2.4644(16) . ?
Ca3 O5 2.6248(18) 1_556 ?
Ca3 B1 2.758(2) 1_556 ?
Ca3 O5 2.8359(18) 4_455 ?
Ca3 B1 2.915(2) 4_455 ?
Ca3 O6 2.9359(7) . ?
Ca3 B2 3.0363(10) . ?
Ca3 B1 3.181(2) 4_456 ?
Er2 O2 2.2967(16) 4_556 ?
Er2 O3 2.3223(17) 3_546 ?
Er2 O5 2.3426(15) . ?
Er2 O2 2.3476(16) 4 ?
Er2 O1 2.3528(17) 1_554 ?
Er2 O1 2.3586(16) . ?
O1 B2 1.376(2) . ?
O2 B1 1.376(2) . ?
O4 B1 1.387(2) . ?
O5 B1 1.374(3) . ?
O6 B2 1.383(4) . ?

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
O3 Er1 O3 103.69(11) 1_556 . ?
O3 Er1 O6 176.19(12) 1_556 3_554 ?
O3 Er1 O6 80.12(11) . 3_554 ?
O3 Er1 O4 97.03(4) 1_556 2_565 ?
O3 Er1 O4 101.76(4) . 2_565 ?
O6 Er1 O4 82.07(4) 3_554 2_565 ?
O3 Er1 O4 97.03(4) 1_556 . ?
O3 Er1 O4 101.76(4) . . ?
O6 Er1 O4 82.07(4) 3_554 . ?
O4 Er1 O4 148.79(7) 2_565 . ?
O3 Er1 O6 79.12(11) 1_556 3 ?
O3 Er1 O6 177.19(11) . 3 ?
O6 Er1 O6 97.07(10) 3_554 3 ?
O4 Er1 O6 77.75(4) 2_565 3 ?
O4 Er1 O6 77.75(4) . 3 ?
O3 Er1 Er1 38.37(7) 1_556 1_556 ?
O3 Er1 Er1 142.06(7) . 1_556 ?
O6 Er1 Er1 137.82(7) 3_554 1_556 ?
O4 Er1 Er1 86.97(4) 2_565 1_556 ?
O4 Er1 Er1 86.97(4) . 1_556 ?
O6 Er1 Er1 40.74(7) 3 1_556 ?
O3 Er1 Er1 141.63(7) 1_556 1_554 ?
O3 Er1 Er1 37.94(7) . 1_554 ?
O6 Er1 Er1 42.18(7) 3_554 1_554 ?
O4 Er1 Er1 93.03(4) 2_565 1_554 ?
O4 Er1 Er1 93.03(4) . 1_554 ?
O6 Er1 Er1 139.26(7) 3 1_554 ?
Er1 Er1 Er1 180.0 1_556 1_554 ?
O3 Er1 Ca2 34.75(4) 1_556 4_455 ?
O3 Er1 Ca2 83.71(6) . 4_455 ?
O6 Er1 Ca2 147.21(4) 3_554 4_455 ?
O4 Er1 Ca2 129.37(4) 2_565 4_455 ?
O4 Er1 Ca2 73.54(4) . 4_455 ?
O6 Er1 Ca2 98.76(6) 3 4_455 ?
Er1 Er1 Ca2 63.265(5) 1_556 4_455 ?
Er1 Er1 Ca2 116.735(5) 1_554 4_455 ?
O3 Er1 Ca2 34.75(4) 1_556 3_455 ?
O3 Er1 Ca2 83.71(6) . 3_455 ?
O6 Er1 Ca2 147.21(3) 3_554 3_455 ?
O4 Er1 Ca2 73.54(4) 2_565 3_455 ?
O4 Er1 Ca2 129.37(4) . 3_455 ?
O6 Er1 Ca2 98.76(6) 3 3_455 ?
Er1 Er1 Ca2 63.265(6) 1_556 3_455 ?
Er1 Er1 Ca2 116.735(5) 1_554 3_455 ?
Ca2 Er1 Ca2 56.894(11) 4_455 3_455 ?
O3 Er1 Ca2 84.85(6) 1_556 4_454 ?
O3 Er1 Ca2 33.67(4) . 4_454 ?
O6 Er1 Ca2 98.50(6) 3_554 4_454 ?
O4 Er1 Ca2 132.34(4) 2_565 4_454 ?
O4 Er1 Ca2 76.67(4) . 4_454 ?
O6 Er1 Ca2 147.75(3) 3 4_454 ?
Er1 Er1 Ca2 118.361(7) 1_556 4_454 ?
Er1 Er1 Ca2 61.640(7) 1_554 4_454 ?
Ca2 Er1 Ca2 55.096(8) 4_455 4_454 ?
Ca2 Er1 Ca2 82.815(11) 3_455 4_454 ?
O3 Er1 Ca2 84.85(6) 1_556 3_454 ?
O3 Er1 Ca2 33.67(4) . 3_454 ?
O6 Er1 Ca2 98.50(6) 3_554 3_454 ?
O4 Er1 Ca2 76.67(4) 2_565 3_454 ?
O4 Er1 Ca2 132.34(4) . 3_454 ?
O6 Er1 Ca2 147.75(3) 3 3_454 ?
Er1 Er1 Ca2 118.361(7) 1_556 3_454 ?
Er1 Er1 Ca2 61.640(6) 1_554 3_454 ?
Ca2 Er1 Ca2 82.815(11) 4_455 3_454 ?
Ca2 Er1 Ca2 55.096(8) 3_455 3_454 ?
Ca2 Er1 Ca2 55.984(11) 4_454 3_454 ?
O4 Ca3 O1 102.90(5) 4_455 . ?
O4 Ca3 O4 97.55(6) 4_455 4_456 ?
O1 Ca3 O4 101.68(5) . 4_456 ?
O4 Ca3 O2 123.25(5) 4_455 1_556 ?
O1 Ca3 O2 128.51(5) . 1_556 ?
O4 Ca3 O2 94.17(5) 4_456 1_556 ?
O4 Ca3 O5 89.52(6) 4_455 . ?
O1 Ca3 O5 77.46(5) . . ?
O4 Ca3 O5 172.87(6) 4_456 . ?
O2 Ca3 O5 81.12(5) 1_556 . ?
O4 Ca3 O5 176.80(5) 4_455 1_556 ?
O1 Ca3 O5 77.20(5) . 1_556 ?
O4 Ca3 O5 85.54(5) 4_456 1_556 ?
O2 Ca3 O5 55.43(5) 1_556 1_556 ?
O5 Ca3 O5 87.38(5) . 1_556 ?
O4 Ca3 B1 148.16(6) 4_455 1_556 ?
O1 Ca3 B1 98.66(6) . 1_556 ?
O4 Ca3 B1 100.72(6) 4_456 1_556 ?
O2 Ca3 B1 29.91(5) 1_556 1_556 ?
O5 Ca3 B1 72.55(6) . 1_556 ?
O5 Ca3 B1 29.45(5) 1_556 1_556 ?
O4 Ca3 O5 54.40(5) 4_455 4_455 ?
O1 Ca3 O5 157.30(5) . 4_455 ?
O4 Ca3 O5 83.03(5) 4_456 4_455 ?
O2 Ca3 O5 72.50(5) 1_556 4_455 ?
O5 Ca3 O5 100.50(4) . 4_455 ?
O5 Ca3 O5 125.48(3) 1_556 4_455 ?
B1 Ca3 O5 102.27(5) 1_556 4_455 ?
O4 Ca3 B1 27.94(5) 4_455 4_455 ?
O1 Ca3 B1 129.97(6) . 4_455 ?
O4 Ca3 B1 84.66(6) 4_456 4_455 ?
O2 Ca3 B1 99.83(5) 1_556 4_455 ?
O5 Ca3 B1 101.36(6) . 4_455 ?
O5 Ca3 B1 152.54(5) 1_556 4_455 ?
B1 Ca3 B1 129.23(3) 1_556 4_455 ?
O5 Ca3 B1 27.61(5) 4_455 4_455 ?
O4 Ca3 O6 67.47(7) 4_455 . ?
O1 Ca3 O6 52.40(6) . . ?
O4 Ca3 O6 69.87(7) 4_456 . ?
O2 Ca3 O6 162.67(7) 1_556 . ?
O5 Ca3 O6 114.06(7) . . ?
O5 Ca3 O6 114.60(7) 1_556 . ?
B1 Ca3 O6 143.76(7) 1_556 . ?
O5 Ca3 O6 110.77(6) 4_455 . ?
B1 Ca3 O6 85.77(7) 4_455 . ?
O4 Ca3 B2 85.46(7) 4_455 . ?
O1 Ca3 B2 25.69(6) . . ?
O4 Ca3 B2 85.54(7) 4_456 . ?
O2 Ca3 B2 150.92(7) 1_556 . ?
O5 Ca3 B2 95.95(6) . . ?
O5 Ca3 B2 95.65(6) 1_556 . ?
B1 Ca3 B2 121.64(7) 1_556 . ?
O5 Ca3 B2 135.96(6) 4_455 . ?
B1 Ca3 B2 109.07(7) 4_455 . ?
O6 Ca3 B2 26.70(7) . . ?
O4 Ca3 B1 91.19(5) 4_455 4_456 ?
O1 Ca3 B1 125.03(6) . 4_456 ?
O4 Ca3 B1 23.35(5) 4_456 4_456 ?
O2 Ca3 B1 78.92(5) 1_556 4_456 ?
O5 Ca3 B1 156.55(5) . 4_456 ?
O5 Ca3 B1 91.34(5) 1_556 4_456 ?
B1 Ca3 B1 95.36(5) 1_556 4_456 ?
O5 Ca3 B1 61.68(5) 4_455 4_456 ?
B1 Ca3 B1 70.32(4) 4_455 4_456 ?
O6 Ca3 B1 87.71(7) . 4_456 ?
B2 Ca3 B1 107.47(6) . 4_456 ?
O2 Er2 O3 90.40(7) 4_556 3_546 ?
O2 Er2 O5 85.07(6) 4_556 . ?
O3 Er2 O5 175.47(8) 3_546 . ?
O2 Er2 O2 98.45(5) 4_556 4 ?
O3 Er2 O2 92.13(7) 3_546 4 ?
O5 Er2 O2 88.45(5) . 4 ?
O2 Er2 O1 167.76(6) 4_556 1_554 ?
O3 Er2 O1 101.83(7) 3_546 1_554 ?
O5 Er2 O1 82.70(6) . 1_554 ?
O2 Er2 O1 80.72(5) 4 1_554 ?
O2 Er2 O1 81.65(5) 4_556 . ?
O3 Er2 O1 100.04(7) 3_546 . ?
O5 Er2 O1 79.43(5) . . ?
O2 Er2 O1 167.84(6) 4 . ?
O1 Er2 O1 96.58(6) 1_554 . ?
O2 Er2 Ca2 41.32(4) 4_556 1_556 ?
O3 Er2 Ca2 88.84(7) 3_546 1_556 ?
O5 Er2 Ca2 87.82(4) . 1_556 ?
O2 Er2 Ca2 139.77(4) 4 1_556 ?
O1 Er2 Ca2 138.23(4) 1_554 1_556 ?
O1 Er2 Ca2 41.65(4) . 1_556 ?
O2 Er2 Ca2 138.68(4) 4_556 1_554 ?
O3 Er2 Ca2 91.16(7) 3_546 1_554 ?
O5 Er2 Ca2 92.18(4) . 1_554 ?
O2 Er2 Ca2 40.23(4) 4 1_554 ?
O1 Er2 Ca2 41.77(4) 1_554 1_554 ?
O1 Er2 Ca2 138.35(4) . 1_554 ?
Ca2 Er2 Ca2 180.0 1_556 1_554 ?
O2 Er2 Ca3 42.86(4) 4_556 4 ?
O3 Er2 Ca3 123.37(6) 3_546 4 ?
O5 Er2 Ca3 52.65(4) . 4 ?
O2 Er2 Ca3 71.63(4) 4 4 ?
O1 Er2 Ca3 126.66(4) 1_554 4 ?
O1 Er2 Ca3 101.28(4) . 4 ?
Ca2 Er2 Ca3 74.437(8) 1_556 4 ?
Ca2 Er2 Ca3 105.562(8) 1_554 4 ?
O2 Er2 Ca2 115.77(4) 4_556 2 ?
O3 Er2 Ca2 39.28(5) 3_546 2 ?
O5 Er2 Ca2 143.75(4) . 2 ?
O2 Er2 Ca2 115.17(4) 4 2 ?
O1 Er2 Ca2 75.10(4) 1_554 2 ?
O1 Er2 Ca2 75.14(4) . 2 ?
Ca2 Er2 Ca2 90.0 1_556 2 ?
Ca2 Er2 Ca2 90.0 1_554 2 ?
Ca3 Er2 Ca2 158.161(8) 4 2 ?
O2 Er2 Ca3 85.82(4) 4_556 . ?
O3 Er2 Ca3 138.33(6) 3_546 . ?
O5 Er2 Ca3 41.51(4) . . ?
O2 Er2 Ca3 129.49(4) 4 . ?
O1 Er2 Ca3 85.39(4) 1_554 . ?
O1 Er2 Ca3 38.36(4) . . ?
Ca2 Er2 Ca3 61.832(8) 1_556 . ?
Ca2 Er2 Ca3 118.167(8) 1_554 . ?
Ca3 Er2 Ca3 78.979(9) 4 . ?
Ca2 Er2 Ca3 107.438(7) 2 . ?
O2 Er2 Ca3 130.00(4) 4_556 1_554 ?
O3 Er2 Ca3 139.56(6) 3_546 1_554 ?
O5 Er2 Ca3 44.97(4) . 1_554 ?
O2 Er2 Ca3 84.52(4) 4 1_554 ?
O1 Er2 Ca3 37.82(4) 1_554 1_554 ?
O1 Er2 Ca3 86.15(4) . 1_554 ?
Ca2 Er2 Ca3 118.908(9) 1_556 1_554 ?
Ca2 Er2 Ca3 61.091(9) 1_554 1_554 ?
Ca3 Er2 Ca3 93.763(9) 4 1_554 ?
Ca2 Er2 Ca3 107.312(7) 2 1_554 ?
Ca3 Er2 Ca3 57.076(11) . 1_554 ?
B2 O1 Ca3 106.97(14) . . ?
B2 O1 Ca2 123.16(15) . 1_556 ?
Ca3 O1 Ca2 104.02(6) . 1_556 ?
B2 O1 Er2 120.64(15) . . ?
Ca3 O1 Er2 102.82(6) . . ?
Ca2 O1 Er2 96.58(6) 1_556 . ?
B1 O2 Ca2 143.10(13) . 4_454 ?
B1 O2 Ca2 107.48(12) . 4_455 ?
Ca2 O2 Ca2 98.45(5) 4_454 4_455 ?
B1 O2 Ca3 87.89(11) . 1_554 ?
Ca2 O2 Ca3 97.37(6) 4_454 1_554 ?
Ca2 O2 Ca3 126.72(7) 4_455 1_554 ?
Er1 O3 Er1 103.69(11) 1_554 . ?
Er1 O3 Ca2 112.14(8) 1_554 4_454 ?
Er1 O3 Ca2 113.89(8) . 4_454 ?
Er1 O3 Ca2 112.14(8) 1_554 3_454 ?
Er1 O3 Ca2 113.89(8) . 3_454 ?
Ca2 O3 Ca2 101.44(10) 4_454 3_454 ?
B1 O4 Ca3 100.04(12) . 4 ?
B1 O4 Ca3 114.61(12) . 4_554 ?
Ca3 O4 Ca3 97.55(6) 4 4_554 ?
B1 O4 Er1 113.59(12) . . ?
Ca3 O4 Er1 117.38(6) 4 . ?
Ca3 O4 Er1 112.25(6) 4_554 . ?
B1 O5 Er2 139.05(13) . . ?
B1 O5 Ca3 120.96(12) . . ?
Er2 O5 Ca3 99.44(5) . . ?
B1 O5 Ca3 80.66(11) . 1_554 ?
Er2 O5 Ca3 95.92(6) . 1_554 ?
Ca3 O5 Ca3 87.38(5) . 1_554 ?
B1 O5 Ca3 79.40(11) . 4 ?
Er2 O5 Ca3 86.30(5) . 4 ?
Ca3 O5 Ca3 120.15(6) . 4 ?
Ca3 O5 Ca3 151.74(6) 1_554 4 ?
B2 O6 Er1 129.2(2) . 3_446 ?
B2 O6 Er1 133.7(2) . 3_445 ?
Er1 O6 Er1 97.07(10) 3_446 3_445 ?
B2 O6 Ca3 80.70(5) . . ?
Er1 O6 Ca3 95.12(6) 3_446 . ?
Er1 O6 Ca3 97.11(6) 3_445 . ?
B2 O6 Ca3 80.70(5) . 2 ?
Er1 O6 Ca3 95.12(6) 3_446 2 ?
Er1 O6 Ca3 97.11(6) 3_445 2 ?
Ca3 O6 Ca3 161.29(11) . 2 ?
O5 B1 O2 118.32(17) . . ?
O5 B1 O4 121.12(17) . . ?
O2 B1 O4 120.57(17) . . ?
O5 B1 Ca3 69.89(11) . 1_554 ?
O2 B1 Ca3 62.20(10) . 1_554 ?
O4 B1 Ca3 141.94(14) . 1_554 ?
O5 B1 Ca3 72.99(11) . 4 ?
O2 B1 Ca3 158.19(14) . 4 ?
O4 B1 Ca3 52.02(9) . 4 ?
Ca3 B1 Ca3 137.94(7) 1_554 4 ?
O5 B1 Ca2 105.15(12) . 4_455 ?
O2 B1 Ca2 47.09(9) . 4_455 ?
O4 B1 Ca2 114.17(12) . 4_455 ?
Ca3 B1 Ca2 94.67(6) 1_554 4_455 ?
Ca3 B1 Ca2 113.72(7) 4 4_455 ?
O5 B1 Ca3 105.33(12) . 4_554 ?
O2 B1 Ca3 119.67(13) . 4_554 ?
O4 B1 Ca3 42.04(8) . 4_554 ?
Ca3 B1 Ca3 101.20(6) 1_554 4_554 ?
Ca3 B1 Ca3 70.32(4) 4 4_554 ?
Ca2 B1 Ca3 148.95(7) 4_455 4_554 ?
O1 B2 O1 120.2(2) . 2 ?
O1 B2 O6 119.92(12) . . ?
O1 B2 O6 119.92(12) 2 . ?
O1 B2 Ca3 47.34(9) . . ?
O1 B2 Ca3 167.45(17) 2 . ?
O6 B2 Ca3 72.60(5) . . ?
O1 B2 Ca3 167.45(17) . 2 ?
O1 B2 Ca3 47.34(9) 2 2 ?
O6 B2 Ca3 72.60(5) . 2 ?
Ca3 B2 Ca3 145.14(10) . 2 ?
O1 B2 Ca2 99.43(15) . 2 ?
O1 B2 Ca2 38.20(11) 2 2 ?
O6 B2 Ca2 128.44(15) . 2 ?
Ca3 B2 Ca2 135.86(8) . 2 ?
Ca3 B2 Ca2 70.87(3) 2 2 ?

