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

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

data_3_sq
_database_code_depnum_ccdc_archive 'CCDC 1866609'
_audit_update_record             
;
2018-09-09 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Be6C24H48ClO16 + CH2Cl2'
_chemical_formula_sum            'C25 H50 Be6 Cl6 O16'
_chemical_formula_weight         873.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Be Be 0.0005 0.0002 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   19.481(4)
_cell_length_b                   9.5492(19)
_cell_length_c                   21.762(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.72(3)
_cell_angle_gamma                90
_cell_volume                     3877.2(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9356
_cell_measurement_theta_min      4.21
_cell_measurement_theta_max      64.17

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_F_000             1816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    0.509
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  STOE_IPDS_2
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10000
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.324
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             3895
_reflns_number_gt                3201
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0669P)²+7.1537P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3895
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0525
_refine_ls_wR_factor_ref         0.1482
_refine_ls_wR_factor_gt          0.1403
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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
Cl1 Cl 0.64891(3) 0.55103(7) 0.40524(3) 0.03093(18) Uani 1 1 d . . . . .
Cl2 Cl 0.62733(4) 0.76965(7) 0.65107(4) 0.03583(19) Uani 1 1 d . . . . .
O1 O 0.66196(9) 0.5974(2) 0.54574(10) 0.0289(4) Uani 1 1 d . . . . .
O2 O 0.63664(12) 0.0991(2) 0.49081(12) 0.0417(5) Uani 1 1 d . . . . .
O3 O 0.58362(9) 0.46888(19) 0.61215(9) 0.0259(4) Uani 1 1 d . . . . .
O4 O 0.57507(9) 0.39698(19) 0.49285(9) 0.0250(4) Uani 1 1 d . . . . .
O5 O 0.56719(10) 0.1955(2) 0.57808(12) 0.0380(5) Uani 1 1 d . . . . .
O6 O 0.46179(9) 0.34094(18) 0.53821(9) 0.0225(4) Uani 1 1 d . . . . .
O7 O 0.72925(10) 0.5313(2) 0.65594(9) 0.0294(4) Uani 1 1 d . . . . .
O8 O 0.67258(10) 0.3543(2) 0.72912(10) 0.0309(4) Uani 1 1 d . . . . .
C1 C 0.76225(15) 0.5204(3) 0.72414(14) 0.0319(6) Uani 1 1 d . . . . .
H1A H 0.7843 0.6111 0.7411 0.038 Uiso 1 1 calc R U . . .
H1B H 0.8004 0.4485 0.7330 0.038 Uiso 1 1 calc R U . . .
C2 C 0.59668(14) 0.3533(3) 0.71710(14) 0.0305(6) Uani 1 1 d . . . . .
H2A H 0.5854 0.3714 0.7579 0.037 Uiso 1 1 calc R U . . .
H2B H 0.5785 0.2587 0.7022 0.037 Uiso 1 1 calc R U . . .
C3 C 0.55709(14) 0.4605(3) 0.66749(13) 0.0282(6) Uani 1 1 d . . . . .
H3A H 0.5056 0.4358 0.6531 0.034 Uiso 1 1 calc R U . . .
H3B H 0.5614 0.5538 0.6881 0.034 Uiso 1 1 calc R U . . .
C4 C 0.55736(15) 0.2956(3) 0.44215(15) 0.0319(6) Uani 1 1 d . . . . .
H4A H 0.5408 0.3451 0.4005 0.038 Uiso 1 1 calc R U . . .
H4B H 0.5172 0.2370 0.4468 0.038 Uiso 1 1 calc R U . . .
C5 C 0.77581(15) 0.5920(3) 0.62217(15) 0.0340(6) Uani 1 1 d . . . . .
H5A H 0.8228 0.5438 0.6336 0.041 Uiso 1 1 calc R U . . .
H5B H 0.7837 0.6928 0.6324 0.041 Uiso 1 1 calc R U . . .
C6 C 0.70632(15) 0.4809(3) 0.75677(14) 0.0311(6) Uani 1 1 d . . . . .
H6A H 0.7291 0.4677 0.8033 0.037 Uiso 1 1 calc R U . . .
