# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_2016312_0m
_database_code_depnum_ccdc_archive 'CCDC 1550846'
_audit_update_record             
;
2017-05-18 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;
_audit_creation_date             2016-06-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.25(Be12 H16 O48 P16), 2(C3 H5 N2)'
_chemical_formula_sum            'C6 H14 Be3 N4 O12 P4'
_chemical_formula_weight         485.12
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
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                   9.4886(7)
_cell_length_b                   13.8218(10)
_cell_length_c                   13.2987(10)
_cell_angle_alpha                90
_cell_angle_beta                 100.092(4)
_cell_angle_gamma                90
_cell_volume                     1717.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3854
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      2.63
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0517 before and 0.0448 after correction.
The Ratio of minimum to maximum transmission is 0.8861.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7665
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.688
_diffrn_reflns_theta_min         2.632
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1768
_reflns_number_total             1999
_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 v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1999
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0405
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0311P)²+7.4198P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.0993
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N2-H2A
 0.88 with sigma of 0.02
3. Restrained planarity
 C1, C2, C3, N1, N2
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1B), C2(H2B), C3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_special_details      
;
The structure was solved using Direct Methods (ShelXS). RE = 0.4, Nqual =  -1, Ralpha = 0.086
;
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
Be1 Be 0.4506(3) 0.4083(2) 0.6047(2) 0.0178(6) Uani 1 1 d . U . . .
Be2 Be 1.0000 0.2681(3) 0.7500 0.0154(8) Uani 1 2 d S TU P . .
O1 O 0.4998(2) 0.29909(14) 0.35095(14) 0.0270(4) Uani 1 1 d . U . . .
O2 O 0.5458(2) 0.47472(13) 0.38355(15) 0.0267(4) Uani 1 1 d . U . . .
O3 O 0.39330(19) 0.37902(14) 0.48610(13) 0.0244(4) Uani 1 1 d . U . . .
O4 O 0.6081(2) 0.36277(15) 0.64200(14) 0.0281(4) Uani 1 1 d . U . . .
O5 O 0.6745(2) 0.37383(16) 0.83401(14) 0.0301(5) Uani 1 1 d . U . . .
O6 O 0.85974(18) 0.33722(13) 0.72807(14) 0.0227(4) Uani 1 1 d . U . . .
P1 P 0.44029(7) 0.39352(5) 0.38458(5) 0.01661(16) Uani 1 1 d . U . . .
H1 H 0.325(3) 0.4172(18) 0.3142(18) 0.007(6) Uiso 1 1 d . . . . .
P2 P 0.70385(6) 0.32699(4) 0.73723(5) 0.01574(16) Uani 1 1 d . U . . .
H2 H 0.676(3) 0.236(2) 0.742(2) 0.016(7) Uiso 1 1 d . . . . .
C1 C 0.4497(4) 0.1248(3) 0.5615(3) 0.0506(10) Uani 1 1 d . U . . .
H1B H 0.3555 0.1440 0.5602 0.061 Uiso 1 1 calc R . . . .
C2 C 0.6640(4) 0.1149(3) 0.5310(3) 0.0533(10) Uani 1 1 d . U . . .
H2B H 0.7455 0.1265 0.5030 0.064 Uiso 1 1 calc R . . . .
C3 C 0.6538(3) 0.0525(3) 0.5968(2) 0.0370(8) Uani 1 1 d . U . . .
H3 H 0.7273 0.0115 0.6261 0.044 Uiso 1 1 calc R . . . .
N1 N 0.5437(4) 0.1616(2) 0.5072(2) 0.0444(7) Uani 1 1 d . U . . .
H1A H 0.532(5) 0.210(4) 0.461(4) 0.080(15) Uiso 1 1 d . . . . .
N2 N 0.5226(5) 0.0529(3) 0.6191(3) 0.0726(11) Uani 1 1 d D U . . .
H2A H 0.484(5) 0.011(3) 0.663(3) 0.078(15) Uiso 1 1 d 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
Be1 O2 1.625(4) 5_666 ?
Be1 O3 1.627(3) . ?
Be1 O4 1.617(4) . ?
Be1 O5 1.625(4) 2_656 ?
Be2 O1 1.632(3) 7_656 ?