_refine_diff_density_max         3.621
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.306

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

data_mo_NdCOB_100K_0m_b
_database_code_depnum_ccdc_archive 'CCDC 2372144'
loop_
_audit_author_name
_audit_author_address

'fatiha azrour romain viennois jerome long dominique granier fapeng yu shujun zhang frederico alabarse mickael beaudhuin jerome rouquette'
;ICGM Univ Montpellier CNRS ENSCM  Montpellier France
France
;
_audit_update_record             
;
2024-07-19 deposited with the CCDC.	2024-11-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'B3 Ca4 Nd O10'
_chemical_formula_sum            'B3 Ca4 Nd O10'

_chemical_formula_weight         496.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source




B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_H-M_alt        'C m'
_space_group_name_Hall           'C -2y'

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

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

_cell_length_a                   8.1143(10)
_cell_length_b                   16.033(2)
_cell_length_c                   3.5924(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.322(8)
_cell_angle_gamma                90
_cell_volume                     458.26(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9659
_cell_measurement_theta_min      5.716
_cell_measurement_theta_max      148.2

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      3.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.602
_exptl_crystal_F_000             470
_exptl_transmission_factor_min   0.828
_exptl_transmission_factor_max   1
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.047
_exptl_absorpt_coefficient_mu    7.945
_shelx_estimated_absorpt_T_min   0.828
_shelx_estimated_absorpt_T_max   1
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'D8 VENTURE  '
_diffrn_measurement_method       'profile data from θ/2θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14555
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.541
_diffrn_reflns_theta_max         45.293
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measured_fraction_theta_full 0.717
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_Laue_measured_fraction_full 0.717
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_point_group_measured_fraction_full 0.647
_reflns_number_total             3579
_reflns_number_gt                3579
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_max     0.893
_reflns_Friedel_fraction_full    0.576

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_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)+(0.0542P)²+2.9251P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.0066(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1738 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3579
_refine_ls_number_parameters     91
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0243
_refine_ls_wR_factor_ref         0.0588
_refine_ls_wR_factor_gt          0.0588
_refine_ls_goodness_of_fit_ref   0.780
_refine_ls_restrained_S_all      0.780
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.43757(2) 0.500000 0.52755(2) 0.00286(4) Uani 0.991(2) 2 d S T P . .
Ca2 Ca 0.29422(6) 0.88660(3) 0.19728(13) 0.00336(10) Uani 0.9953(11) 1 d . . P
. .
Ca3 Ca 0.66947(6) 0.81801(3) -0.13490(13) 0.00454(7) Uani 1 1 d . . . . .
Ca1 Ca 0.43757(2) 0.500000 0.52755(2) 0.00286(4) Uani 0.009(2) 2 d S T P . .
Nd2 Nd 0.29422(6) 0.88660(3) 0.19728(13) 0.00336(10) Uani 0.0047(11) 1 d . . P
. .
O1 O 0.4714(3) 0.92532(12) -0.2258(6) 0.0054(2) Uani 1 1 d . . . . .
O2 O 0.6384(2) 0.67009(13) 0.6391(6) 0.0060(2) Uani 1 1 d . . . . .
O3 O 0.6138(4) 0.500000 1.1103(9) 0.0038(4) Uani 1 2 d S T P . .
O4 O 0.3429(2) 0.64534(13) 0.4408(5) 0.0052(2) Uani 1 1 d . . . . .
O5 O 0.4688(3) 0.76956(13) 0.2486(6) 0.0066(3) Uani 1 1 d . . . . .
O6 O 0.7310(4) 1.000000 -0.0813(10) 0.0074(5) Uani 1 2 d S T P . .
B1 B 0.4828(3) 0.69497(17) 0.4413(8) 0.0042(3) Uani 1 1 d . . . . .
B2 B 0.5573(5) 1.000000 -0.1781(11) 0.0040(4) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O3 2.266(3) 1_554 ?
Nd1 O3 2.292(3) . ?
Nd1 O6 2.389(4) 3_446 ?
Nd1 O4 2.454(2) 2_565 ?
Nd1 O4 2.454(2) . ?
Nd1 O6 2.481(3) 3_445 ?
Nd1 Nd1 3.5923(4) 1_556 ?
Nd1 Nd1 3.5924(4) 1_554 ?
Nd1 Ca2 3.7996(6) 4_565 ?
Nd1 Ca2 3.7996(6) 3_545 ?
Nd1 Ca2 3.8387(6) 4_566 ?
Nd1 Ca2 3.8387(6) 3_546 ?
Ca3 O1 2.333(2) . ?
Ca3 O4 2.337(2) 4_565 ?
Ca3 O4 2.343(2) 4_564 ?
Ca3 O5 2.456(2) . ?
Ca3 O2 2.503(2) 1_554 ?
Ca3 O5 2.597(2) 1_554 ?
Ca3 B1 2.756(3) 1_554 ?
Ca3 O5 2.908(2) 4_565 ?
Ca3 B1 2.954(3) 4_565 ?
Ca3 O6 2.9602(8) . ?
Ca3 B2 3.0515(13) . ?
Ca3 B1 3.217(3) 4_564 ?
Nd2 O3 2.316(2) 3_454 ?
Nd2 O2 2.334(2) 4_464 ?
Nd2 O5 2.337(2) . ?
Nd2 O1 2.362(2) 1_556 ?
Nd2 O1 2.371(2) . ?
Nd2 O2 2.394(2) 4_465 ?
Nd2 B1 3.120(3) 4_465 ?
O1 B2 1.379(3) . ?
O2 B1 1.381(3) . ?
O4 B1 1.386(3) . ?
O5 B1 1.375(3) . ?
O6 B2 1.384(5) . ?