H6B H 0.6702 0.5565 0.7511 0.037 Uiso 1 1 calc R U . . .
C7 C 0.67675(14) 0.1505(3) 0.55166(16) 0.0358(7) Uani 1 1 d . . . . .
H7A H 0.6865 0.2515 0.5483 0.043 Uiso 1 1 calc R U . . .
H7B H 0.7233 0.1010 0.5658 0.043 Uiso 1 1 calc R U . . .
C8 C 0.63658(15) 0.1293(3) 0.60034(17) 0.0367(7) Uani 1 1 d . . . . .
H8A H 0.6306 0.0279 0.6068 0.044 Uiso 1 1 calc R U . . .
H8B H 0.6639 0.1704 0.6419 0.044 Uiso 1 1 calc R U . . .
C9 C 0.73702(15) 0.5714(4) 0.55283(15) 0.0379(7) Uani 1 1 d . . . . .
H9A H 0.7551 0.6375 0.5261 0.045 Uiso 1 1 calc R U . . .
H9B H 0.7440 0.4747 0.5394 0.045 Uiso 1 1 calc R U . . .
C10 C 0.50516(15) 0.1176(3) 0.57664(17) 0.0380(7) Uani 1 1 d . . . . .
H10A H 0.5049 0.0943 0.6209 0.046 Uiso 1 1 calc R U . . .
H10B H 0.5047 0.0290 0.5529 0.046 Uiso 1 1 calc R U . . .
C11 C 0.61959(18) 0.2016(3) 0.44141(16) 0.0392(7) Uani 1 1 d . . . . .
H11A H 0.6083 0.1534 0.3994 0.047 Uiso 1 1 calc R U . . .
H11B H 0.6624 0.2607 0.4453 0.047 Uiso 1 1 calc R U . . .
C12 C 0.44232(18) 0.2004(3) 0.5453(3) 0.0625(13) Uani 1 1 d . . . . .
H12A H 0.4185 0.1601 0.5025 0.075 Uiso 1 1 calc R U . . .
H12B H 0.4080 0.1975 0.5711 0.075 Uiso 1 1 calc R U . . .
Be1 Be 0.60422(17) 0.5501(4) 0.47971(16) 0.0237(6) Uani 1 1 d . . . . .
Be2 Be 0.54698(17) 0.3649(3) 0.55343(18) 0.0247(7) Uani 1 1 d . . . . .
Be3 Be 0.64393(19) 0.5840(4) 0.61321(18) 0.0300(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 Be1 2.049(3) . ?
Cl2 Be3 2.020(4) . ?
O1 C9 1.447(3) . ?
O1 Be3 1.610(4) . ?
O1 Be1 1.614(4) . ?
O2 C7 1.417(4) . ?
O2 C11 1.421(4) . ?
O3 C3 1.443(3) . ?
O3 Be3 1.604(4) . ?
O3 Be2 1.613(4) . ?
O4 C4 1.433(3) . ?
O4 Be2 1.596(4) . ?
O4 Be1 1.623(4) . ?
O5 C10 1.411(3) . ?
O5 C8 1.444(3) . ?
O5 Be2 1.715(4) . ?
O6 C12 1.415(3) . ?
O6 Be2 1.613(4) . ?
O6 Be1 1.613(4) 5_666 ?
O7 C1 1.441(3) . ?
O7 C5 1.443(3) . ?
O7 Be3 1.730(4) . ?
O8 C6 1.424(3) . ?
O8 C2 1.426(3) . ?
C1 C6 1.509(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.526(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C11 1.512(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C9 1.494(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.501(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C12 1.452(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
Be1 O6 1.613(4) 5_666 ?

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
C9 O1 Be3 111.6(2) . . ?
C9 O1 Be1 118.1(2) . . ?
Be3 O1 Be1 120.7(2) . . ?
C7 O2 C11 114.5(2) . . ?
C3 O3 Be3 117.5(2) . . ?
C3 O3 Be2 116.4(2) . . ?
Be3 O3 Be2 126.0(2) . . ?
C4 O4 Be2 116.3(2) . . ?
C4 O4 Be1 119.4(2) . . ?
Be2 O4 Be1 122.6(2) . . ?
C10 O5 C8 119.3(2) . . ?