Be2 O1 1.632(3) 8_556 ?
Be2 O6 1.623(3) . ?
Be2 O6 1.623(3) 2_756 ?
O1 Be2 1.632(3) 7_656 ?
O1 P1 1.5202(19) . ?
O2 Be1 1.625(4) 5_666 ?
O2 P1 1.5058(19) . ?
O3 P1 1.5076(18) . ?
O4 P2 1.5068(19) . ?
O5 Be1 1.625(4) 2_656 ?
O5 P2 1.5097(19) . ?
O6 P2 1.5120(18) . ?
P1 H1 1.35(2) . ?
P2 H2 1.28(3) . ?
C1 H1B 0.9300 . ?
C1 N1 1.342(5) . ?
C1 N2 1.365(6) . ?
C2 H2B 0.9300 . ?
C2 C3 1.244(5) . ?
C2 N1 1.301(5) . ?
C3 H3 0.9300 . ?
C3 N2 1.330(5) . ?
N1 H1A 0.90(5) . ?
N2 H2A 0.942(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Be1 O3 109.8(2) 5_666 . ?
O2 Be1 O5 104.4(2) 5_666 2_656 ?
O4 Be1 O2 110.8(2) . 5_666 ?
O4 Be1 O3 109.6(2) . . ?
O4 Be1 O5 116.7(2) . 2_656 ?
O5 Be1 O3 105.3(2) 2_656 . ?
O1 Be2 O1 110.7(3) 7_656 8_556 ?
O6 Be2 O1 107.83(10) . 7_656 ?
O6 Be2 O1 107.83(10) 2_756 8_556 ?
O6 Be2 O1 111.32(10) 2_756 7_656 ?
O6 Be2 O1 111.32(10) . 8_556 ?
O6 Be2 O6 107.8(3) 2_756 . ?
P1 O1 Be2 141.64(17) . 7_656 ?
P1 O2 Be1 138.04(17) . 5_666 ?
P1 O3 Be1 137.23(17) . . ?
P2 O4 Be1 140.72(17) . . ?
P2 O5 Be1 144.46(18) . 2_656 ?
P2 O6 Be2 135.52(17) . . ?
O1 P1 H1 107.6(10) . . ?
O2 P1 O1 110.82(11) . . ?
O2 P1 O3 114.12(11) . . ?
O2 P1 H1 105.8(10) . . ?
O3 P1 O1 109.44(11) . . ?
O3 P1 H1 108.8(10) . . ?
O4 P2 O5 113.68(11) . . ?
O4 P2 O6 110.84(11) . . ?
O4 P2 H2 105.4(12) . . ?
O5 P2 O6 110.98(11) . . ?
O5 P2 H2 107.7(12) . . ?
O6 P2 H2 107.9(12) . . ?
N1 C1 H1B 127.5 . . ?
N1 C1 N2 105.0(3) . . ?
N2 C1 H1B 127.5 . . ?
C3 C2 H2B 125.0 . . ?
C3 C2 N1 110.0(3) . . ?
N1 C2 H2B 125.0 . . ?
C2 C3 H3 124.9 . . ?
C2 C3 N2 110.2(3) . . ?
N2 C3 H3 124.9 . . ?
C1 N1 H1A 129(3) . . ?
C2 N1 C1 108.6(3) . . ?
C2 N1 H1A 122(3) . . ?
C1 N2 H2A 125(3) . . ?
C3 N2 C1 106.2(3) . . ?
C3 N2 H2A 128(3) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_2016313_0m
_database_code_depnum_ccdc_archive 'CCDC 1550847'
_audit_update_record             
;
2017-05-18 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;
_audit_creation_date             2016-06-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Be3 H4 O12 P4, 2(C3 H5 N2)'
_chemical_formula_sum            'C6 H14 Be3 N4 O12 P4'
_chemical_formula_weight         485.12
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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                   8.3233(5)
_cell_length_b                   8.4561(6)
_cell_length_c                   13.3101(8)
_cell_angle_alpha                96.149(3)
_cell_angle_beta                 95.184(3)
_cell_angle_gamma                111.344(3)
_cell_volume                     859.02(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.65
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0485 before and 0.0368 after correction.