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
O3 Nd1 O3 104.03(13) 1_554 . ?
O3 Nd1 O6 174.78(11) 1_554 3_446 ?
O3 Nd1 O6 81.19(13) . 3_446 ?
O3 Nd1 O4 97.96(5) 1_554 2_565 ?
O3 Nd1 O4 103.87(5) . 2_565 ?
O6 Nd1 O4 80.59(5) 3_446 2_565 ?
O3 Nd1 O4 97.96(5) 1_554 . ?
O3 Nd1 O4 103.87(5) . . ?
O6 Nd1 O4 80.59(5) 3_446 . ?
O4 Nd1 O4 143.41(9) 2_565 . ?
O3 Nd1 O6 79.73(13) 1_554 3_445 ?
O3 Nd1 O6 176.24(13) . 3_445 ?
O6 Nd1 O6 95.04(12) 3_446 3_445 ?
O4 Nd1 O6 75.38(5) 2_565 3_445 ?
O4 Nd1 O6 75.38(5) . 3_445 ?
O3 Nd1 Nd1 141.76(8) 1_554 1_556 ?
O3 Nd1 Nd1 37.73(8) . 1_556 ?
O6 Nd1 Nd1 43.46(8) 3_446 1_556 ?
O4 Nd1 Nd1 93.76(5) 2_565 1_556 ?
O4 Nd1 Nd1 93.76(5) . 1_556 ?
O6 Nd1 Nd1 138.51(8) 3_445 1_556 ?
O3 Nd1 Nd1 38.24(8) 1_554 1_554 ?
O3 Nd1 Nd1 142.27(8) . 1_554 ?
O6 Nd1 Nd1 136.54(8) 3_446 1_554 ?
O4 Nd1 Nd1 86.24(5) 2_565 1_554 ?
O4 Nd1 Nd1 86.24(5) . 1_554 ?
O6 Nd1 Nd1 41.49(8) 3_445 1_554 ?
Nd1 Nd1 Nd1 180.0 1_556 1_554 ?
O3 Nd1 Ca2 34.42(4) 1_554 4_565 ?
O3 Nd1 Ca2 84.73(7) . 4_565 ?
O6 Nd1 Ca2 148.09(4) 3_446 4_565 ?
O4 Nd1 Ca2 130.79(5) 2_565 4_565 ?
O4 Nd1 Ca2 75.20(5) . 4_565 ?
O6 Nd1 Ca2 98.56(7) 3_445 4_565 ?
Nd1 Nd1 Ca2 117.503(9) 1_556 4_565 ?
Nd1 Nd1 Ca2 62.497(9) 1_554 4_565 ?
O3 Nd1 Ca2 34.42(4) 1_554 3_545 ?
O3 Nd1 Ca2 84.73(7) . 3_545 ?
O6 Nd1 Ca2 148.09(3) 3_446 3_545 ?
O4 Nd1 Ca2 75.20(5) 2_565 3_545 ?
O4 Nd1 Ca2 130.79(5) . 3_545 ?
O6 Nd1 Ca2 98.56(7) 3_445 3_545 ?
Nd1 Nd1 Ca2 117.503(9) 1_556 3_545 ?
Nd1 Nd1 Ca2 62.497(9) 1_554 3_545 ?
Ca2 Nd1 Ca2 57.179(16) 4_565 3_545 ?
O3 Nd1 Ca2 85.32(7) 1_554 4_566 ?
O3 Nd1 Ca2 33.80(4) . 4_566 ?
O6 Nd1 Ca2 99.27(7) 3_446 4_566 ?
O4 Nd1 Ca2 135.07(5) 2_565 4_566 ?
O4 Nd1 Ca2 78.96(5) . 4_566 ?
O6 Nd1 Ca2 148.03(4) 3_445 4_566 ?
Nd1 Nd1 Ca2 61.397(9) 1_556 4_566 ?
Nd1 Nd1 Ca2 118.604(10) 1_554 4_566 ?
Ca2 Nd1 Ca2 56.106(10) 4_565 4_566 ?
Ca2 Nd1 Ca2 84.011(15) 3_545 4_566 ?
O3 Nd1 Ca2 85.32(7) 1_554 3_546 ?
O3 Nd1 Ca2 33.80(4) . 3_546 ?
O6 Nd1 Ca2 99.27(7) 3_446 3_546 ?
O4 Nd1 Ca2 78.96(5) 2_565 3_546 ?
O4 Nd1 Ca2 135.07(5) . 3_546 ?
O6 Nd1 Ca2 148.03(4) 3_445 3_546 ?
Nd1 Nd1 Ca2 61.397(9) 1_556 3_546 ?
Nd1 Nd1 Ca2 118.604(9) 1_554 3_546 ?
Ca2 Nd1 Ca2 84.011(15) 4_565 3_546 ?
Ca2 Nd1 Ca2 56.106(10) 3_545 3_546 ?
Ca2 Nd1 Ca2 56.544(16) 4_566 3_546 ?
O1 Ca3 O4 102.53(7) . 4_565 ?
O1 Ca3 O4 102.08(7) . 4_564 ?
O4 Ca3 O4 100.28(8) 4_565 4_564 ?
O1 Ca3 O5 78.31(7) . . ?
O4 Ca3 O5 86.19(7) 4_565 . ?
O4 Ca3 O5 173.21(8) 4_564 . ?
O1 Ca3 O2 129.09(7) . 1_554 ?
O4 Ca3 O2 122.01(7) 4_565 1_554 ?
O4 Ca3 O2 93.53(7) 4_564 1_554 ?
O5 Ca3 O2 81.18(7) . 1_554 ?
O1 Ca3 O5 78.57(7) . 1_554 ?
O4 Ca3 O5 176.27(7) 4_565 1_554 ?
O4 Ca3 O5 82.89(7) 4_564 1_554 ?
O5 Ca3 O5 90.58(8) . 1_554 ?
O2 Ca3 O5 55.51(6) 1_554 1_554 ?
O1 Ca3 B1 99.31(8) . 1_554 ?
O4 Ca3 B1 147.03(8) 4_565 1_554 ?
O4 Ca3 B1 98.92(8) 4_564 1_554 ?
O5 Ca3 B1 74.37(8) . 1_554 ?
O2 Ca3 B1 29.95(7) 1_554 1_554 ?
O5 Ca3 B1 29.58(7) 1_554 1_554 ?
O1 Ca3 O5 155.61(7) . 4_565 ?
O4 Ca3 O5 53.14(6) 4_565 4_565 ?
O4 Ca3 O5 82.93(7) 4_564 4_565 ?
O5 Ca3 O5 99.53(6) . 4_565 ?
O2 Ca3 O5 73.60(6) 1_554 4_565 ?
O5 Ca3 O5 125.82(5) 1_554 4_565 ?
B1 Ca3 O5 103.50(7) 1_554 4_565 ?
O1 Ca3 B1 128.65(7) . 4_565 ?
O4 Ca3 B1 27.33(7) 4_565 4_565 ?
O4 Ca3 B1 85.94(7) 4_564 4_565 ?
O5 Ca3 B1 99.14(8) . 4_565 ?
O2 Ca3 B1 100.28(7) 1_554 4_565 ?
O5 Ca3 B1 152.35(7) 1_554 4_565 ?
B1 Ca3 B1 129.84(5) 1_554 4_565 ?
O5 Ca3 B1 27.12(7) 4_565 4_565 ?
O1 Ca3 O6 52.05(8) . . ?
O4 Ca3 O6 68.28(8) 4_565 . ?
O4 Ca3 O6 71.33(9) 4_564 . ?
O5 Ca3 O6 113.40(9) . . ?
O2 Ca3 O6 163.71(9) 1_554 . ?
O5 Ca3 O6 114.82(8) 1_554 . ?
B1 Ca3 O6 143.97(9) 1_554 . ?
O5 Ca3 O6 109.31(8) 4_565 . ?
B1 Ca3 O6 85.00(8) 4_565 . ?
O1 Ca3 B2 25.49(8) . . ?
O4 Ca3 B2 85.78(9) 4_565 . ?
O4 Ca3 B2 86.47(9) 4_564 . ?
O5 Ca3 B2 96.13(9) . . ?
O2 Ca3 B2 151.57(8) 1_554 . ?
O5 Ca3 B2 96.42(8) 1_554 . ?
B1 Ca3 B2 122.01(9) 1_554 . ?
O5 Ca3 B2 134.34(8) 4_565 . ?
B1 Ca3 B2 108.07(9) 4_565 . ?
O6 Ca3 B2 26.57(9) . . ?
O1 Ca3 B1 124.63(7) . 4_564 ?
O4 Ca3 B1 92.33(7) 4_565 4_564 ?
O4 Ca3 B1 22.61(7) 4_564 4_564 ?
O5 Ca3 B1 156.59(7) . 4_564 ?
O2 Ca3 B1 79.85(7) 1_554 4_564 ?
O5 Ca3 B1 89.91(7) 1_554 4_564 ?
B1 Ca3 B1 95.27(7) 1_554 4_564 ?
O5 Ca3 B1 61.88(7) 4_565 4_564 ?
B1 Ca3 B1 71.06(6) 4_565 4_564 ?
O6 Ca3 B1 87.46(9) . 4_564 ?
B2 Ca3 B1 107.07(9) . 4_564 ?
O3 Nd2 O2 88.19(9) 3_454 4_464 ?
O3 Nd2 O5 176.58(9) 3_454 . ?
O2 Nd2 O5 88.44(8) 4_464 . ?
O3 Nd2 O1 99.88(9) 3_454 1_556 ?
O2 Nd2 O1 171.82(8) 4_464 1_556 ?
O5 Nd2 O1 83.50(8) . 1_556 ?
O3 Nd2 O1 98.89(9) 3_454 . ?
O2 Nd2 O1 81.12(7) 4_464 . ?
O5 Nd2 O1 80.00(7) . . ?
O1 Nd2 O1 98.77(8) 1_556 . ?
O3 Nd2 O2 89.17(9) 3_454 4_465 ?
O2 Nd2 O2 98.88(7) 4_464 4_465 ?
O5 Nd2 O2 91.93(7) . 4_465 ?
O1 Nd2 O2 80.07(7) 1_556 4_465 ?
O1 Nd2 O2 171.93(8) . 4_465 ?
O3 Nd2 B1 80.90(9) 3_454 4_465 ?
O2 Nd2 B1 75.30(7) 4_464 4_465 ?
O5 Nd2 B1 98.81(8) . 4_465 ?
O1 Nd2 B1 104.52(7) 1_556 4_465 ?
O1 Nd2 B1 156.41(7) . 4_465 ?
O2 Nd2 B1 24.82(7) 4_465 4_465 ?
O3 Nd2 Ca3 123.10(7) 3_454 4_465 ?
O2 Nd2 Ca3 44.33(5) 4_464 4_465 ?
O5 Nd2 Ca3 54.26(6) . 4_465 ?
O1 Nd2 Ca3 128.24(5) 1_556 4_465 ?
O1 Nd2 Ca3 101.20(5) . 4_465 ?
O2 Nd2 Ca3 73.78(5) 4_465 4_465 ?
B1 Nd2 Ca3 61.08(5) 4_465 4_465 ?
O3 Nd2 Ca2 90.62(8) 3_454 1_556 ?
O2 Nd2 Ca2 138.82(5) 4_464 1_556 ?
O5 Nd2 Ca2 92.30(5) . 1_556 ?
O1 Nd2 Ca2 40.71(5) 1_556 1_556 ?
O1 Nd2 Ca2 139.48(5) . 1_556 ?
O2 Nd2 Ca2 39.94(5) 4_465 1_556 ?
B1 Nd2 Ca2 63.90(5) 4_465 1_556 ?
Ca3 Nd2 Ca2 106.181(11) 4_465 1_556 ?
O3 Nd2 Ca2 89.38(8) 3_454 1_554 ?
O2 Nd2 Ca2 41.18(5) 4_464 1_554 ?
O5 Nd2 Ca2 87.70(5) . 1_554 ?
O1 Nd2 Ca2 139.29(5) 1_556 1_554 ?
O1 Nd2 Ca2 40.52(5) . 1_554 ?
O2 Nd2 Ca2 140.06(5) 4_465 1_554 ?
B1 Nd2 Ca2 116.10(5) 4_465 1_554 ?
Ca3 Nd2 Ca2 73.818(11) 4_465 1_554 ?
Ca2 Nd2 Ca2 180.00(3) 1_556 1_554 ?
O3 Nd2 Ca2 38.29(6) 3_454 2_575 ?
O2 Nd2 Ca2 112.91(5) 4_464 2_575 ?
O5 Nd2 Ca2 143.43(6) . 2_575 ?
O1 Nd2 Ca2 74.76(5) 1_556 2_575 ?
O1 Nd2 Ca2 74.82(5) . 2_575 ?
O2 Nd2 Ca2 112.31(5) 4_465 2_575 ?
B1 Nd2 Ca2 114.78(5) 4_465 2_575 ?
Ca3 Nd2 Ca2 156.813(11) 4_465 2_575 ?
Ca2 Nd2 Ca2 90.0 1_556 2_575 ?
Ca2 Nd2 Ca2 90.0 1_554 2_575 ?
O3 Nd2 Ca3 137.53(8) 3_454 . ?
O2 Nd2 Ca3 87.00(5) 4_464 . ?
O5 Nd2 Ca3 41.61(5) . . ?
O1 Nd2 Ca3 87.88(5) 1_556 . ?
O1 Nd2 Ca3 38.72(5) . . ?
O2 Nd2 Ca3 133.24(6) 4_465 . ?
B1 Nd2 Ca3 137.64(5) 4_465 . ?
Ca3 Nd2 Ca3 79.273(14) 4_465 . ?
Ca2 Nd2 Ca3 119.376(13) 1_556 . ?
Ca2 Nd2 Ca3 60.624(13) 1_554 . ?
Ca2 Nd2 Ca3 107.529(11) 2_575 . ?
B2 O1 Ca3 107.79(18) . . ?
B2 O1 Ca2 122.9(2) . 1_554 ?
Ca3 O1 Ca2 102.29(8) . 1_554 ?
B2 O1 Nd2 120.20(19) . . ?
Ca3 O1 Nd2 101.83(8) . . ?
Ca2 O1 Nd2 98.77(8) 1_554 . ?
B1 O2 Ca2 147.24(18) . 4_566 ?
B1 O2 Ca2 108.48(16) . 4_565 ?
Ca2 O2 Ca2 98.88(7) 4_566 4_565 ?
B1 O2 Ca3 85.23(15) . 1_556 ?
Ca2 O2 Ca3 95.01(7) 4_566 1_556 ?
Ca2 O2 Ca3 122.83(9) 4_565 1_556 ?
Nd1 O3 Nd1 104.03(12) 1_556 . ?
Nd1 O3 Ca2 112.02(10) 1_556 4_566 ?
Nd1 O3 Ca2 112.81(9) . 4_566 ?
Nd1 O3 Ca2 112.02(10) 1_556 3_546 ?
Nd1 O3 Ca2 112.81(9) . 3_546 ?
Ca2 O3 Ca2 103.42(12) 4_566 3_546 ?
B1 O4 Ca3 101.98(15) . 4_465 ?
B1 O4 Ca3 116.85(16) . 4_466 ?
Ca3 O4 Ca3 100.28(8) 4_465 4_466 ?
B1 O4 Nd1 107.99(15) . . ?
Ca3 O4 Nd1 118.05(8) 4_465 . ?
Ca3 O4 Nd1 111.62(8) 4_466 . ?
B1 O5 Nd2 136.64(18) . . ?
B1 O5 Ca3 123.98(17) . . ?
Nd2 O5 Ca3 99.22(8) . . ?
B1 O5 Ca3 81.65(15) . 1_556 ?
Nd2 O5 Ca3 95.51(8) . 1_556 ?
Ca3 O5 Ca3 90.58(8) . 1_556 ?
B1 O5 Ca3 78.31(15) . 4_465 ?
Nd2 O5 Ca3 85.02(7) . 4_465 ?
Ca3 O5 Ca3 118.10(8) . 4_465 ?
Ca3 O5 Ca3 150.94(8) 1_556 4_465 ?
B2 O6 Nd1 130.5(3) . 3_554 ?
B2 O6 Nd1 134.4(3) . 3 ?
Nd1 O6 Nd1 95.05(12) 3_554 3 ?
B2 O6 Ca3 80.40(6) . . ?
Nd1 O6 Ca3 95.20(7) 3_554 . ?
Nd1 O6 Ca3 97.67(7) 3 . ?
B2 O6 Ca3 80.40(6) . 2_575 ?
Nd1 O6 Ca3 95.20(7) 3_554 2_575 ?
Nd1 O6 Ca3 97.67(7) 3 2_575 ?
Ca3 O6 Ca3 160.60(13) . 2_575 ?
O5 B1 O2 119.2(2) . . ?
O5 B1 O4 120.8(2) . . ?
O2 B1 O4 120.1(2) . . ?
O5 B1 Ca3 68.77(15) . 1_556 ?
O2 B1 Ca3 64.82(14) . 1_556 ?
O4 B1 Ca3 140.58(18) . 1_556 ?
O5 B1 Ca3 74.57(15) . 4_465 ?
O2 B1 Ca3 156.17(19) . 4_465 ?
O4 B1 Ca3 50.69(12) . 4_465 ?
Ca3 B1 Ca3 137.86(10) 1_556 4_465 ?
O5 B1 Ca2 102.39(16) . 4_565 ?
O2 B1 Ca2 46.70(12) . 4_565 ?
O4 B1 Ca2 117.87(17) . 4_565 ?
Ca3 B1 Ca2 93.88(8) 1_556 4_565 ?
Ca3 B1 Ca2 114.01(9) 4_465 4_565 ?
O5 B1 Ca3 107.43(16) . 4_466 ?
O2 B1 Ca3 117.75(17) . 4_466 ?
O4 B1 Ca3 40.54(12) . 4_466 ?
Ca3 B1 Ca3 100.63(8) 1_556 4_466 ?
Ca3 B1 Ca3 71.06(6) 4_465 4_466 ?
Ca2 B1 Ca3 149.88(10) 4_565 4_466 ?
O1 B2 O1 120.5(3) 2_575 . ?
O1 B2 O6 119.74(16) 2_575 . ?
O1 B2 O6 119.74(16) . . ?
O1 B2 Ca3 46.72(12) 2_575 2_575 ?
O1 B2 Ca3 167.2(2) . 2_575 ?
O6 B2 Ca3 73.03(7) . 2_575 ?
O1 B2 Ca3 167.2(2) 2_575 . ?
O1 B2 Ca3 46.73(12) . . ?
O6 B2 Ca3 73.03(7) . . ?
Ca3 B2 Ca3 145.96(14) 2_575 . ?
O1 B2 Ca2 38.55(14) 2_575 2_575 ?
O1 B2 Ca2 100.3(2) . 2_575 ?
O6 B2 Ca2 127.46(19) . 2_575 ?
Ca3 B2 Ca2 70.22(4) 2_575 2_575 ?
Ca3 B2 Ca2 135.99(11) . 2_575 ?

