# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2011


data_global

_journal_coden_Cambridge         1350

loop_
_publ_author_name
'Luo, Xiuchao'
'Luo, Daibing'
'Gong, Maochu'
'Chen, Yaoqiang'
'Lin, Zhien'

_publ_contact_author_name        'Lin, Zhien'
_publ_contact_author_email       zhienlin@scu.edu.cn

_publ_section_title              
;
(C2H8N)2[Be3(HPO3)4]: A low-density beryllium phosphite with
large 16-membered rings and helical channels
;

# Attachment '- 1.CIF'

data_1
_database_code_depnum_ccdc_archive 'CCDC 809522'
#TrackingRef '- 1.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H20 Be3 N2 O12 P4'
_chemical_formula_weight         439.13

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_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                   14.6905(8)
_cell_length_b                   8.0472(4)
_cell_length_c                   15.8688(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.929(7)
_cell_angle_gamma                90.00
_cell_volume                     1727.74(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9541
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3194
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1517
_reflns_number_gt                1311
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+5.2465P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1517
_refine_ls_number_parameters     122
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.0939
_refine_ls_wR_factor_gt          0.0896
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.107
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.51646(5) 0.39359(10) 0.39624(5) 0.0185(2) Uani 1 1 d . . .
H1 H 0.543(2) 0.269(4) 0.3544(18) 0.020(8) Uiso 1 1 d . . .
P2 P 0.35225(6) 0.15057(11) 0.62141(5) 0.0224(2) Uani 1 1 d . . .
H2 H 0.409(2) 0.006(4) 0.6484(19) 0.022(8) Uiso 1 1 d . . .
Be1 Be 0.3616(3) 0.3681(5) 0.4714(2) 0.0225(9) Uani 1 1 d . . .
Be2 Be 0.5000 0.6341(7) 0.2500 0.0215(12) Uani 1 2 d S . .
O1 O 0.60778(15) 0.4498(3) 0.47698(14) 0.0279(5) Uani 1 1 d . . .
O2 O 0.43775(16) 0.3215(3) 0.42348(14) 0.0314(6) Uani 1 1 d . . .
O3 O 0.47610(16) 0.5266(3) 0.32434(14) 0.0320(6) Uani 1 1 d . . .
O4 O 0.24836(15) 0.1064(3) 0.60813(13) 0.0331(6) Uani 1 1 d . . .
O5 O 0.40071(16) 0.2532(3) 0.70613(13) 0.0351(6) Uani 1 1 d . . .
O6 O 0.36486(15) 0.2190(3) 0.53872(13) 0.0254(5) Uani 1 1 d . . .
N1 N 0.1661(2) -0.2626(4) 0.64142(18) 0.0316(7) Uani 1 1 d . . .
H1D H 0.1419 -0.2177 0.6803 0.038 Uiso 1 1 calc R . .
H1E H 0.1577 -0.1881 0.5967 0.038 Uiso 1 1 calc R . .
C1 C 0.2722(3) -0.2929(6) 0.6907(3) 0.0535(12) Uani 1 1 d . . .
H1A H 0.3048 -0.1904 0.7160 0.080 Uiso 1 1 calc R . .
H1B H 0.2993 -0.3373 0.6493 0.080 Uiso 1 1 calc R . .
H1C H 0.2820 -0.3711 0.7392 0.080 Uiso 1 1 calc R . .
C2 C 0.1099(3) -0.4122(5) 0.6012(3) 0.0516(11) Uani 1 1 d . . .
H2A H 0.0414 -0.3842 0.5697 0.077 Uiso 1 1 calc R . .
H2B H 0.1169 -0.4911 0.6487 0.077 Uiso 1 1 calc R . .
H2C H 0.1345 -0.4598 0.5587 0.077 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0182(4) 0.0213(4) 0.0184(4) -0.0025(3) 0.0097(3) -0.0039(3)
P2 0.0198(4) 0.0297(5) 0.0170(4) 0.0015(3) 0.0064(3) -0.0060(4)
Be1 0.0184(19) 0.032(2) 0.0167(17) 0.0032(17) 0.0059(15) -0.0086(18)
Be2 0.019(3) 0.031(3) 0.013(2) 0.000 0.004(2) 0.000
O1 0.0232(11) 0.0270(12) 0.0271(11) 0.0001(10) 0.0030(9) -0.0039(10)
O2 0.0292(12) 0.0398(14) 0.0319(12) -0.0024(11) 0.0194(10) -0.0133(11)
O3 0.0275(12) 0.0389(14) 0.0258(11) 0.0076(10) 0.0064(9) -0.0085(11)
O4 0.0213(12) 0.0552(16) 0.0187(10) 0.0087(11) 0.0034(9) -0.0141(11)
O5 0.0327(13) 0.0547(16) 0.0181(10) -0.0060(11) 0.0100(9) -0.0227(12)
O6 0.0286(11) 0.0296(13) 0.0204(10) 0.0013(9) 0.0123(9) -0.0066(10)
N1 0.0361(16) 0.0339(16) 0.0305(14) 0.0047(13) 0.0191(12) 0.0101(14)
C1 0.031(2) 0.071(3) 0.055(2) 0.014(2) 0.0136(18) -0.001(2)
C2 0.047(2) 0.051(3) 0.048(2) -0.011(2) 0.0082(19) -0.005(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O2 1.500(2) . ?
P1 O3 1.507(2) . ?
P1 O1 1.519(2) . ?
P1 H1 1.34(3) . ?
P2 O6 1.499(2) . ?
P2 O4 1.500(2) . ?
P2 O5 1.500(2) . ?
P2 H2 1.40(3) . ?
Be1 O6 1.596(4) . ?
Be1 O2 1.622(4) . ?
Be1 O4 1.629(4) 7_556 ?
Be1 O1 1.654(5) 5_666 ?
Be2 O3 1.608(4) 2_655 ?
Be2 O3 1.608(4) . ?
Be2 O5 1.626(4) 5_666 ?
Be2 O5 1.626(4) 6_565 ?
O1 Be1 1.654(5) 5_666 ?
O4 Be1 1.629(4) 7_556 ?
O5 Be2 1.626(4) 5_666 ?
N1 C2 1.459(5) . ?
N1 C1 1.467(4) . ?
N1 H1D 0.9000 . ?
N1 H1E 0.9000 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?