The Ratio of minimum to maximum transmission is 0.9124.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14302
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.587
_diffrn_reflns_theta_min         1.554
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3792
_reflns_number_total             3943
_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 v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3943
_refine_ls_number_restraints     81
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0583
_refine_ls_restrained_S_all      1.140
_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)+(0.0352P)²+3.9593P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1412
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H,H) groups, All C(H) groups, All N(H) groups
2. Restrained distances
 P1-H1
 1.3 with sigma of 0.02
3. Restrained planarity
 C4, C5, C6, N3, N4
 with sigma of 0.1
 C1, C2, C3, N1, N2
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C4(H4A), C5(H5), C6(H6), N3(H3B), N4(H4B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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
Be1 Be 0.4550(6) 0.6331(6) 0.3909(3) 0.0195(8) Uani 1 1 d . U . . .
Be2 Be -0.2400(6) 0.2257(5) 0.2482(3) 0.0177(8) Uani 1 1 d . U . . .
Be3 Be 0.3534(6) 0.5411(6) 0.1008(3) 0.0197(8) Uani 1 1 d . U . . .
O1 O 0.3056(4) 0.7114(4) 0.6487(2) 0.0293(6) Uani 1 1 d . U . . .
O2 O 0.4325(4) 0.4871(4) 0.6207(2) 0.0304(6) Uani 1 1 d . U . . .
O3 O 0.4840(4) 0.7210(4) 0.5095(2) 0.0285(6) Uani 1 1 d . U . . .
O4 O 0.2528(3) 0.5264(4) 0.3529(2) 0.0328(6) Uani 1 1 d . U . . .
O5 O -0.0280(3) 0.3024(3) 0.2672(2) 0.0275(6) Uani 1 1 d . U . . .
O6 O 0.1895(4) 0.4589(4) 0.1604(2) 0.0392(8) Uani 1 1 d . U . . .
O7 O 0.5519(4) 0.7926(4) 0.3308(2) 0.0318(6) Uani 1 1 d . U . . .
O8 O 0.6954(3) 1.0184(3) 0.2268(2) 0.0235(5) Uani 1 1 d . U . . .
O9 O 0.4731(4) 0.7397(3) 0.1386(2) 0.0323(6) Uani 1 1 d . U . . .
O10 O 0.2706(3) 0.5187(4) -0.0184(2) 0.0276(6) Uani 1 1 d . U . . .
O11 O 0.5342(4) 0.5809(3) -0.1105(2) 0.0284(6) Uani 1 1 d . U . . .
O12 O 0.3177(4) 0.7137(4) -0.1495(2) 0.0331(6) Uani 1 1 d . U . . .
P1 P 0.45729(11) 0.67120(11) 0.61347(6) 0.0184(2) Uani 1 1 d D U . . .
P2 P 0.53098(11) 0.86951(11) 0.23534(7) 0.0175(2) Uani 1 1 d . U . . .
H2 H 0.395(5) 0.926(5) 0.241(3) 0.007(8) Uiso 1 1 d . . . . .
P3 P 0.11697(11) 0.46988(11) 0.25927(7) 0.0187(2) Uani 1 1 d . U . . .
H3 H 0.049(6) 0.588(6) 0.256(3) 0.027(11) Uiso 1 1 d . . . . .
H1 H 0.601(4) 0.771(5) 0.676(3) 0.032 Uiso 1 1 d DR . . . .
H4 H 0.246(6) 0.410(6) -0.197(4) 0.032 Uiso 1 1 d R . . . .
P4 P 0.34470(12) 0.55706(11) -0.11667(6) 0.0195(2) Uani 1 1 d . U . . .
C1 C 0.1772(6) 0.9195(7) 0.4399(4) 0.0489(12) Uani 1 1 d . U . . .
H1A H 0.2932 0.9903 0.4413 0.059 Uiso 1 1 calc R . . . .
C2 C 0.0383(8) 0.9240(7) 0.3810(4) 0.0507(12) Uani 1 1 d . U . . .
H2A H 0.0393 0.9995 0.3349 0.061 Uiso 1 1 calc R . . . .
C3 C -0.0532(7) 0.7201(7) 0.4736(4) 0.0504(12) Uani 1 1 d . U . . .