_refine_diff_density_max         3.183
_refine_diff_density_min         -1.382
_refine_diff_density_rms         0.261

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

data_mo_GdCOB_100K_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2372143'
loop_
_audit_author_name
_audit_author_address

'fatiha azrour romain viennois jerome long dominique granier fapeng yu shujun zhang frederico alabarse mickael beaudhuin jerome rouquette'
;ICGM Univ Montpellier CNRS ENSCM  Montpellier France
France
;
_audit_update_record             
;
2024-07-19 deposited with the CCDC.	2024-11-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'B3 Ca4 Gd O10'
_chemical_formula_sum            'B3 Ca4 Gd O10'

_chemical_formula_weight         510.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source



B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1943 3.0179 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_H-M_alt        'C m'
_space_group_name_Hall           'C -2y'

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

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

_cell_length_a                   8.0872(4)
_cell_length_b                   16.0094(8)
_cell_length_c                   3.5531(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.2630(10)
_cell_angle_gamma                90
_cell_volume                     451.16(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9844
_cell_measurement_theta_min      5.732
_cell_measurement_theta_max      147.9

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      3.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.754
_exptl_crystal_F_000             478
_exptl_transmission_factor_min   0.626
_exptl_transmission_factor_max   1
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.089
_exptl_absorpt_coefficient_mu    9.666
_shelx_estimated_absorpt_T_min   0.626
_shelx_estimated_absorpt_T_max   1
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'D8 VENTURE  '
_diffrn_measurement_method       'profile data from θ/2θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13349
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.544
_diffrn_reflns_theta_max         45.287
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measured_fraction_theta_full 0.753
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_Laue_measured_fraction_full 0.753
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_point_group_measured_fraction_full 0.632
_reflns_number_total             3268
_reflns_number_gt                3268
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.790
_reflns_Friedel_fraction_max     0.752
_reflns_Friedel_fraction_full    0.508

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_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)+(0.0193P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.0028(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1442 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.125(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3268
_refine_ls_number_parameters     91
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0190
_refine_ls_wR_factor_ref         0.0395
_refine_ls_wR_factor_gt          0.0395
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.087
_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 0.56251(2) 0.500000 0.47277(2) 0.00217(3) Uani 0.9611(16) 2 d S T P . .
Ca2 Ca 0.70306(4) 0.11266(2) 0.79987(9) 0.00316(8) Uani 0.9805(8) 1 d . . P . .
Ca3 Ca 0.32443(4) 0.18212(2) 1.12744(9) 0.00435(5) Uani 1 1 d . . . . .
Ca1 Ca 0.56251(2) 0.500000 0.47277(2) 0.00217(3) Uani 0.0389(16) 2 d S T P . .
Gd2 Gd 0.70306(4) 0.11266(2) 0.79987(9) 0.00316(8) Uani 0.0195(8) 1 d . . P . .
O1 O 0.52336(19) 0.07469(9) 1.2216(4) 0.00531(17) Uani 1 1 d . . . . .
O2 O 0.35412(18) 0.32790(9) 0.3567(4) 0.00563(17) Uani 1 1 d . . . . .
O3 O 0.3881(3) 0.500000 -0.1077(7) 0.0038(3) Uani 1 2 d S T P . .
O4 O 0.64914(18) 0.35720(9) 0.5511(4) 0.00503(17) Uani 1 1 d . . . . .
O5 O 0.5303(2) 0.23098(9) 0.7504(4) 0.00631(18) Uani 1 1 d . . . . .
O6 O 0.2631(3) 0.000000 1.0760(8) 0.0063(3) Uani 1 2 d S T P . .
B1 B 0.5117(2) 0.30537(12) 0.5540(6) 0.0040(2) Uani 1 1 d . . . . .
B2 B 0.4374(3) 0.000000 1.1741(8) 0.0036(3) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O3 2.243(3) 1_556 ?
Gd1 O3 2.260(2) . ?
Gd1 O6 2.348(3) 3_554 ?
Gd1 O4 2.3913(14) . ?
Gd1 O4 2.3913(14) 2_565 ?
Gd1 O6 2.422(3) 3 ?
Gd1 Gd1 3.55310(19) 1_554 ?
Gd1 Gd1 3.5531(2) 1_556 ?
Gd1 Ca2 3.7913(3) 4_455 ?
Gd1 Ca2 3.7913(3) 3_455 ?
Gd1 Ca2 3.8347(3) 4_454 ?
Gd1 Ca2 3.8347(3) 3_454 ?
Ca3 O1 2.3341(15) . ?
Ca3 O4 2.3377(14) 4_455 ?
Ca3 O4 2.3465(15) 4_456 ?
Ca3 O5 2.4594(15) . ?
Ca3 O2 2.4681(15) 1_556 ?
Ca3 O5 2.6159(16) 1_556 ?
Ca3 B1 2.754(2) 1_556 ?
Ca3 O5 2.8539(16) 4_455 ?
Ca3 B1 2.9284(19) 4_455 ?
Ca3 O6 2.9572(6) . ?
Ca3 B2 3.0502(9) . ?
Ca3 B1 3.199(2) 4_456 ?
Gd2 O2 2.3168(14) 4_556 ?
Gd2 O3 2.3258(16) 3_546 ?
Gd2 O5 2.3400(15) . ?
Gd2 O1 2.3531(15) 1_554 ?
Gd2 O1 2.3617(15) . ?
Gd2 O2 2.3725(15) 4 ?
Gd2 B1 3.0931(19) 4 ?
O1 B2 1.377(2) . ?
O2 B1 1.377(2) . ?
O4 B1 1.389(2) . ?
O5 B1 1.374(2) . ?
O6 B2 1.384(4) . ?