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 P1 O3 111.88(13) . . ?
O2 P1 O1 113.51(12) . . ?
O3 P1 O1 112.64(13) . . ?
O2 P1 H1 104.8(12) . . ?
O3 P1 H1 105.1(12) . . ?
O1 P1 H1 108.2(12) . . ?
O6 P2 O4 115.47(12) . . ?
O6 P2 O5 113.88(13) . . ?
O4 P2 O5 110.98(13) . . ?
O6 P2 H2 108.0(11) . . ?
O4 P2 H2 107.5(12) . . ?
O5 P2 H2 99.5(11) . . ?
O6 Be1 O2 107.1(3) . . ?
O6 Be1 O4 112.0(2) . 7_556 ?
O2 Be1 O4 108.8(2) . 7_556 ?
O6 Be1 O1 113.8(2) . 5_666 ?
O2 Be1 O1 109.5(2) . 5_666 ?
O4 Be1 O1 105.6(3) 7_556 5_666 ?
O3 Be2 O3 114.9(4) 2_655 . ?
O3 Be2 O5 101.43(11) 2_655 5_666 ?
O3 Be2 O5 113.69(10) . 5_666 ?
O3 Be2 O5 113.69(10) 2_655 6_565 ?
O3 Be2 O5 101.43(11) . 6_565 ?
O5 Be2 O5 112.2(4) 5_666 6_565 ?
P1 O1 Be1 131.5(2) . 5_666 ?
P1 O2 Be1 142.7(2) . . ?
P1 O3 Be2 143.45(19) . . ?
P2 O4 Be1 136.59(19) . 7_556 ?
P2 O5 Be2 136.40(15) . 5_666 ?
P2 O6 Be1 151.7(2) . . ?
C2 N1 C1 113.5(3) . . ?
C2 N1 H1D 108.9 . . ?
C1 N1 H1D 108.9 . . ?
C2 N1 H1E 108.9 . . ?
C1 N1 H1E 108.9 . . ?
H1D N1 H1E 107.7 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

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
N1 H1D O5 0.90 2.14 2.947(3) 149.1 4_546
N1 H1D O3 0.90 2.30 3.025(4) 137.9 7_556
N1 H1E O1 0.90 2.07 2.953(3) 166.1 3_445

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.070