H3A H -0.1260 0.6301 0.5026 0.060 Uiso 1 1 calc R . . . .
N1 N 0.1156(5) 0.7933(5) 0.4959(3) 0.0407(9) Uani 1 1 d . U . . .
H1B H 0.177(8) 0.771(8) 0.539(5) 0.052(17) Uiso 1 1 d . . . . .
N2 N -0.1020(6) 0.7967(7) 0.4028(3) 0.0508(11) Uani 1 1 d . U . . .
H2B H -0.208(10) 0.768(10) 0.373(6) 0.09(3) Uiso 1 1 d . . . . .
C4 C 0.9266(10) 1.0182(12) -0.1216(4) 0.076(2) Uani 1 1 d . U . . .
H4A H 0.9997 0.9993 -0.1662 0.091 Uiso 1 1 calc R . . . .
C5 C 0.8036(9) 1.1258(9) -0.0137(4) 0.0603(16) Uani 1 1 d . U . . .
H5 H 0.7710 1.1984 0.0302 0.072 Uiso 1 1 calc R . . . .
C6 C 0.7278(9) 0.9711(12) -0.0305(6) 0.0775(19) Uani 1 1 d . U . . .
H6 H 0.6348 0.9098 0.0017 0.093 Uiso 1 1 calc R . . . .
N3 N 0.7875(8) 0.9089(6) -0.0928(4) 0.0685(16) Uani 1 1 d . U . . .
H3B H 0.7439 0.8013 -0.1172 0.082 Uiso 1 1 calc R . . . .
N4 N 0.9342(9) 1.1789(8) -0.0634(5) 0.0897(19) Uani 1 1 d . U . . .
H4B H 1.0070 1.2819 -0.0627 0.108 Uiso 1 1 calc R . . . .


_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
Be1 O2 1.619(5) 2_666 ?
Be1 O3 1.628(5) . ?
Be1 O4 1.595(5) . ?
Be1 O7 1.633(5) . ?
Be2 O1 1.630(5) 2_566 ?
Be2 O5 1.627(5) . ?
Be2 O8 1.619(5) 1_445 ?
Be2 O12 1.624(5) 2_565 ?
Be3 O6 1.610(5) . ?
Be3 O9 1.605(5) . ?
Be3 O10 1.634(5) . ?
Be3 O11 1.632(5) 2_665 ?
O1 Be2 1.630(5) 2_566 ?
O1 P1 1.521(3) . ?
O2 Be1 1.619(5) 2_666 ?
O2 P1 1.509(3) . ?
O3 P1 1.502(3) . ?
O4 P3 1.511(3) . ?
O5 P3 1.511(3) . ?
O6 P3 1.505(3) . ?
O7 P2 1.512(3) . ?
O8 Be2 1.619(5) 1_665 ?
O8 P2 1.509(3) . ?
O9 P2 1.515(3) . ?
O10 P4 1.513(3) . ?
O11 Be3 1.632(5) 2_665 ?
O11 P4 1.509(3) . ?
O12 Be2 1.624(5) 2_565 ?
O12 P4 1.523(3) . ?
P1 H1 1.334(19) . ?
P2 H2 1.39(4) . ?
P3 H3 1.32(4) . ?
P4 H4 1.48(5) . ?
C1 H1A 0.9300 . ?
C1 C2 1.351(8) . ?
C1 N1 1.341(7) . ?
C2 H2A 0.9300 . ?
C2 N2 1.349(7) . ?
C3 H3A 0.9300 . ?
C3 N1 1.303(7) . ?
C3 N2 1.314(7) . ?
N1 H1B 0.82(6) . ?
N2 H2B 0.87(8) . ?
C4 H4A 0.9300 . ?
C4 N3 1.311(9) . ?
C4 N4 1.467(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.213(10) . ?
C5 N4 1.288(9) . ?
C6 H6 0.9300 . ?
C6 N3 1.176(10) . ?
N3 H3B 0.8600 . ?
N4 H4B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Be1 O3 109.6(3) 2_666 . ?
O2 Be1 O7 104.0(3) 2_666 . ?
O3 Be1 O7 104.5(3) . . ?
O4 Be1 O2 111.5(3) . 2_666 ?