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
O3 Gd1 O3 104.20(10) 1_556 . ?
O3 Gd1 O6 175.41(9) 1_556 3_554 ?
O3 Gd1 O6 80.39(10) . 3_554 ?
O3 Gd1 O4 97.50(4) 1_556 . ?
O3 Gd1 O4 102.87(4) . . ?
O6 Gd1 O4 81.31(4) 3_554 . ?
O3 Gd1 O4 97.50(4) 1_556 2_565 ?
O3 Gd1 O4 102.87(4) . 2_565 ?
O6 Gd1 O4 81.31(4) 3_554 2_565 ?
O4 Gd1 O4 145.88(7) . 2_565 ?
O3 Gd1 O6 79.12(10) 1_556 3 ?
O3 Gd1 O6 176.67(11) . 3 ?
O6 Gd1 O6 96.28(9) 3_554 3 ?
O4 Gd1 O6 76.50(4) . 3 ?
O4 Gd1 O6 76.50(4) 2_565 3 ?
O3 Gd1 Gd1 141.94(6) 1_556 1_554 ?
O3 Gd1 Gd1 37.74(6) . 1_554 ?
O6 Gd1 Gd1 42.66(6) 3_554 1_554 ?
O4 Gd1 Gd1 93.40(3) . 1_554 ?
O4 Gd1 Gd1 93.40(3) 2_565 1_554 ?
O6 Gd1 Gd1 138.94(7) 3 1_554 ?
O3 Gd1 Gd1 38.06(6) 1_556 1_556 ?
O3 Gd1 Gd1 142.26(6) . 1_556 ?
O6 Gd1 Gd1 137.34(6) 3_554 1_556 ?
O4 Gd1 Gd1 86.60(3) . 1_556 ?
O4 Gd1 Gd1 86.60(3) 2_565 1_556 ?
O6 Gd1 Gd1 41.06(7) 3 1_556 ?
Gd1 Gd1 Gd1 180.0 1_554 1_556 ?
O3 Gd1 Ca2 34.63(3) 1_556 4_455 ?
O3 Gd1 Ca2 84.30(6) . 4_455 ?
O6 Gd1 Ca2 147.68(3) 3_554 4_455 ?
O4 Gd1 Ca2 74.59(3) . 4_455 ?
O4 Gd1 Ca2 130.08(3) 2_565 4_455 ?
O6 Gd1 Ca2 98.62(6) 3 4_455 ?
Gd1 Gd1 Ca2 117.149(5) 1_554 4_455 ?
Gd1 Gd1 Ca2 62.851(5) 1_556 4_455 ?
O3 Gd1 Ca2 34.63(3) 1_556 3_455 ?
O3 Gd1 Ca2 84.30(6) . 3_455 ?
O6 Gd1 Ca2 147.68(3) 3_554 3_455 ?
O4 Gd1 Ca2 130.08(3) . 3_455 ?
O4 Gd1 Ca2 74.59(3) 2_565 3_455 ?
O6 Gd1 Ca2 98.62(6) 3 3_455 ?
Gd1 Gd1 Ca2 117.149(5) 1_554 3_455 ?
Gd1 Gd1 Ca2 62.851(5) 1_556 3_455 ?
Ca2 Gd1 Ca2 56.815(10) 4_455 3_455 ?
O3 Gd1 Ca2 85.18(5) 1_556 4_454 ?
O3 Gd1 Ca2 33.80(3) . 4_454 ?
O6 Gd1 Ca2 98.87(5) 3_554 4_454 ?
O4 Gd1 Ca2 78.00(3) . 4_454 ?
O4 Gd1 Ca2 133.74(3) 2_565 4_454 ?
O6 Gd1 Ca2 147.87(3) 3 4_454 ?
Gd1 Gd1 Ca2 61.612(5) 1_554 4_454 ?
Gd1 Gd1 Ca2 118.387(5) 1_556 4_454 ?
Ca2 Gd1 Ca2 55.536(5) 4_455 4_454 ?
Ca2 Gd1 Ca2 83.203(9) 3_455 4_454 ?
O3 Gd1 Ca2 85.18(5) 1_556 3_454 ?
O3 Gd1 Ca2 33.80(3) . 3_454 ?
O6 Gd1 Ca2 98.87(5) 3_554 3_454 ?
O4 Gd1 Ca2 133.74(3) . 3_454 ?
O4 Gd1 Ca2 78.00(3) 2_565 3_454 ?
O6 Gd1 Ca2 147.87(3) 3 3_454 ?
Gd1 Gd1 Ca2 61.612(5) 1_554 3_454 ?
Gd1 Gd1 Ca2 118.387(5) 1_556 3_454 ?
Ca2 Gd1 Ca2 83.203(9) 4_455 3_454 ?
Ca2 Gd1 Ca2 55.536(5) 3_455 3_454 ?
Ca2 Gd1 Ca2 56.115(10) 4_454 3_454 ?
O1 Ca3 O4 102.13(5) . 4_455 ?
O1 Ca3 O4 101.32(5) . 4_456 ?
O4 Ca3 O4 98.67(5) 4_455 4_456 ?
O1 Ca3 O5 77.97(5) . . ?
O4 Ca3 O5 88.15(5) 4_455 . ?
O4 Ca3 O5 173.12(5) 4_456 . ?
O1 Ca3 O2 129.02(5) . 1_556 ?
O4 Ca3 O2 123.16(5) 4_455 1_556 ?
O4 Ca3 O2 94.24(5) 4_456 1_556 ?
O5 Ca3 O2 81.17(5) . 1_556 ?
O1 Ca3 O5 78.01(5) . 1_556 ?
O4 Ca3 O5 176.86(5) 4_455 1_556 ?
O4 Ca3 O5 84.36(5) 4_456 1_556 ?
O5 Ca3 O5 88.81(5) . 1_556 ?
O2 Ca3 O5 55.47(5) 1_556 1_556 ?
O1 Ca3 B1 99.18(5) . 1_556 ?
O4 Ca3 B1 148.11(5) 4_455 1_556 ?
O4 Ca3 B1 100.10(5) 4_456 1_556 ?
O5 Ca3 B1 73.38(6) . 1_556 ?
O2 Ca3 B1 29.94(5) 1_556 1_556 ?
O5 Ca3 B1 29.50(5) 1_556 1_556 ?
O1 Ca3 O5 156.13(5) . 4_455 ?
O4 Ca3 O5 54.04(4) 4_455 4_455 ?
O4 Ca3 O5 83.07(5) 4_456 4_455 ?
O5 Ca3 O5 100.38(4) . 4_455 ?
O2 Ca3 O5 73.29(4) 1_556 4_455 ?
O5 Ca3 O5 125.86(3) 1_556 4_455 ?
B1 Ca3 O5 103.14(5) 1_556 4_455 ?
O1 Ca3 B1 128.87(5) . 4_455 ?
O4 Ca3 B1 27.79(5) 4_455 4_455 ?
O4 Ca3 B1 85.23(5) 4_456 4_455 ?
O5 Ca3 B1 100.59(5) . 4_455 ?
O2 Ca3 B1 100.38(5) 1_556 4_455 ?
O5 Ca3 B1 152.71(5) 1_556 4_455 ?
B1 Ca3 B1 129.88(3) 1_556 4_455 ?
O5 Ca3 B1 27.45(5) 4_455 4_455 ?
O1 Ca3 O6 52.04(6) . . ?
O4 Ca3 O6 67.33(6) 4_455 . ?
O4 Ca3 O6 70.13(7) 4_456 . ?
O5 Ca3 O6 113.77(7) . . ?
O2 Ca3 O6 163.15(7) 1_556 . ?
O5 Ca3 O6 114.74(6) 1_556 . ?
B1 Ca3 O6 143.89(6) 1_556 . ?
O5 Ca3 O6 109.71(6) 4_455 . ?
B1 Ca3 O6 84.99(6) 4_455 . ?
O1 Ca3 B2 25.46(6) . . ?
O4 Ca3 B2 85.07(6) 4_455 . ?
O4 Ca3 B2 85.45(6) 4_456 . ?
O5 Ca3 B2 96.10(6) . . ?
O2 Ca3 B2 151.30(6) 1_556 . ?
O5 Ca3 B2 96.06(6) 1_556 . ?
B1 Ca3 B2 121.89(6) 1_556 . ?
O5 Ca3 B2 134.81(6) 4_455 . ?
B1 Ca3 B2 108.17(6) 4_455 . ?
O6 Ca3 B2 26.58(7) . . ?
O1 Ca3 B1 124.39(5) . 4_456 ?
O4 Ca3 B1 91.81(5) 4_455 4_456 ?
O4 Ca3 B1 23.09(5) 4_456 4_456 ?
O5 Ca3 B1 156.95(5) . 4_456 ?
O2 Ca3 B1 79.60(5) 1_556 4_456 ?
O5 Ca3 B1 90.67(5) 1_556 4_456 ?
B1 Ca3 B1 95.46(5) 1_556 4_456 ?
O5 Ca3 B1 61.84(5) 4_455 4_456 ?
B1 Ca3 B1 70.73(4) 4_455 4_456 ?
O6 Ca3 B1 87.27(6) . 4_456 ?
B2 Ca3 B1 106.87(6) . 4_456 ?
O2 Gd2 O3 88.88(7) 4_556 3_546 ?
O2 Gd2 O5 86.52(6) 4_556 . ?
O3 Gd2 O5 175.39(7) 3_546 . ?
O2 Gd2 O1 169.89(5) 4_556 1_554 ?
O3 Gd2 O1 101.17(7) 3_546 1_554 ?
O5 Gd2 O1 83.43(5) . 1_554 ?
O2 Gd2 O1 81.44(5) 4_556 . ?
O3 Gd2 O1 99.76(7) 3_546 . ?
O5 Gd2 O1 79.84(5) . . ?
O1 Gd2 O1 97.81(6) 1_554 . ?
O2 Gd2 O2 98.52(5) 4_556 4 ?
O3 Gd2 O2 90.24(7) 3_546 4 ?
O5 Gd2 O2 90.16(5) . 4 ?
O1 Gd2 O2 80.46(5) 1_554 4 ?
O1 Gd2 O2 169.99(5) . 4 ?
O2 Gd2 B1 75.34(5) 4_556 4 ?
O3 Gd2 B1 80.58(6) 3_546 4 ?
O5 Gd2 B1 97.95(5) . 4 ?
O1 Gd2 B1 104.94(5) 1_554 4 ?
O1 Gd2 B1 156.78(5) . 4 ?
O2 Gd2 B1 25.02(5) 4 4 ?
O2 Gd2 Ca2 138.67(4) 4_556 1_554 ?
O3 Gd2 Ca2 90.89(6) 3_546 1_554 ?
O5 Gd2 Ca2 92.38(4) . 1_554 ?
O1 Gd2 Ca2 41.19(4) 1_554 1_554 ?
O1 Gd2 Ca2 138.99(4) . 1_554 ?
O2 Gd2 Ca2 40.16(3) 4 1_554 ?
B1 Gd2 Ca2 63.89(4) 4 1_554 ?
O2 Gd2 Ca2 41.33(4) 4_556 1_556 ?
O3 Gd2 Ca2 89.11(6) 3_546 1_556 ?
O5 Gd2 Ca2 87.62(4) . 1_556 ?
O1 Gd2 Ca2 138.81(4) 1_554 1_556 ?
O1 Gd2 Ca2 41.01(4) . 1_556 ?
O2 Gd2 Ca2 139.84(3) 4 1_556 ?
B1 Gd2 Ca2 116.11(4) 4 1_556 ?
Ca2 Gd2 Ca2 180.0 1_554 1_556 ?
O2 Gd2 Ca3 43.60(4) 4_556 4 ?
O3 Gd2 Ca3 122.75(5) 3_546 4 ?
O5 Gd2 Ca3 53.12(4) . 4 ?
O1 Gd2 Ca3 127.44(4) 1_554 4 ?
O1 Gd2 Ca3 101.23(4) . 4 ?
O2 Gd2 Ca3 72.66(4) 4 4 ?
B1 Gd2 Ca3 60.96(4) 4 4 ?
Ca2 Gd2 Ca3 105.853(8) 1_554 4 ?
Ca2 Gd2 Ca3 74.147(8) 1_556 4 ?
O2 Gd2 Ca2 114.25(4) 4_556 2 ?
O3 Gd2 Ca2 39.15(5) 3_546 2 ?
O5 Gd2 Ca2 144.05(4) . 2 ?
O1 Gd2 Ca2 75.03(4) 1_554 2 ?
O1 Gd2 Ca2 75.08(3) . 2 ?
O2 Gd2 Ca2 113.64(4) 4 2 ?
B1 Gd2 Ca2 115.10(4) 4 2 ?
Ca2 Gd2 Ca2 90.0 1_554 2 ?
Ca2 Gd2 Ca2 90.0 1_556 2 ?
Ca3 Gd2 Ca2 157.391(7) 4 2 ?
O2 Gd2 Ca3 86.44(4) 4_556 . ?
O3 Gd2 Ca3 138.33(6) 3_546 . ?
O5 Gd2 Ca3 41.63(4) . . ?
O1 Gd2 Ca3 86.77(4) 1_554 . ?
O1 Gd2 Ca3 38.62(4) . . ?
O2 Gd2 Ca3 131.40(4) 4 . ?
B1 Gd2 Ca3 137.17(4) 4 . ?
Ca2 Gd2 Ca3 118.820(7) 1_554 . ?
Ca2 Gd2 Ca3 61.181(7) 1_556 . ?
Ca3 Gd2 Ca3 79.030(9) 4 . ?
Ca2 Gd2 Ca3 107.712(7) 2 . ?
B2 O1 Ca3 107.75(13) . . ?
B2 O1 Ca2 122.84(14) . 1_556 ?
Ca3 O1 Ca2 103.04(6) . 1_556 ?
B2 O1 Gd2 120.30(14) . . ?
Ca3 O1 Gd2 102.22(6) . . ?
Ca2 O1 Gd2 97.81(6) 1_556 . ?
B1 O2 Ca2 145.43(13) . 4_454 ?
B1 O2 Ca2 108.21(11) . 4_455 ?
Ca2 O2 Ca2 98.52(5) 4_454 4_455 ?
B1 O2 Ca3 86.62(10) . 1_554 ?
Ca2 O2 Ca3 96.05(5) 4_454 1_554 ?
Ca2 O2 Ca3 124.66(6) 4_455 1_554 ?
Gd1 O3 Gd1 104.20(10) 1_554 . ?
Gd1 O3 Ca2 112.14(7) 1_554 4_454 ?
Gd1 O3 Ca2 113.49(7) . 4_454 ?
Gd1 O3 Ca2 112.14(7) 1_554 3_454 ?
Gd1 O3 Ca2 113.49(7) . 3_454 ?
Ca2 O3 Ca2 101.70(9) 4_454 3_454 ?
B1 O4 Ca3 100.49(11) . 4 ?
B1 O4 Ca3 115.40(11) . 4_554 ?
Ca3 O4 Ca3 98.67(5) 4 4_554 ?
B1 O4 Gd1 110.82(11) . . ?
Ca3 O4 Gd1 118.24(6) 4 . ?
Ca3 O4 Gd1 112.44(6) 4_554 . ?
B1 O5 Gd2 138.11(12) . . ?
B1 O5 Ca3 122.28(12) . . ?
Gd2 O5 Ca3 99.17(5) . . ?
B1 O5 Ca3 80.85(11) . 1_554 ?
Gd2 O5 Ca3 95.36(5) . 1_554 ?
Ca3 O5 Ca3 88.81(5) . 1_554 ?
B1 O5 Ca3 79.30(10) . 4 ?
Gd2 O5 Ca3 85.90(5) . 4 ?
Ca3 O5 Ca3 119.35(6) . 4 ?
Ca3 O5 Ca3 151.32(6) 1_554 4 ?
B2 O6 Gd1 129.6(2) . 3_446 ?
B2 O6 Gd1 134.1(2) . 3_445 ?
Gd1 O6 Gd1 96.28(9) 3_446 3_445 ?
B2 O6 Ca3 80.46(5) . 2 ?
Gd1 O6 Ca3 95.17(6) 3_446 2 ?
Gd1 O6 Ca3 97.47(5) 3_445 2 ?
B2 O6 Ca3 80.46(5) . . ?
Gd1 O6 Ca3 95.17(6) 3_446 . ?
Gd1 O6 Ca3 97.47(5) 3_445 . ?
Ca3 O6 Ca3 160.77(10) 2 . ?
O5 B1 O2 118.96(17) . . ?
O5 B1 O4 120.89(16) . . ?
O2 B1 O4 120.15(16) . . ?
O5 B1 Ca3 69.65(10) . 1_554 ?
O2 B1 Ca3 63.44(9) . 1_554 ?
O4 B1 Ca3 141.16(13) . 1_554 ?
O5 B1 Ca3 73.25(10) . 4 ?
O2 B1 Ca3 157.49(13) . 4 ?
O4 B1 Ca3 51.72(9) . 4 ?
Ca3 B1 Ca3 137.66(7) 1_554 4 ?
O5 B1 Ca2 103.80(12) . 4_455 ?
O2 B1 Ca2 46.77(9) . 4_455 ?
O4 B1 Ca2 116.09(11) . 4_455 ?
Ca3 B1 Ca2 94.13(5) 1_554 4_455 ?
Ca3 B1 Ca2 114.16(6) 4 4_455 ?
O5 B1 Ca3 106.07(11) . 4_554 ?
O2 B1 Ca3 118.76(12) . 4_554 ?
O4 B1 Ca3 41.50(8) . 4_554 ?
Ca3 B1 Ca3 100.65(6) 1_554 4_554 ?
Ca3 B1 Ca3 70.73(4) 4 4_554 ?
Ca2 B1 Ca3 149.73(7) 4_455 4_554 ?
O1 B2 O1 120.5(2) . 2 ?
O1 B2 O6 119.73(12) . . ?
O1 B2 O6 119.73(12) 2 . ?
O1 B2 Ca3 167.28(16) . 2 ?
O1 B2 Ca3 46.78(8) 2 2 ?
O6 B2 Ca3 72.96(5) . 2 ?
O1 B2 Ca3 46.79(8) . . ?
O1 B2 Ca3 167.28(16) 2 . ?
O6 B2 Ca3 72.96(5) . . ?
Ca3 B2 Ca3 145.84(10) 2 . ?
O1 B2 Ca2 99.91(15) . 2 ?
O1 B2 Ca2 38.45(10) 2 2 ?
O6 B2 Ca2 127.83(13) . 2 ?
Ca3 B2 Ca2 70.44(3) 2 2 ?
Ca3 B2 Ca2 135.78(8) . 2 ?

_refine_diff_density_max         2.896
_refine_diff_density_min         -1.530
_refine_diff_density_rms         0.340

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

data_mo_TmCOB_100K_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2372141'
loop_
_audit_author_name
_audit_author_address

'fatiha azrour romain viennois jerome long dominique granier fapeng yu shujun zhang frederico alabarse mickael beaudhuin jerome rouquette'
;ICGM Univ Montpellier CNRS ENSCM  Montpellier France
France
;
_audit_update_record             
;
2024-07-19 deposited with the CCDC.	2024-11-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'B3 Ca4 O10 Tm'
_chemical_formula_sum            'B3 Ca4 O10 Tm'

_chemical_formula_weight         521.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source



B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.1943 3.0179 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_H-M_alt        'C m'
_space_group_name_Hall           'C -2y'

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

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

_cell_length_a                   8.0503(4)
_cell_length_b                   15.9908(7)
_cell_length_c                   3.5137(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.1745(10)
_cell_angle_gamma                90
_cell_volume                     443.75(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9709
_cell_measurement_theta_min      5.753
_cell_measurement_theta_max      144.7

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      3.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.904
_exptl_crystal_F_000             488
_exptl_transmission_factor_min   0.484
_exptl_transmission_factor_max   1
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.025
_exptl_absorpt_coefficient_mu    12.352
_shelx_estimated_absorpt_T_min   0.484
_shelx_estimated_absorpt_T_max   1
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.484
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'D8 VENTURE  '
_diffrn_measurement_method       'profile data from θ/2θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19054
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.547
_diffrn_reflns_theta_max         45.287
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.948
_reflns_number_total             3671
_reflns_number_gt                3671
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_max     0.946
_reflns_Friedel_fraction_full    0.913

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_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)+(0.0670P)²+0.9485P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.083(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1772 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3671
_refine_ls_number_parameters     91
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0851
_refine_ls_wR_factor_gt          0.0851
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm1 Tm 0.56243(2) 0.500000 0.47245(2) 0.00174(7) Uani 0.758(2) 2 d S T P . .
Ca2 Ca 0.70212(6) 0.11234(3) 0.79545(13) 0.00299(12) Uani 0.8788(11) 1 d . . P
. .
Ca3 Ca 0.31674(9) 0.18078(5) 1.1173(2) 0.00517(11) Uani 1 1 d . . . . .
Ca1 Ca 0.56243(2) 0.500000 0.47245(2) 0.00174(7) Uani 0.242(2) 2 d S T P . .
Tm2 Tm 0.70212(6) 0.11234(3) 0.79545(13) 0.00299(12) Uani 0.1212(11) 1 d . . P
. .
O1 O 0.5187(4) 0.07446(18) 1.2151(9) 0.0062(4) Uani 1 1 d . . . . .
O2 O 0.3446(4) 0.32484(19) 0.3494(9) 0.0061(3) Uani 1 1 d . . . . .
O3 O 0.3877(6) 0.500000 -0.1088(15) 0.0072(6) Uani 1 2 d S T P . .
O4 O 0.6391(4) 0.35858(19) 0.5400(8) 0.0053(3) Uani 1 1 d . . . . .
O5 O 0.5269(4) 0.23027(19) 0.7434(9) 0.0071(4) Uani 1 1 d . . . . .
O6 O 0.2586(7) 0.000000 1.0722(17) 0.0108(7) Uani 1 2 d S T P . .
B1 B 0.5049(5) 0.3049(2) 0.5449(12) 0.0044(5) Uani 1 1 d . . . . .
B2 B 0.4320(7) 0.000000 1.1675(17) 0.0041(6) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tm1 O3 2.224(5) 1_556 ?
Tm1 O3 2.244(5) . ?
Tm1 O6 2.309(5) 3_554 ?
Tm1 O4 2.344(3) . ?
Tm1 O4 2.344(3) 2_565 ?
Tm1 O6 2.376(6) 3 ?
Tm1 Tm1 3.5137(2) 1_554 ?
Tm1 Tm1 3.51371(19) 1_556 ?
Tm1 Ca2 3.7688(5) 4_455 ?
Tm1 Ca2 3.7688(5) 3_455 ?
Tm1 Ca2 3.8242(5) 4_454 ?
Tm1 Ca2 3.8242(5) 3_454 ?
Ca3 O4 2.330(3) 4_455 ?
Ca3 O1 2.332(3) . ?
Ca3 O4 2.339(3) 4_456 ?
Ca3 O2 2.440(3) 1_556 ?
Ca3 O5 2.465(3) . ?
Ca3 O5 2.624(3) 1_556 ?
Ca3 B1 2.758(4) 1_556 ?
Ca3 O5 2.829(4) 4_455 ?
Ca3 B1 2.906(4) 4_455 ?
Ca3 O6 2.9278(12) . ?
Ca3 B2 3.0308(19) . ?
Ca3 B1 3.174(4) 4_456 ?
Tm2 O2 2.291(3) 4_556 ?
Tm2 O3 2.319(3) 3_546 ?
Tm2 O2 2.341(3) 4 ?
Tm2 O5 2.341(3) . ?
Tm2 O1 2.353(3) 1_554 ?
Tm2 O1 2.359(3) . ?
O1 B2 1.374(4) . ?
O2 B1 1.377(5) . ?
O4 B1 1.382(5) . ?
O5 B1 1.377(5) . ?
O6 B2 1.371(8) . ?