C10 O5 Be2 111.8(2) . . ?
C8 O5 Be2 128.8(2) . . ?
C12 O6 Be2 113.9(2) . . ?
C12 O6 Be1 114.7(2) . 5_666 ?
Be2 O6 Be1 131.3(2) . 5_666 ?
C1 O7 C5 113.2(2) . . ?
C1 O7 Be3 130.5(2) . . ?
C5 O7 Be3 104.9(2) . . ?
C6 O8 C2 114.3(2) . . ?
O7 C1 C6 109.5(2) . . ?
O7 C1 H1A 109.8 . . ?
C6 C1 H1A 109.8 . . ?
O7 C1 H1B 109.8 . . ?
C6 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
O8 C2 C3 114.3(2) . . ?
O8 C2 H2A 108.7 . . ?
C3 C2 H2A 108.7 . . ?
O8 C2 H2B 108.7 . . ?
C3 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
O3 C3 C2 113.5(2) . . ?
O3 C3 H3A 108.9 . . ?
C2 C3 H3A 108.9 . . ?
O3 C3 H3B 108.9 . . ?
C2 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
O4 C4 C11 113.1(2) . . ?
O4 C4 H4A 109.0 . . ?
C11 C4 H4A 109.0 . . ?
O4 C4 H4B 109.0 . . ?
C11 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
O7 C5 C9 104.6(2) . . ?
O7 C5 H5A 110.8 . . ?
C9 C5 H5A 110.8 . . ?
O7 C5 H5B 110.8 . . ?
C9 C5 H5B 110.8 . . ?
H5A C5 H5B 108.9 . . ?
O8 C6 C1 108.8(2) . . ?
O8 C6 H6A 109.9 . . ?
C1 C6 H6A 109.9 . . ?
O8 C6 H6B 109.9 . . ?
C1 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
O2 C7 C8 110.7(3) . . ?
O2 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
O5 C8 C7 109.4(2) . . ?
O5 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
O5 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
O1 C9 C5 106.7(2) . . ?
O1 C9 H9A 110.4 . . ?
C5 C9 H9A 110.4 . . ?
O1 C9 H9B 110.4 . . ?
C5 C9 H9B 110.4 . . ?
H9A C9 H9B 108.6 . . ?
O5 C10 C12 108.9(2) . . ?
O5 C10 H10A 109.9 . . ?
C12 C10 H10A 109.9 . . ?
O5 C10 H10B 109.9 . . ?
C12 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
O2 C11 C4 114.5(3) . . ?
O2 C11 H11A 108.6 . . ?
C4 C11 H11A 108.6 . . ?
O2 C11 H11B 108.6 . . ?
C4 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
O6 C12 C10 110.6(3) . . ?
O6 C12 H12A 109.5 . . ?
C10 C12 H12A 109.5 . . ?
O6 C12 H12B 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
O6 Be1 O1 109.7(2) 5_666 . ?
O6 Be1 O4 109.2(2) 5_666 . ?
O1 Be1 O4 106.5(2) . . ?
O6 Be1 Cl1 107.25(18) 5_666 . ?
O1 Be1 Cl1 110.93(18) . . ?
O4 Be1 Cl1 113.16(19) . . ?
O4 Be2 O6 115.8(2) . . ?
O4 Be2 O3 111.0(2) . . ?
O6 Be2 O3 116.4(2) . . ?
O4 Be2 O5 109.7(2) . . ?
O6 Be2 O5 93.46(19) . . ?
O3 Be2 O5 108.9(2) . . ?
O3 Be3 O1 113.1(2) . . ?
O3 Be3 O7 113.3(2) . . ?
O1 Be3 O7 94.9(2) . . ?
O3 Be3 Cl2 113.9(2) . . ?
O1 Be3 Cl2 113.9(2) . . ?
O7 Be3 Cl2 106.1(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1A O8 0.99 2.49 3.474(4) 172.0 4_656
C3 H3A Cl1 0.99 2.91 3.869(3) 162.5 5_666
C3 H3A O6 0.99 2.56 3.108(3) 114.5 .
C3 H3B Cl2 0.99 2.67 3.316(3) 122.9 .
C6 H6B Cl2 0.99 2.92 3.637(3) 130.0 .