O4 Be1 O3 110.2(3) . . ?
O4 Be1 O7 116.6(3) . . ?
O5 Be2 O1 107.6(3) . 2_566 ?
O8 Be2 O1 111.0(3) 1_445 2_566 ?
O8 Be2 O5 107.2(3) 1_445 . ?
O8 Be2 O12 107.7(3) 1_445 2_565 ?
O12 Be2 O1 110.7(3) 2_565 2_566 ?
O12 Be2 O5 112.6(3) 2_565 . ?
O6 Be3 O10 105.5(3) . . ?
O6 Be3 O11 105.1(3) . 2_665 ?
O9 Be3 O6 116.6(3) . . ?
O9 Be3 O10 108.7(3) . . ?
O9 Be3 O11 111.4(3) . 2_665 ?
O11 Be3 O10 109.2(3) 2_665 . ?
P1 O1 Be2 141.1(2) . 2_566 ?
P1 O2 Be1 137.6(3) . 2_666 ?
P1 O3 Be1 140.2(2) . . ?
P3 O4 Be1 142.5(3) . . ?
P3 O5 Be2 136.5(2) . . ?
P3 O6 Be3 145.2(3) . . ?
P2 O7 Be1 142.8(3) . . ?
P2 O8 Be2 135.6(2) . 1_665 ?
P2 O9 Be3 139.5(3) . . ?
P4 O10 Be3 135.0(2) . . ?
P4 O11 Be3 136.4(2) . 2_665 ?
P4 O12 Be2 140.6(3) . 2_565 ?
O1 P1 H1 108(2) . . ?
O2 P1 O1 110.90(17) . . ?
O2 P1 H1 108(2) . . ?
O3 P1 O1 109.39(16) . . ?
O3 P1 O2 114.52(16) . . ?
O3 P1 H1 106(2) . . ?
O7 P2 O9 113.53(17) . . ?
O7 P2 H2 107.8(15) . . ?
O8 P2 O7 110.96(15) . . ?
O8 P2 O9 110.81(16) . . ?
O8 P2 H2 109.6(15) . . ?
O9 P2 H2 103.8(15) . . ?
O4 P3 H3 107.6(19) . . ?
O5 P3 O4 110.75(16) . . ?
O5 P3 H3 107.6(19) . . ?
O6 P3 O4 113.94(17) . . ?
O6 P3 O5 110.95(17) . . ?
O6 P3 H3 105.6(19) . . ?
O10 P4 O12 110.08(17) . . ?
O10 P4 H4 108.2(18) . . ?
O11 P4 O10 113.37(16) . . ?
O11 P4 O12 110.54(17) . . ?
O11 P4 H4 107.2(18) . . ?
O12 P4 H4 107.1(18) . . ?
C2 C1 H1A 126.6 . . ?
N1 C1 H1A 126.6 . . ?
N1 C1 C2 106.9(4) . . ?
C1 C2 H2A 127.0 . . ?
N2 C2 C1 106.0(5) . . ?
N2 C2 H2A 127.0 . . ?
N1 C3 H3A 126.2 . . ?
N1 C3 N2 107.6(5) . . ?
N2 C3 H3A 126.2 . . ?
C1 N1 H1B 124(4) . . ?
C3 N1 C1 109.9(4) . . ?
C3 N1 H1B 127(4) . . ?
C2 N2 H2B 125(5) . . ?
C3 N2 C2 109.7(4) . . ?
C3 N2 H2B 126(5) . . ?
N3 C4 H4A 129.9 . . ?
N3 C4 N4 100.1(5) . . ?
N4 C4 H4A 129.9 . . ?
C6 C5 H5 123.7 . . ?
C6 C5 N4 112.7(6) . . ?
N4 C5 H5 123.7 . . ?
C5 C6 H6 124.6 . . ?
N3 C6 C5 110.9(7) . . ?
N3 C6 H6 124.6 . . ?
C4 N3 H3B 123.0 . . ?
C6 N3 C4 114.0(6) . . ?
C6 N3 H3B 123.0 . . ?
C4 N4 H4B 129.0 . . ?
C5 N4 C4 102.1(5) . . ?
C5 N4 H4B 129.0 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