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
O3 Tm1 O3 103.70(19) 1_556 . ?
O3 Tm1 O6 176.2(2) 1_556 3_554 ?
O3 Tm1 O6 80.09(19) . 3_554 ?
O3 Tm1 O4 96.94(8) 1_556 . ?
O3 Tm1 O4 101.45(7) . . ?
O6 Tm1 O4 82.18(7) 3_554 . ?
O3 Tm1 O4 96.94(8) 1_556 2_565 ?
O3 Tm1 O4 101.45(7) . 2_565 ?
O6 Tm1 O4 82.18(7) 3_554 2_565 ?
O4 Tm1 O4 149.48(14) . 2_565 ?
O3 Tm1 O6 79.06(19) 1_556 3 ?
O3 Tm1 O6 177.2(2) . 3 ?
O6 Tm1 O6 97.15(19) 3_554 3 ?
O4 Tm1 O6 78.08(7) . 3 ?
O4 Tm1 O6 78.08(7) 2_565 3 ?
O3 Tm1 Tm1 141.65(13) 1_556 1_554 ?
O3 Tm1 Tm1 37.95(12) . 1_554 ?
O6 Tm1 Tm1 42.14(14) 3_554 1_554 ?
O4 Tm1 Tm1 92.88(7) . 1_554 ?
O4 Tm1 Tm1 92.88(7) 2_565 1_554 ?
O6 Tm1 Tm1 139.29(13) 3 1_554 ?
O3 Tm1 Tm1 38.35(13) 1_556 1_556 ?
O3 Tm1 Tm1 142.05(12) . 1_556 ?
O6 Tm1 Tm1 137.86(14) 3_554 1_556 ?
O4 Tm1 Tm1 87.12(7) . 1_556 ?
O4 Tm1 Tm1 87.12(7) 2_565 1_556 ?
O6 Tm1 Tm1 40.70(13) 3 1_556 ?
Tm1 Tm1 Tm1 180.0 1_554 1_556 ?
O3 Tm1 Ca2 34.75(7) 1_556 4_455 ?
O3 Tm1 Ca2 83.73(11) . 4_455 ?
O6 Tm1 Ca2 147.19(7) 3_554 4_455 ?
O4 Tm1 Ca2 73.30(7) . 4_455 ?
O4 Tm1 Ca2 129.21(7) 2_565 4_455 ?
O6 Tm1 Ca2 98.69(11) 3 4_455 ?
Tm1 Tm1 Ca2 116.763(7) 1_554 4_455 ?
Tm1 Tm1 Ca2 63.238(7) 1_556 4_455 ?
O3 Tm1 Ca2 34.75(7) 1_556 3_455 ?
O3 Tm1 Ca2 83.73(11) . 3_455 ?
O6 Tm1 Ca2 147.19(7) 3_554 3_455 ?
O4 Tm1 Ca2 129.21(7) . 3_455 ?
O4 Tm1 Ca2 73.30(7) 2_565 3_455 ?
O6 Tm1 Ca2 98.69(11) 3 3_455 ?
Tm1 Tm1 Ca2 116.763(7) 1_554 3_455 ?
Tm1 Tm1 Ca2 63.238(7) 1_556 3_455 ?
Ca2 Tm1 Ca2 56.931(14) 4_455 3_455 ?
O3 Tm1 Ca2 84.88(12) 1_556 4_454 ?
O3 Tm1 Ca2 33.68(7) . 4_454 ?
O6 Tm1 Ca2 98.46(13) 3_554 4_454 ?
O4 Tm1 Ca2 76.29(7) . 4_454 ?
O4 Tm1 Ca2 132.01(7) 2_565 4_454 ?
O6 Tm1 Ca2 147.71(6) 3 4_454 ?
Tm1 Tm1 Ca2 61.638(7) 1_554 4_454 ?
Tm1 Tm1 Ca2 118.362(7) 1_556 4_454 ?
Ca2 Tm1 Ca2 55.124(7) 4_455 4_454 ?
Ca2 Tm1 Ca2 82.876(12) 3_455 4_454 ?
O3 Tm1 Ca2 84.88(12) 1_556 3_454 ?
O3 Tm1 Ca2 33.68(7) . 3_454 ?
O6 Tm1 Ca2 98.46(13) 3_554 3_454 ?
O4 Tm1 Ca2 132.01(7) . 3_454 ?
O4 Tm1 Ca2 76.29(7) 2_565 3_454 ?
O6 Tm1 Ca2 147.71(6) 3 3_454 ?
Tm1 Tm1 Ca2 61.638(7) 1_554 3_454 ?
Tm1 Tm1 Ca2 118.362(7) 1_556 3_454 ?
Ca2 Tm1 Ca2 82.876(12) 4_455 3_454 ?
Ca2 Tm1 Ca2 55.124(7) 3_455 3_454 ?
Ca2 Tm1 Ca2 56.034(14) 4_454 3_454 ?
O4 Ca3 O1 102.96(11) 4_455 . ?
O4 Ca3 O4 97.62(11) 4_455 4_456 ?
O1 Ca3 O4 101.83(11) . 4_456 ?
O4 Ca3 O2 123.17(10) 4_455 1_556 ?
O1 Ca3 O2 128.54(11) . 1_556 ?
O4 Ca3 O2 94.00(10) 4_456 1_556 ?
O4 Ca3 O5 89.52(11) 4_455 . ?
O1 Ca3 O5 77.38(10) . . ?
O4 Ca3 O5 172.80(11) 4_456 . ?
O2 Ca3 O5 81.19(10) 1_556 . ?
O4 Ca3 O5 176.67(10) 4_455 1_556 ?
O1 Ca3 O5 77.20(10) . 1_556 ?
O4 Ca3 O5 85.58(10) 4_456 1_556 ?
O2 Ca3 O5 55.42(9) 1_556 1_556 ?
O5 Ca3 O5 87.27(11) . 1_556 ?
O4 Ca3 B1 147.98(11) 4_455 1_556 ?
O1 Ca3 B1 98.67(11) . 1_556 ?
O4 Ca3 B1 100.75(11) 4_456 1_556 ?
O2 Ca3 B1 29.92(10) 1_556 1_556 ?
O5 Ca3 B1 72.43(12) . 1_556 ?
O5 Ca3 B1 29.50(11) 1_556 1_556 ?
O4 Ca3 O5 54.54(9) 4_455 4_455 ?
O1 Ca3 O5 157.50(10) . 4_455 ?
O4 Ca3 O5 83.08(9) 4_456 4_455 ?
O2 Ca3 O5 72.22(9) 1_556 4_455 ?
O5 Ca3 O5 100.40(8) . 4_455 ?
O5 Ca3 O5 125.26(6) 1_556 4_455 ?
B1 Ca3 O5 101.98(10) 1_556 4_455 ?
O4 Ca3 B1 27.95(11) 4_455 4_455 ?
O1 Ca3 B1 130.07(11) . 4_455 ?
O4 Ca3 B1 84.74(11) 4_456 4_455 ?
O2 Ca3 B1 99.68(10) 1_556 4_455 ?
O5 Ca3 B1 101.30(11) . 4_455 ?
O5 Ca3 B1 152.47(10) 1_556 4_455 ?
B1 Ca3 B1 129.04(7) 1_556 4_455 ?
O5 Ca3 B1 27.73(10) 4_455 4_455 ?
O4 Ca3 O6 67.77(14) 4_455 . ?
O1 Ca3 O6 52.23(12) . . ?
O4 Ca3 O6 69.99(13) 4_456 . ?
O2 Ca3 O6 162.53(14) 1_556 . ?
O5 Ca3 O6 114.02(13) . . ?
O5 Ca3 O6 114.42(13) 1_556 . ?
B1 Ca3 O6 143.62(14) 1_556 . ?
O5 Ca3 O6 111.26(12) 4_455 . ?
B1 Ca3 O6 86.15(13) 4_455 . ?
O4 Ca3 B2 85.55(14) 4_455 . ?
O1 Ca3 B2 25.71(13) . . ?
O4 Ca3 B2 85.67(13) 4_456 . ?
O2 Ca3 B2 150.93(13) 1_556 . ?
O5 Ca3 B2 95.92(13) . . ?
O5 Ca3 B2 95.65(13) 1_556 . ?
B1 Ca3 B2 121.67(14) 1_556 . ?
O5 Ca3 B2 136.23(13) 4_455 . ?
B1 Ca3 B2 109.21(14) 4_455 . ?
O6 Ca3 B2 26.53(14) . . ?
O4 Ca3 B1 91.33(11) 4_455 4_456 ?
O1 Ca3 B1 125.16(11) . 4_456 ?
O4 Ca3 B1 23.33(10) 4_456 4_456 ?
O2 Ca3 B1 78.67(10) 1_556 4_456 ?
O5 Ca3 B1 156.44(10) . 4_456 ?
O5 Ca3 B1 91.26(10) 1_556 4_456 ?
B1 Ca3 B1 95.25(11) 1_556 4_456 ?
O5 Ca3 B1 61.76(10) 4_455 4_456 ?
B1 Ca3 B1 70.46(9) 4_455 4_456 ?
O6 Ca3 B1 87.94(13) . 4_456 ?
B2 Ca3 B1 107.62(13) . 4_456 ?
O2 Tm2 O3 90.80(14) 4_556 3_546 ?
O2 Tm2 O2 98.69(11) 4_556 4 ?
O3 Tm2 O2 92.53(13) 3_546 4 ?
O2 Tm2 O5 84.72(11) 4_556 . ?
O3 Tm2 O5 175.52(15) 3_546 . ?
O2 Tm2 O5 88.17(10) 4 . ?
O2 Tm2 O1 167.39(11) 4_556 1_554 ?
O3 Tm2 O1 101.81(14) 3_546 1_554 ?
O2 Tm2 O1 80.61(10) 4 1_554 ?
O5 Tm2 O1 82.67(11) . 1_554 ?
O2 Tm2 O1 81.51(10) 4_556 . ?
O3 Tm2 O1 100.02(14) 3_546 . ?
O2 Tm2 O1 167.45(11) 4 . ?
O5 Tm2 O1 79.34(10) . . ?
O1 Tm2 O1 96.43(11) 1_554 . ?
O2 Tm2 Ca2 138.82(7) 4_556 1_554 ?
O3 Tm2 Ca2 91.16(13) 3_546 1_554 ?
O2 Tm2 Ca2 40.13(7) 4 1_554 ?
O5 Tm2 Ca2 92.22(7) . 1_554 ?
O1 Tm2 Ca2 41.85(7) 1_554 1_554 ?
O1 Tm2 Ca2 138.28(8) . 1_554 ?
O2 Tm2 Ca2 41.18(7) 4_556 1_556 ?
O3 Tm2 Ca2 88.84(13) 3_546 1_556 ?
O2 Tm2 Ca2 139.87(7) 4 1_556 ?
O5 Tm2 Ca2 87.78(7) . 1_556 ?
O1 Tm2 Ca2 138.15(7) 1_554 1_556 ?
O1 Tm2 Ca2 41.72(8) . 1_556 ?
Ca2 Tm2 Ca2 180.0 1_554 1_556 ?
O2 Tm2 Ca3 42.80(8) 4_556 4 ?
O3 Tm2 Ca3 123.63(10) 3_546 4 ?
O2 Tm2 Ca3 71.54(7) 4 4 ?
O5 Tm2 Ca3 52.50(9) . 4 ?
O1 Tm2 Ca3 126.52(7) 1_554 4 ?
O1 Tm2 Ca3 101.25(7) . 4 ?
Ca2 Tm2 Ca3 105.516(14) 1_554 4 ?
Ca2 Tm2 Ca3 74.486(14) 1_556 4 ?
O2 Tm2 Ca2 116.01(8) 4_556 2 ?
O3 Tm2 Ca2 39.22(9) 3_546 2 ?
O2 Tm2 Ca2 115.42(7) 4 2 ?
O5 Tm2 Ca2 143.67(8) . 2 ?
O1 Tm2 Ca2 75.08(7) 1_554 2 ?
O1 Tm2 Ca2 75.12(7) . 2 ?
Ca2 Tm2 Ca2 90.0 1_554 2 ?
Ca2 Tm2 Ca2 90.0 1_556 2 ?
Ca3 Tm2 Ca2 158.340(14) 4 2 ?
O2 Tm2 Ca3 85.49(8) 4_556 . ?
O3 Tm2 Ca3 138.23(11) 3_546 . ?
O2 Tm2 Ca3 129.18(8) 4 . ?
O5 Tm2 Ca3 41.50(8) . . ?
O1 Tm2 Ca3 85.29(8) 1_554 . ?
O1 Tm2 Ca3 38.27(8) . . ?
Ca2 Tm2 Ca3 118.172(14) 1_554 . ?
Ca2 Tm2 Ca3 61.829(14) 1_556 . ?
Ca3 Tm2 Ca3 78.898(16) 4 . ?
Ca2 Tm2 Ca3 107.354(14) 2 . ?
O2 Tm2 Ca3 129.64(8) 4_556 1_554 ?
O3 Tm2 Ca3 139.49(12) 3_546 1_554 ?
O2 Tm2 Ca3 84.27(7) 4 1_554 ?
O5 Tm2 Ca3 44.98(8) . 1_554 ?
O1 Tm2 Ca3 37.78(8) 1_554 1_554 ?
O1 Tm2 Ca3 86.00(8) . 1_554 ?
Ca2 Tm2 Ca3 61.155(13) 1_554 1_554 ?
Ca2 Tm2 Ca3 118.846(13) 1_556 1_554 ?
Ca3 Tm2 Ca3 93.624(15) 4 1_554 ?
Ca2 Tm2 Ca3 107.241(14) 2 1_554 ?
Ca3 Tm2 Ca3 57.017(13) . 1_554 ?
B2 O1 Ca3 106.9(3) . . ?
B2 O1 Ca2 123.2(3) . 1_556 ?
Ca3 O1 Ca2 104.04(12) . 1_556 ?
B2 O1 Tm2 120.7(3) . . ?
Ca3 O1 Tm2 102.93(11) . . ?
Ca2 O1 Tm2 96.43(11) 1_556 . ?
B1 O2 Ca2 142.4(3) . 4_454 ?
B1 O2 Ca2 107.4(2) . 4_455 ?
Ca2 O2 Ca2 98.69(11) 4_454 4_455 ?
B1 O2 Ca3 88.0(2) . 1_554 ?
Ca2 O2 Ca3 97.57(11) 4_454 1_554 ?
Ca2 O2 Ca3 127.15(13) 4_455 1_554 ?
Tm1 O3 Tm1 103.70(19) 1_554 . ?
Tm1 O3 Ca2 112.11(16) 1_554 4_454 ?
Tm1 O3 Ca2 113.87(15) . 4_454 ?
Tm1 O3 Ca2 112.11(16) 1_554 3_454 ?
Tm1 O3 Ca2 113.87(15) . 3_454 ?
Ca2 O3 Ca2 101.55(18) 4_454 3_454 ?
B1 O4 Ca3 99.8(2) . 4 ?
B1 O4 Ca3 114.6(2) . 4_554 ?
Ca3 O4 Ca3 97.61(11) 4 4_554 ?
B1 O4 Tm1 114.1(2) . . ?
Ca3 O4 Tm1 116.99(12) 4 . ?
Ca3 O4 Tm1 112.12(12) 4_554 . ?
B1 O5 Tm2 139.0(2) . . ?
B1 O5 Ca3 120.9(2) . . ?
Tm2 O5 Ca3 99.51(11) . . ?
B1 O5 Ca3 80.7(2) . 1_554 ?
Tm2 O5 Ca3 95.93(11) . 1_554 ?
Ca3 O5 Ca3 87.27(11) . 1_554 ?
B1 O5 Ca3 79.2(2) . 4 ?
Tm2 O5 Ca3 86.48(10) . 4 ?
Ca3 O5 Ca3 120.22(12) . 4 ?
Ca3 O5 Ca3 151.71(12) 1_554 4 ?
B2 O6 Tm1 129.5(4) . 3_446 ?
B2 O6 Tm1 133.4(4) . 3_445 ?
Tm1 O6 Tm1 97.15(19) 3_446 3_445 ?
B2 O6 Ca3 80.93(10) . . ?
Tm1 O6 Ca3 95.05(11) 3_446 . ?
Tm1 O6 Ca3 96.88(12) 3_445 . ?
B2 O6 Ca3 80.93(10) . 2 ?
Tm1 O6 Ca3 95.05(11) 3_446 2 ?
Tm1 O6 Ca3 96.88(12) 3_445 2 ?
Ca3 O6 Ca3 161.8(2) . 2 ?
O5 B1 O2 118.0(3) . . ?
O5 B1 O4 121.4(3) . . ?
O2 B1 O4 120.6(3) . . ?
O5 B1 Ca3 69.8(2) . 1_554 ?
O2 B1 Ca3 62.11(19) . 1_554 ?
O4 B1 Ca3 142.0(3) . 1_554 ?
O5 B1 Ca3 73.0(2) . 4 ?
O2 B1 Ca3 158.1(3) . 4 ?
O4 B1 Ca3 52.21(18) . 4 ?
Ca3 B1 Ca3 138.01(15) 1_554 4 ?
O5 B1 Ca2 105.2(2) . 4_455 ?
O2 B1 Ca2 47.09(18) . 4_455 ?
O4 B1 Ca2 113.9(2) . 4_455 ?
Ca3 B1 Ca2 94.83(11) 1_554 4_455 ?
Ca3 B1 Ca2 113.43(13) 4 4_455 ?
O5 B1 Ca3 105.5(2) . 4_554 ?
O2 B1 Ca3 119.9(3) . 4_554 ?
O4 B1 Ca3 42.07(16) . 4_554 ?
Ca3 B1 Ca3 101.26(12) 1_554 4_554 ?
Ca3 B1 Ca3 70.46(9) 4 4_554 ?
Ca2 B1 Ca3 148.78(14) 4_455 4_554 ?
O6 B2 O1 119.9(3) . . ?
O6 B2 O1 119.9(3) . 2 ?
O1 B2 O1 120.1(5) . 2 ?
O6 B2 Ca3 72.54(11) . . ?
O1 B2 Ca3 47.40(18) . . ?
O1 B2 Ca3 167.5(4) 2 . ?
O6 B2 Ca3 72.54(11) . 2 ?
O1 B2 Ca3 167.5(4) . 2 ?
O1 B2 Ca3 47.40(18) 2 2 ?
Ca3 B2 Ca3 145.0(2) . 2 ?
O6 B2 Ca2 128.7(3) . 2 ?
O1 B2 Ca2 99.4(3) . 2 ?
O1 B2 Ca2 38.2(2) 2 2 ?
Ca3 B2 Ca2 135.90(16) . 2 ?
Ca3 B2 Ca2 70.96(5) 2 2 ?