C7 H7A O4 0.99 2.57 3.105(3) 114.1 .
C7 H7B Cl1 0.99 2.79 3.779(3) 174.8 7_656
C8 H8A Cl2 0.99 2.65 3.627(3) 167.4 1_545
C8 H8B O8 0.99 2.56 3.440(4) 148.7 .
C11 H11B Cl1 0.99 2.90 3.512(3) 121.2 .
C12 H12B Cl1 0.99 2.75 3.325(4) 117.1 5_666

_refine_diff_density_max         0.693
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.075



_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_062_0m
_database_code_depnum_ccdc_archive 'CCDC 1866610'
_audit_update_record             
;
2018-09-09 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
_audit_creation_date             2017-06-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H40 Be6 Cl4 O14, 2(C6 H6)'
_chemical_formula_sum            'C48 H52 Be6 Cl4 O14'
_chemical_formula_weight         1048.75
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8872(5)
_cell_length_b                   12.0013(6)
_cell_length_c                   12.2122(6)
_cell_angle_alpha                108.235(2)
_cell_angle_beta                 103.883(2)
_cell_angle_gamma                106.623(2)
_cell_volume                     1229.35(11)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      24.91
_cell_measurement_theta_min      2.36
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9341
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0833 before and 0.0482 after correction. The Ratio of minimum to maximum transmission is 0.9341. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.086
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32034
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.909
_diffrn_reflns_theta_max         24.909
_diffrn_reflns_theta_min         2.306
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3716
_reflns_number_total             4297
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4297
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0402
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0414P)²+1.6165P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1004
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C17(H17A,H17B), C18(H18A,H18B), C1(H1A,H1B), C10(H10A,H10B),
 C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C7(H7), C12(H12), C4(H4), C6(H6), C13(H13), C21(H21), C14(H14),
 C5(H5), C24(H24), C20(H20), C22(H22), C19(H19), C23(H23)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl2 Cl 0.76564(6) 0.84228(5) 1.02112(5) 0.02080(15) Uani 1 1 d . . . . .
Cl1 Cl 0.13881(6) 0.49038(5) 0.73846(5) 0.02354(15) Uani 1 1 d . . . . .
O1 O 0.51439(16) 0.32475(13) 0.95849(13) 0.0136(3) Uani 1 1 d . . . . .
O3 O 0.64319(16) 0.55823(13) 0.95408(13) 0.0145(3) Uani 1 1 d . . . . .
O4 O 0.47794(16) 0.63369(13) 0.81596(13) 0.0150(3) Uani 1 1 d . . . . .
O7 O 0.38293(16) 0.38747(13) 0.77723(13) 0.0143(3) Uani 1 1 d . . . . .
O5 O 0.34975(17) 0.48182(14) 0.59732(13) 0.0180(3) Uani 1 1 d . . . . .
O6 O 0.37418(18) 0.25589(15) 0.54005(14) 0.0207(4) Uani 1 1 d . . . . .
O2 O 0.66399(17) 0.35730(15) 0.82176(14) 0.0187(3) Uani 1 1 d . . . . .
C16 C 0.2516(2) 0.3844(2) 0.48183(19) 0.0173(5) Uani 1 1 d . . . . .
C11 C 0.2630(3) 0.2670(2) 0.4565(2) 0.0182(5) Uani 1 1 d . . . . .
C8 C 0.6069(2) 0.2588(2) 0.9529(2) 0.0173(5) Uani 1 1 d . . . . .
C15 C 0.1493(3) 0.4023(2) 0.3965(2) 0.0202(5) Uani 1 1 d . . . . .
H15 H 0.1407 0.4824 0.4156 0.024 Uiso 1 1 calc R . . . .
C3 C 0.6944(3) 0.2782(2) 0.8817(2) 0.0194(5) Uani 1 1 d . . . . .
C9 C 0.2719(3) 0.2591(2) 0.7044(2) 0.0194(5) Uani 1 1 d . . . . .
H9A H 0.1745 0.2614 0.6623 0.023 Uiso 1 1 calc R . . . .
H9B H 0.2556 0.2152 0.7594 0.023 Uiso 1 1 calc R . . . .