_refine_diff_density_max         4.930
_refine_diff_density_min         -5.653
_refine_diff_density_rms         0.554

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

data_mo_PrCOB_100K_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2400871'
loop_
_audit_author_name
_audit_author_address
'fatiha azrour mickael beaudhuin jerome rouquette'
;Universite de montpellier
France
;
_audit_update_record             
;
2024-11-06 deposited with the CCDC.	2024-11-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'B3 Ca4 O10 Pr'
_chemical_formula_sum            'B3 Ca4 O10 Pr'

_chemical_formula_weight         493.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source



B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 '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'


_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_H-M_alt        'C m'
_space_group_name_Hall           'C -2y'

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

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

_cell_length_a                   8.1188(2)
_cell_length_b                   16.0589(3)
_cell_length_c                   3.59720(10)
_cell_angle_alpha                90
_cell_angle_beta                 101.41
_cell_angle_gamma                90
_cell_volume                     459.725(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9554
_cell_measurement_theta_min      5.073
_cell_measurement_theta_max      144.8

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      3.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.566
_exptl_crystal_F_000             468
_exptl_transmission_factor_min   0.733
_exptl_transmission_factor_max   1
_exptl_crystal_size_max          0.113
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.049
_exptl_absorpt_coefficient_mu    7.572
_shelx_estimated_absorpt_T_min   0.733
_shelx_estimated_absorpt_T_max   1
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'D8 VENTURE'
_diffrn_measurement_method       'profile data from θ/2θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36185
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.537
_diffrn_reflns_theta_max         72.654
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_point_group_measured_fraction_full 0.953
_reflns_number_total             8810
_reflns_number_gt                8809
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_max     0.866
_reflns_Friedel_fraction_full    0.914

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1252P)²+0.0296P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.035(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.968(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8810
_refine_ls_number_parameters     92
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1298
_refine_ls_wR_factor_gt          0.1298
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.56242(2) 0.500000 0.47226(2) 0.00294(3) Uani 0.993(2) 2 d S T P . .
Ca2 Ca 0.70656(5) 0.11362(2) 0.80328(11) 0.00285(7) Uani 0.9965(12) 1 d . . P .
.
Ca3 Ca 0.33173(6) 0.18181(3) 1.13623(12) 0.00434(5) Uani 1 1 d . . . . .
Ca1 Ca 0.56242(2) 0.500000 0.47226(2) 0.00294(3) Uani 0.007(2) 2 d S T P . .
Pr2 Pr 0.70656(5) 0.11362(2) 0.80328(11) 0.00285(7) Uani 0.0035(12) 1 d . . P .
.
O1 O 0.5300(3) 0.07456(10) 1.2261(5) 0.00526(17) Uani 1 1 d . . . . .
O2 O 0.3632(2) 0.33012(12) 0.3611(5) 0.00573(18) Uani 1 1 d . . . . .
O3 O 0.3857(3) 0.500000 -0.1113(7) 0.0036(2) Uani 1 2 d S T P . .
O4 O 0.6588(2) 0.35384(11) 0.5613(5) 0.00495(16) Uani 1 1 d . . . . .
O5 O 0.5314(3) 0.23016(11) 0.7506(6) 0.0064(2) Uani 1 1 d . . . . .
O6 O 0.2708(4) 0.000000 1.0817(9) 0.0078(4) Uani 1 2 d S T P . .
B1 B 0.5178(4) 0.30469(16) 0.5591(8) 0.0038(2) Uani 1 1 d . . . . .
B2 B 0.4446(5) 0.000000 1.1797(11) 0.0033(3) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 O3 2.270(3) 1_556 ?
Pr1 O3 2.296(3) . ?
Pr1 O6 2.404(3) 3_554 ?
Pr1 O4 2.4747(18) 2_565 ?
Pr1 O4 2.4748(18) . ?
Pr1 O6 2.490(3) 3 ?
Pr1 Pr1 3.59719(9) 1_556 ?
Pr1 Pr1 3.59721(10) 1_554 ?
Pr1 Ca2 3.8020(4) 4_455 ?
Pr1 Ca2 3.8020(4) 3_455 ?
Pr1 Ca2 3.8361(4) 4_454 ?
Pr1 Ca2 3.8361(4) 3_454 ?
Ca3 O4 2.330(2) 4_455 ?
Ca3 O1 2.336(2) . ?
Ca3 O4 2.342(2) 4_456 ?
Ca3 O5 2.459(2) . ?
Ca3 O2 2.512(2) 1_556 ?
Ca3 O5 2.588(2) 1_556 ?
Ca3 B1 2.753(3) 1_556 ?
Ca3 O5 2.921(2) 4_455 ?
Ca3 B1 2.960(3) 4_455 ?
Ca3 O6 2.9612(7) . ?
Ca3 B2 3.0547(12) . ?
Ca3 B1 3.224(3) 4_456 ?
Pr2 O3 2.3157(17) 3_546 ?
Pr2 O2 2.3346(18) 4_556 ?
Pr2 O5 2.3355(18) . ?
Pr2 O1 2.362(2) 1_554 ?
Pr2 O1 2.372(2) . ?
Pr2 O2 2.401(2) 4 ?
Pr2 B1 3.123(3) 4 ?
O1 B2 1.377(3) . ?
O2 B1 1.377(3) . ?
O4 B1 1.389(3) . ?
O5 B1 1.374(3) . ?
O6 B2 1.385(5) . ?