C7 C 0.6199(3) 0.1791(2) 1.0120(2) 0.0213(5) Uani 1 1 d . . . . .
H7 H 0.5614 0.1647 1.0613 0.026 Uiso 1 1 calc R . . . .
C12 C 0.1715(3) 0.1666(2) 0.3427(2) 0.0228(5) Uani 1 1 d . . . . .
H12 H 0.1778 0.0857 0.3246 0.027 Uiso 1 1 calc R . . . .
C17 C 0.4011(3) 0.6138(2) 0.6102(2) 0.0215(5) Uani 1 1 d . . . . .
H17A H 0.3201 0.6466 0.6112 0.026 Uiso 1 1 calc R . . . .
H17B H 0.4363 0.6223 0.5427 0.026 Uiso 1 1 calc R . . . .
C4 C 0.7959(3) 0.2217(2) 0.8666(2) 0.0230(5) Uani 1 1 d . . . . .
H4 H 0.8547 0.2369 0.8177 0.028 Uiso 1 1 calc R . . . .
C18 C 0.5300(3) 0.6816(2) 0.7333(2) 0.0196(5) Uani 1 1 d . . . . .
H18A H 0.6200 0.6640 0.7254 0.023 Uiso 1 1 calc R . . . .
H18B H 0.5578 0.7748 0.7643 0.023 Uiso 1 1 calc R . . . .
C6 C 0.7208(3) 0.1206(2) 0.9973(2) 0.0240(5) Uani 1 1 d . . . . .
H6 H 0.7301 0.0650 1.0368 0.029 Uiso 1 1 calc R . . . .
C1 C 0.7971(2) 0.5697(2) 0.9733(2) 0.0224(5) Uani 1 1 d . . . . .
H1A H 0.8368 0.5493 1.0438 0.027 Uiso 1 1 calc R . . . .
H1B H 0.8630 0.6575 0.9906 0.027 Uiso 1 1 calc R . . . .
C13 C 0.0708(3) 0.1841(2) 0.2554(2) 0.0236(5) Uani 1 1 d . . . . .
H13 H 0.0096 0.1157 0.1770 0.028 Uiso 1 1 calc R . . . .
C10 C 0.3230(3) 0.1858(2) 0.6092(2) 0.0220(5) Uani 1 1 d . . . . .
H10A H 0.4064 0.1663 0.6512 0.026 Uiso 1 1 calc R . . . .
H10B H 0.2380 0.1039 0.5513 0.026 Uiso 1 1 calc R . . . .
C21 C 0.5882(3) 0.0564(2) 0.3090(2) 0.0299(6) Uani 1 1 d . . . . .
H21 H 0.5133 0.0056 0.2286 0.036 Uiso 1 1 calc R . . . .
C2 C 0.7920(3) 0.4760(2) 0.8555(2) 0.0263(5) Uani 1 1 d . . . . .
H2A H 0.7768 0.5075 0.7895 0.032 Uiso 1 1 calc R . . . .
H2B H 0.8876 0.4622 0.8684 0.032 Uiso 1 1 calc R . . . .
C14 C 0.0594(3) 0.3016(2) 0.2826(2) 0.0234(5) Uani 1 1 d . . . . .
H14 H -0.0104 0.3131 0.2229 0.028 Uiso 1 1 calc R . . . .
C5 C 0.8085(3) 0.1408(2) 0.9267(2) 0.0263(6) Uani 1 1 d . . . . .
H5 H 0.8770 0.0999 0.9190 0.032 Uiso 1 1 calc R . . . .
C24 C 0.8052(3) 0.2058(3) 0.5421(2) 0.0363(7) Uani 1 1 d . . . . .
H24 H 0.8800 0.2567 0.6226 0.044 Uiso 1 1 calc R . . . .
C20 C 0.5450(3) 0.0895(3) 0.4077(3) 0.0353(6) Uani 1 1 d . . . . .
H20 H 0.4408 0.0609 0.3972 0.042 Uiso 1 1 calc R . . . .
C22 C 0.7369(3) 0.0949(3) 0.3234(3) 0.0406(7) Uani 1 1 d . . . . .
H22 H 0.7659 0.0702 0.2536 0.049 Uiso 1 1 calc R . . . .