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
O3 Pr1 O3 103.95(11) 1_556 . ?
O3 Pr1 O6 174.65(9) 1_556 3_554 ?
O3 Pr1 O6 81.39(11) . 3_554 ?
O3 Pr1 O4 98.02(5) 1_556 2_565 ?
O3 Pr1 O4 104.04(5) . 2_565 ?
O6 Pr1 O4 80.48(5) 3_554 2_565 ?
O3 Pr1 O4 98.02(5) 1_556 . ?
O3 Pr1 O4 104.04(5) . . ?
O6 Pr1 O4 80.48(5) 3_554 . ?
O4 Pr1 O4 143.03(9) 2_565 . ?
O3 Pr1 O6 80.04(11) 1_556 3 ?
O3 Pr1 O6 176.00(10) . 3 ?
O6 Pr1 O6 94.61(11) 3_554 3 ?
O4 Pr1 O6 75.15(5) 2_565 3 ?
O4 Pr1 O6 75.15(5) . 3 ?
O3 Pr1 Pr1 38.28(7) 1_556 1_556 ?
O3 Pr1 Pr1 142.24(7) . 1_556 ?
O6 Pr1 Pr1 136.37(7) 3_554 1_556 ?
O4 Pr1 Pr1 86.17(4) 2_565 1_556 ?
O4 Pr1 Pr1 86.17(4) . 1_556 ?
O6 Pr1 Pr1 41.76(8) 3 1_556 ?
O3 Pr1 Pr1 141.72(7) 1_556 1_554 ?
O3 Pr1 Pr1 37.76(7) . 1_554 ?
O6 Pr1 Pr1 43.63(7) 3_554 1_554 ?
O4 Pr1 Pr1 93.83(4) 2_565 1_554 ?
O4 Pr1 Pr1 93.83(4) . 1_554 ?
O6 Pr1 Pr1 138.24(8) 3 1_554 ?
Pr1 Pr1 Pr1 180.0 1_556 1_554 ?
O3 Pr1 Ca2 34.38(4) 1_556 4_455 ?
O3 Pr1 Ca2 84.85(6) . 4_455 ?
O6 Pr1 Ca2 148.15(3) 3_554 4_455 ?
O4 Pr1 Ca2 130.92(4) 2_565 4_455 ?
O4 Pr1 Ca2 75.21(4) . 4_455 ?
O6 Pr1 Ca2 98.64(7) 3 4_455 ?
Pr1 Pr1 Ca2 62.384(6) 1_556 4_455 ?
Pr1 Pr1 Ca2 117.616(6) 1_554 4_455 ?
O3 Pr1 Ca2 34.38(4) 1_556 3_455 ?
O3 Pr1 Ca2 84.85(6) . 3_455 ?
O6 Pr1 Ca2 148.15(3) 3_554 3_455 ?
O4 Pr1 Ca2 75.21(4) 2_565 3_455 ?
O4 Pr1 Ca2 130.92(4) . 3_455 ?
O6 Pr1 Ca2 98.64(7) 3 3_455 ?
Pr1 Pr1 Ca2 62.384(6) 1_556 3_455 ?
Pr1 Pr1 Ca2 117.616(6) 1_554 3_455 ?
Ca2 Pr1 Ca2 57.357(12) 4_455 3_455 ?
O3 Pr1 Ca2 85.30(6) 1_556 4_454 ?
O3 Pr1 Ca2 33.88(4) . 4_454 ?
O6 Pr1 Ca2 99.39(6) 3_554 4_454 ?
O4 Pr1 Ca2 135.39(4) 2_565 4_454 ?
O4 Pr1 Ca2 79.03(4) . 4_454 ?
O6 Pr1 Ca2 148.04(3) 3 4_454 ?
Pr1 Pr1 Ca2 118.574(6) 1_556 4_454 ?
Pr1 Pr1 Ca2 61.426(6) 1_554 4_454 ?
Ca2 Pr1 Ca2 56.190(6) 4_455 4_454 ?
Ca2 Pr1 Ca2 84.264(10) 3_455 4_454 ?
O3 Pr1 Ca2 85.30(6) 1_556 3_454 ?
O3 Pr1 Ca2 33.88(3) . 3_454 ?
O6 Pr1 Ca2 99.39(6) 3_554 3_454 ?
O4 Pr1 Ca2 79.03(4) 2_565 3_454 ?
O4 Pr1 Ca2 135.39(4) . 3_454 ?
O6 Pr1 Ca2 148.04(3) 3 3_454 ?
Pr1 Pr1 Ca2 118.574(6) 1_556 3_454 ?
Pr1 Pr1 Ca2 61.426(6) 1_554 3_454 ?
Ca2 Pr1 Ca2 84.264(11) 4_455 3_454 ?
Ca2 Pr1 Ca2 56.190(6) 3_455 3_454 ?
Ca2 Pr1 Ca2 56.801(12) 4_454 3_454 ?
O4 Ca3 O1 102.68(6) 4_455 . ?
O4 Ca3 O4 100.70(8) 4_455 4_456 ?
O1 Ca3 O4 102.42(7) . 4_456 ?
O4 Ca3 O5 85.73(7) 4_455 . ?
O1 Ca3 O5 78.33(6) . . ?
O4 Ca3 O5 173.11(8) 4_456 . ?
O4 Ca3 O2 121.60(6) 4_455 1_556 ?
O1 Ca3 O2 129.13(6) . 1_556 ?
O4 Ca3 O2 93.29(7) 4_456 1_556 ?
O5 Ca3 O2 81.13(7) . 1_556 ?
O4 Ca3 O5 175.96(7) 4_455 1_556 ?
O1 Ca3 O5 78.75(6) . 1_556 ?
O4 Ca3 O5 82.59(7) 4_456 1_556 ?
O5 Ca3 O5 90.89(8) . 1_556 ?
O2 Ca3 O5 55.52(6) 1_556 1_556 ?
O4 Ca3 B1 146.62(7) 4_455 1_556 ?
O1 Ca3 B1 99.45(7) . 1_556 ?
O4 Ca3 B1 98.55(8) 4_456 1_556 ?
O5 Ca3 B1 74.60(8) . 1_556 ?
O2 Ca3 B1 29.87(7) 1_556 1_556 ?
O5 Ca3 B1 29.61(7) 1_556 1_556 ?
O4 Ca3 O5 52.95(6) 4_455 4_455 ?
O1 Ca3 O5 155.56(6) . 4_455 ?
O4 Ca3 O5 82.90(6) 4_456 4_455 ?
O5 Ca3 O5 99.26(6) . 4_455 ?
O2 Ca3 O5 73.51(5) 1_556 4_455 ?
O5 Ca3 O5 125.69(4) 1_556 4_455 ?
B1 Ca3 O5 103.34(7) 1_556 4_455 ?
O4 Ca3 B1 27.28(7) 4_455 4_455 ?
O1 Ca3 B1 128.71(7) . 4_455 ?
O4 Ca3 B1 86.07(7) 4_456 4_455 ?
O5 Ca3 B1 98.83(8) . 4_455 ?
O2 Ca3 B1 100.08(7) 1_556 4_455 ?
O5 Ca3 B1 152.13(7) 1_556 4_455 ?
B1 Ca3 B1 129.59(5) 1_556 4_455 ?
O5 Ca3 B1 27.02(6) 4_455 4_455 ?
O4 Ca3 O6 68.62(8) 4_455 . ?
O1 Ca3 O6 51.96(7) . . ?
O4 Ca3 O6 71.85(8) 4_456 . ?
O5 Ca3 O6 113.21(8) . . ?
O2 Ca3 O6 163.97(8) 1_556 . ?
O5 Ca3 O6 114.87(7) 1_556 . ?
B1 Ca3 O6 144.04(9) 1_556 . ?
O5 Ca3 O6 109.45(7) 4_455 . ?
B1 Ca3 O6 85.20(8) 4_455 . ?
O4 Ca3 B2 86.13(8) 4_455 . ?
O1 Ca3 B2 25.41(9) . . ?
O4 Ca3 B2 86.87(9) 4_456 . ?
O5 Ca3 B2 96.09(9) . . ?
O2 Ca3 B2 151.56(8) 1_556 . ?
O5 Ca3 B2 96.45(8) 1_556 . ?
B1 Ca3 B2 122.04(9) 1_556 . ?
O5 Ca3 B2 134.48(8) 4_455 . ?
B1 Ca3 B2 108.29(9) 4_455 . ?
O6 Ca3 B2 26.56(9) . . ?
O4 Ca3 B1 92.38(7) 4_455 4_456 ?
O1 Ca3 B1 124.88(7) . 4_456 ?
O4 Ca3 B1 22.54(7) 4_456 4_456 ?
O5 Ca3 B1 156.37(6) . 4_456 ?
O2 Ca3 B1 79.85(7) 1_556 4_456 ?
O5 Ca3 B1 89.83(7) 1_556 4_456 ?
B1 Ca3 B1 95.14(7) 1_556 4_456 ?
O5 Ca3 B1 61.82(6) 4_455 4_456 ?
B1 Ca3 B1 71.00(6) 4_455 4_456 ?
O6 Ca3 B1 87.72(8) . 4_456 ?
B2 Ca3 B1 107.30(9) . 4_456 ?
O3 Pr2 O2 88.28(8) 3_546 4_556 ?
O3 Pr2 O5 176.96(9) 3_546 . ?
O2 Pr2 O5 88.80(8) 4_556 . ?
O3 Pr2 O1 99.40(8) 3_546 1_554 ?
O2 Pr2 O1 172.20(7) 4_556 1_554 ?
O5 Pr2 O1 83.55(8) . 1_554 ?
O3 Pr2 O1 98.63(8) 3_546 . ?
O2 Pr2 O1 81.18(7) 4_556 . ?
O5 Pr2 O1 80.12(7) . . ?
O1 Pr2 O1 98.91(7) 1_554 . ?
O3 Pr2 O2 89.04(8) 3_546 4 ?
O2 Pr2 O2 98.86(7) 4_556 4 ?
O5 Pr2 O2 92.21(7) . 4 ?
O1 Pr2 O2 80.01(6) 1_554 4 ?
O1 Pr2 O2 172.33(7) . 4 ?
O3 Pr2 B1 81.16(7) 3_546 4 ?
O2 Pr2 B1 75.27(7) 4_556 4 ?
O5 Pr2 B1 98.87(7) . 4 ?
O1 Pr2 B1 104.38(7) 1_554 4 ?
O1 Pr2 B1 156.45(7) . 4 ?
O2 Pr2 B1 24.71(7) 4 4 ?
O3 Pr2 Ca3 123.38(6) 3_546 4 ?
O2 Pr2 Ca3 44.44(5) 4_556 4 ?
O5 Pr2 Ca3 54.47(6) . 4 ?
O1 Pr2 Ca3 128.41(4) 1_554 4 ?
O1 Pr2 Ca3 101.30(4) . 4 ?
O2 Pr2 Ca3 73.94(5) 4 4 ?
B1 Pr2 Ca3 61.06(5) 4 4 ?
O3 Pr2 Ca2 89.52(6) 3_546 1_556 ?
O2 Pr2 Ca2 41.26(5) 4_556 1_556 ?
O5 Pr2 Ca2 87.75(5) . 1_556 ?
O1 Pr2 Ca2 139.36(5) 1_554 1_556 ?
O1 Pr2 Ca2 40.45(5) . 1_556 ?
O2 Pr2 Ca2 140.11(4) 4 1_556 ?
B1 Pr2 Ca2 116.19(5) 4 1_556 ?
Ca3 Pr2 Ca2 73.812(10) 4 1_556 ?
O3 Pr2 Ca2 90.48(6) 3_546 1_554 ?
O2 Pr2 Ca2 138.74(5) 4_556 1_554 ?
O5 Pr2 Ca2 92.26(5) . 1_554 ?
O1 Pr2 Ca2 40.64(5) 1_554 1_554 ?
O1 Pr2 Ca2 139.55(5) . 1_554 ?
O2 Pr2 Ca2 39.89(4) 4 1_554 ?
B1 Pr2 Ca2 63.81(5) 4 1_554 ?
Ca3 Pr2 Ca2 106.189(10) 4 1_554 ?
Ca2 Pr2 Ca2 180.0 1_556 1_554 ?
O3 Pr2 Ca2 38.01(5) 3_546 2 ?
O2 Pr2 Ca2 112.77(5) 4_556 2 ?
O5 Pr2 Ca2 143.26(6) . 2 ?
O1 Pr2 Ca2 74.60(4) 1_554 2 ?
O1 Pr2 Ca2 74.66(4) . 2 ?
O2 Pr2 Ca2 112.11(5) 4 2 ?
B1 Pr2 Ca2 114.83(5) 4 2 ?
Ca3 Pr2 Ca2 156.785(10) 4 2 ?
Ca2 Pr2 Ca2 90.0 1_556 2 ?
Ca2 Pr2 Ca2 90.0 1_554 2 ?
O3 Pr2 Ca3 138.03(6) 3_546 1_554 ?
O2 Pr2 Ca3 133.66(5) 4_556 1_554 ?
O5 Pr2 Ca3 44.87(6) . 1_554 ?
O1 Pr2 Ca3 38.75(5) 1_554 1_554 ?
O1 Pr2 Ca3 88.27(5) . 1_554 ?
O2 Pr2 Ca3 86.19(5) 4 1_554 ?
B1 Pr2 Ca3 107.74(5) 4 1_554 ?
Ca3 Pr2 Ca3 95.123(12) 4 1_554 ?
Ca2 Pr2 Ca3 119.494(10) 1_556 1_554 ?
Ca2 Pr2 Ca3 60.508(10) 1_554 1_554 ?
Ca2 Pr2 Ca3 107.454(10) 2 1_554 ?
B2 O1 Ca3 107.91(19) . . ?
B2 O1 Ca2 122.74(19) . 1_556 ?
Ca3 O1 Ca2 101.98(7) . 1_556 ?
B2 O1 Pr2 120.4(2) . . ?
Ca3 O1 Pr2 101.75(7) . . ?
Ca2 O1 Pr2 98.91(7) 1_556 . ?
B1 O2 Ca2 147.69(17) . 4_454 ?
B1 O2 Ca2 108.49(16) . 4_455 ?
Ca2 O2 Ca2 98.86(7) 4_454 4_455 ?
B1 O2 Ca3 84.81(14) . 1_554 ?
Ca2 O2 Ca3 94.97(7) 4_454 1_554 ?
Ca2 O2 Ca3 122.46(9) 4_455 1_554 ?
Pr1 O3 Pr1 103.96(11) 1_554 . ?
Pr1 O3 Ca2 112.02(8) 1_554 4_454 ?
Pr1 O3 Ca2 112.56(7) . 4_454 ?
Pr1 O3 Ca2 112.02(8) 1_554 3_454 ?
Pr1 O3 Ca2 112.56(7) . 3_454 ?
Ca2 O3 Ca2 103.99(11) 4_454 3_454 ?
B1 O4 Ca3 102.51(15) . 4 ?
B1 O4 Ca3 117.20(15) . 4_554 ?
Ca3 O4 Ca3 100.70(8) 4 4_554 ?
B1 O4 Pr1 107.40(15) . . ?
Ca3 O4 Pr1 117.88(7) 4 . ?
Ca3 O4 Pr1 111.24(7) 4_554 . ?
B1 O5 Pr2 136.53(17) . . ?
B1 O5 Ca3 124.14(16) . . ?
Pr2 O5 Ca3 99.21(6) . . ?
B1 O5 Ca3 81.88(15) . 1_554 ?
Pr2 O5 Ca3 95.59(7) . 1_554 ?
Ca3 O5 Ca3 90.89(8) . 1_554 ?
B1 O5 Ca3 78.07(15) . 4 ?
Pr2 O5 Ca3 84.93(7) . 4 ?
Ca3 O5 Ca3 117.81(8) . 4 ?
Ca3 O5 Ca3 150.91(8) 1_554 4 ?
B2 O6 Pr1 130.6(2) . 3_446 ?
B2 O6 Pr1 134.8(3) . 3_445 ?
Pr1 O6 Pr1 94.61(11) 3_446 3_445 ?
B2 O6 Ca3 80.49(6) . . ?
Pr1 O6 Ca3 95.10(6) 3_446 . ?
Pr1 O6 Ca3 97.69(6) 3_445 . ?
B2 O6 Ca3 80.49(6) . 2 ?
Pr1 O6 Ca3 95.10(6) 3_446 2 ?
Pr1 O6 Ca3 97.69(6) 3_445 2 ?
Ca3 O6 Ca3 160.77(12) . 2 ?
O5 B1 O2 119.5(2) . . ?
O5 B1 O4 120.5(2) . . ?
O2 B1 O4 120.0(2) . . ?
O5 B1 Ca3 68.51(15) . 1_554 ?
O2 B1 Ca3 65.32(14) . 1_554 ?
O4 B1 Ca3 140.51(18) . 1_554 ?
O5 B1 Ca3 74.91(15) . 4 ?
O2 B1 Ca3 155.72(18) . 4 ?
O4 B1 Ca3 50.22(12) . 4 ?
Ca3 B1 Ca3 137.92(10) 1_554 4 ?
O5 B1 Ca2 102.36(16) . 4_455 ?
O2 B1 Ca2 46.80(12) . 4_455 ?
O4 B1 Ca2 118.12(16) . 4_455 ?
Ca3 B1 Ca2 94.04(8) 1_554 4_455 ?
Ca3 B1 Ca2 113.85(9) 4 4_455 ?
O5 B1 Ca3 107.61(16) . 4_554 ?
O2 B1 Ca3 117.45(17) . 4_554 ?
O4 B1 Ca3 40.26(11) . 4_554 ?
Ca3 B1 Ca3 100.72(8) 1_554 4_554 ?
Ca3 B1 Ca3 71.00(6) 4 4_554 ?
Ca2 B1 Ca3 149.73(9) 4_455 4_554 ?
O1 B2 O1 120.8(3) . 2 ?
O1 B2 O6 119.61(17) . . ?
O1 B2 O6 119.61(17) 2 . ?
O1 B2 Ca3 46.69(12) . . ?
O1 B2 Ca3 167.4(2) 2 . ?
O6 B2 Ca3 72.95(7) . . ?
O1 B2 Ca3 167.4(2) . 2 ?
O1 B2 Ca3 46.69(12) 2 2 ?
O6 B2 Ca3 72.95(7) . 2 ?
Ca3 B2 Ca3 145.79(14) . 2 ?

_refine_diff_density_max         10.086
_refine_diff_density_min         -9.194
_refine_diff_density_rms         0.439