C19 C 0.6575(3) 0.1673(3) 0.5264(3) 0.0395(7) Uani 1 1 d . . . . .
H19 H 0.6284 0.1927 0.5960 0.047 Uiso 1 1 calc R . . . .
C23 C 0.8476(3) 0.1713(3) 0.4418(3) 0.0434(8) Uani 1 1 d . . . . .
H23 H 0.9518 0.1991 0.4524 0.052 Uiso 1 1 calc R . . . .
Be2 Be 0.5908(3) 0.6748(3) 0.9551(3) 0.0150(6) Uani 1 1 d . . . . .
Be3 Be 0.3432(3) 0.4958(3) 0.7438(3) 0.0161(6) Uani 1 1 d . . . . .
Be1 Be 0.5326(3) 0.4117(3) 0.8797(3) 0.0160(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl2 Be2 2.001(3) . ?
Cl1 Be3 1.988(3) . ?
O1 C8 1.370(3) . ?
O1 Be2 1.650(3) 2_667 ?
O1 Be1 1.629(3) . ?
O3 C1 1.442(3) . ?
O3 Be2 1.622(3) . ?
O3 Be1 1.593(3) . ?
O4 C18 1.435(3) . ?
O4 Be2 1.621(3) . ?
O4 Be3 1.598(3) . ?
O7 C9 1.441(3) . ?
O7 Be3 1.599(3) . ?
O7 Be1 1.574(3) . ?
O5 C16 1.400(3) . ?
O5 C17 1.462(3) . ?
O5 Be3 1.763(3) . ?
O6 C11 1.378(3) . ?
O6 C10 1.443(3) . ?
O2 C3 1.421(3) . ?
O2 C2 1.467(3) . ?
O2 Be1 1.803(3) . ?
C16 C11 1.388(3) . ?
C16 C15 1.383(3) . ?
C11 C12 1.388(3) . ?
C8 C3 1.390(3) . ?
C8 C7 1.382(3) . ?
C15 H15 0.9500 . ?
C15 C14 1.388(3) . ?
C3 C4 1.378(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.509(3) . ?
C7 H7 0.9500 . ?
C7 C6 1.388(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.387(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.506(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.402(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C6 H6 0.9500 . ?
C6 C5 1.387(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.502(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.388(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C21 H21 0.9500 . ?
C21 C20 1.355(4) . ?
C21 C22 1.358(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C14 H14 0.9500 . ?
C5 H5 0.9500 . ?
C24 H24 0.9500 . ?
C24 C19 1.345(4) . ?
C24 C23 1.370(4) . ?
C20 H20 0.9500 . ?
C20 C19 1.413(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.402(4) . ?
C19 H19 0.9500 . ?
C23 H23 0.9500 . ?
Be2 O1 1.650(3) 2_667 ?

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
C8 O1 Be2 123.63(16) . 2_667 ?
C8 O1 Be1 111.81(17) . . ?
Be1 O1 Be2 124.35(16) . 2_667 ?
C1 O3 Be2 122.58(17) . . ?
C1 O3 Be1 109.03(16) . . ?
Be1 O3 Be2 123.70(17) . . ?
C18 O4 Be2 121.14(17) . . ?
C18 O4 Be3 112.12(16) . . ?
Be3 O4 Be2 119.86(16) . . ?
C9 O7 Be3 115.72(16) . . ?
C9 O7 Be1 119.37(16) . . ?
Be1 O7 Be3 124.90(17) . . ?
C16 O5 C17 119.00(16) . . ?
C16 O5 Be3 127.68(16) . . ?
C17 O5 Be3 103.27(15) . . ?
C11 O6 C10 115.90(17) . . ?
C3 O2 C2 115.72(17) . . ?
C3 O2 Be1 105.02(16) . . ?
C2 O2 Be1 103.48(16) . . ?
C11 C16 O5 116.00(18) . . ?
C15 C16 O5 122.8(2) . . ?
C15 C16 C11 121.2(2) . . ?
O6 C11 C16 119.24(19) . . ?
O6 C11 C12 121.3(2) . . ?
C12 C11 C16 119.2(2) . . ?
O1 C8 C3 114.75(19) . . ?
O1 C8 C7 125.8(2) . . ?
C7 C8 C3 119.5(2) . . ?
C16 C15 H15 120.4 . . ?
C16 C15 C14 119.1(2) . . ?
C14 C15 H15 120.5 . . ?
C8 C3 O2 113.33(19) . . ?
C4 C3 O2 123.4(2) . . ?
C4 C3 C8 123.2(2) . . ?
O7 C9 H9A 109.4 . . ?
O7 C9 H9B 109.4 . . ?
O7 C9 C10 110.95(19) . . ?
H9A C9 H9B 108.0 . . ?
C10 C9 H9A 109.4 . . ?
C10 C9 H9B 109.4 . . ?
C8 C7 H7 120.9 . . ?
C8 C7 C6 118.2(2) . . ?
C6 C7 H7 120.9 . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.1(2) . . ?
C13 C12 H12 119.9 . . ?
O5 C17 H17A 111.4 . . ?
O5 C17 H17B 111.4 . . ?
O5 C17 C18 102.05(17) . . ?
H17A C17 H17B 109.2 . . ?
C18 C17 H17A 111.4 . . ?
C18 C17 H17B 111.4 . . ?
C3 C4 H4 121.5 . . ?
C3 C4 C5 117.0(2) . . ?
C5 C4 H4 121.5 . . ?
O4 C18 C17 106.50(18) . . ?
O4 C18 H18A 110.4 . . ?
O4 C18 H18B 110.4 . . ?
C17 C18 H18A 110.4 . . ?
C17 C18 H18B 110.4 . . ?
H18A C18 H18B 108.6 . . ?
C7 C6 H6 119.0 . . ?
C5 C6 C7 122.1(2) . . ?
C5 C6 H6 119.0 . . ?
O3 C1 H1A 110.5 . . ?
O3 C1 H1B 110.5 . . ?
O3 C1 C2 105.97(18) . . ?
H1A C1 H1B 108.7 . . ?
C2 C1 H1A 110.5 . . ?
C2 C1 H1B 110.5 . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.0(2) . . ?
C14 C13 H13 120.0 . . ?
O6 C10 C9 112.12(18) . . ?
O6 C10 H10A 109.2 . . ?
O6 C10 H10B 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C20 C21 H21 119.5 . . ?
C20 C21 C22 121.0(2) . . ?
C22 C21 H21 119.5 . . ?
O2 C2 C1 105.86(18) . . ?
O2 C2 H2A 110.6 . . ?
O2 C2 H2B 110.6 . . ?
C1 C2 H2A 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
C15 C14 C13 120.4(2) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0(2) . . ?
C6 C5 H5 120.0 . . ?
C19 C24 H24 120.1 . . ?
C19 C24 C23 119.8(3) . . ?
C23 C24 H24 120.1 . . ?
C21 C20 H20 120.5 . . ?
C21 C20 C19 118.9(3) . . ?
C19 C20 H20 120.5 . . ?
C21 C22 H22 120.2 . . ?
C21 C22 C23 119.6(3) . . ?
C23 C22 H22 120.2 . . ?
C24 C19 C20 120.7(3) . . ?
C24 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C24 C23 C22 120.0(3) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
O1 Be2 Cl2 112.10(15) 2_667 . ?
O3 Be2 Cl2 112.98(16) . . ?
O3 Be2 O1 104.00(17) . 2_667 ?
O4 Be2 Cl2 113.47(16) . . ?
O4 Be2 O1 106.40(17) . 2_667 ?
O4 Be2 O3 107.21(17) . . ?
O4 Be3 Cl1 115.67(16) . . ?
O4 Be3 O7 113.67(18) . . ?
O4 Be3 O5 94.14(16) . . ?
O7 Be3 Cl1 114.03(17) . . ?
O7 Be3 O5 110.51(17) . . ?
O5 Be3 Cl1 106.66(14) . . ?
O1 Be1 O2 94.77(15) . . ?
O3 Be1 O1 117.23(18) . . ?
O3 Be1 O2 96.85(16) . . ?
O7 Be1 O1 116.01(19) . . ?
O7 Be1 O3 113.73(18) . . ?
O7 Be1 O2 114.94(17) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
