#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:59:10 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180525 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/94/7219467.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7219467
loop_
_publ_author_name
'Wang, Kangcai'
'Li, Jing'
'Xu, Dingguo'
'Luo, Daibing'
'Lin, Zhien'
_publ_section_title
;
 Open-framework beryllium phosphates with a zeolitic CrB4topology and
 their structural analogues containing 12-ring channels
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              2162
_journal_paper_doi               10.1039/C4CE02226B
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C14 H24 Be2 N2 O16 P4'
_chemical_formula_weight         618.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-11-08 deposited with the CCDC.
2015-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.3000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.8218(3)
_cell_length_b                   21.5546(3)
_cell_length_c                   9.49200(10)
_cell_measurement_reflns_used    6101
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.4690
_cell_measurement_theta_min      3.8750
_cell_volume                     4668.05(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12573
_diffrn_reflns_theta_full        67.08
_diffrn_reflns_theta_max         67.08
_diffrn_reflns_theta_min         5.41
_exptl_absorpt_coefficient_mu    3.777
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         4172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1161P)²+11.4551P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.1812
_reflns_number_gt                3716
_reflns_number_total             4172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02226b2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7219466--7219469.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7219467
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'
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 0.35330(3) 0.33300(4) 0.40633(8) 0.0282(2) Uani 1 1 d . . .
P2 P 0.5000 0.25913(6) 0.2500 0.0328(3) Uani 1 2 d S . .
P3 P 0.16381(4) 0.34755(4) 0.40845(9) 0.0319(3) Uani 1 1 d . . .
P4 P 0.26659(5) 0.47257(4) 0.19748(9) 0.0430(3) Uani 1 1 d . . .
P5 P 0.50849(17) 0.19590(8) 0.7326(5) 0.0325(8) Uani 0.50 1 d P . .
Be1 Be 0.26657(16) 0.42646(16) 0.4914(4) 0.0222(7) Uani 1 1 d . . .
Be2 Be 0.43119(16) 0.2307(2) 0.4954(4) 0.0271(8) Uani 1 1 d . . .
O1 O 0.32195(11) 0.37897(12) 0.4954(3) 0.0409(6) Uani 1 1 d . A .
O2 O 0.39882(11) 0.29827(12) 0.4914(3) 0.0396(6) Uani 1 1 d . . .
O3 O 0.30961(14) 0.28528(17) 0.3468(6) 0.0937(16) Uani 1 1 d . . .
H3 H 0.3269 0.2602 0.2980 0.141 Uiso 1 1 calc R . .
O4 O 0.38152(18) 0.36490(17) 0.2849(4) 0.0762(12) Uani 1 1 d . . .
O5 O 0.46827(10) 0.22001(12) 0.3535(3) 0.0400(6) Uani 1 1 d . . .
O6 O 0.45716(18) 0.2995(2) 0.1640(4) 0.0937(16) Uani 1 1 d . . .
H6 H 0.4754 0.3206 0.1080 0.141 Uiso 1 1 calc R . .
O7 O 0.20431(11) 0.38973(12) 0.4880(3) 0.0419(6) Uani 1 1 d . A .
O8 O 0.14226(18) 0.37765(19) 0.2739(3) 0.0792(12) Uani 1 1 d . . .
O9 O 0.19751(15) 0.28779(15) 0.3700(5) 0.0829(14) Uani 1 1 d . . .
H9 H 0.1795 0.2574 0.3980 0.124 Uiso 1 1 calc R . .
O10 O 0.11376(10) 0.32789(12) 0.4973(3) 0.0372(6) Uani 1 1 d . . .
O11 O 0.26936(10) 0.47333(10) 0.3551(2) 0.0319(5) Uani 1 1 d . A .
O12 O 0.27075(13) 0.53363(11) 0.1347(3) 0.0431(6) Uani 1 1 d . . .
O13 O 0.1937(3) 0.4630(3) 0.1572(6) 0.055(2) Uani 0.527(9) 1 d P A 1
O14 O 0.2915(4) 0.4182(3) 0.1341(6) 0.062(3) Uani 0.527(9) 1 d P A 1
O13' O 0.2345(4) 0.4216(3) 0.1320(6) 0.060(3) Uani 0.473(9) 1 d P A 2
O14' O 0.3380(3) 0.4530(3) 0.1534(7) 0.053(2) Uani 0.473(9) 1 d P A 2
O15 O 0.47362(11) 0.23205(14) 0.6354(3) 0.0446(7) Uani 1 1 d . . .
O16 O 0.5644(3) 0.1800(4) 0.6526(6) 0.071(2) Uani 0.50 1 d P . .
O17 O 0.4779(3) 0.1337(3) 0.7587(10) 0.086(3) Uani 0.50 1 d P . .
N1 N 0.1187(3) 0.4155(3) -0.1250(5) 0.104(2) Uani 1 1 d . . .
N2 N 0.4092(2) 0.3814(3) -0.1335(5) 0.0851(17) Uani 1 1 d . . .
C1 C 0.1786(6) 0.3256(6) -0.1028(16) 0.194(6) Uani 1 1 d . . .
H1A H 0.2116 0.3040 -0.1401 0.290 Uiso 1 1 calc R . .
H1B H 0.1444 0.2998 -0.1110 0.290 Uiso 1 1 calc R . .
H1C H 0.1862 0.3352 -0.0054 0.290 Uiso 1 1 calc R . .
C2 C 0.1693(5) 0.3794(6) -0.1770(8) 0.143(5) Uani 1 1 d . . .
H2A H 0.1625 0.3694 -0.2756 0.171 Uiso 1 1 calc R . .
H2B H 0.2044 0.4049 -0.1700 0.171 Uiso 1 1 calc R . .
C3 C 0.1241(5) 0.4753(5) -0.0812(11) 0.138(4) Uani 1 1 d . . .
H3A H 0.1606 0.4944 -0.0860 0.165 Uiso 1 1 calc R . .
C4 C 0.0792(4) 0.5078(5) -0.0317(15) 0.149(5) Uani 1 1 d . . .
H4 H 0.0851 0.5483 -0.0006 0.179 Uiso 1 1 calc R . .
C5 C 0.0248(3) 0.4822(3) -0.0264(7) 0.101(3) Uani 1 1 d . . .
C6 C 0.0210(4) 0.4198(4) -0.0690(9) 0.119(3) Uani 1 1 d . . .
H6A H -0.0147 0.3992 -0.0629 0.142 Uiso 1 1 calc R . .
C7 C 0.0662(5) 0.3902(5) -0.1169(9) 0.132(4) Uani 1 1 d . . .
H7 H 0.0613 0.3494 -0.1467 0.159 Uiso 1 1 calc R . .
C8 C 0.3336(6) 0.3086(7) -0.0772(13) 0.203(7) Uani 1 1 d . . .
H8A H 0.3089 0.2761 -0.1143 0.304 Uiso 1 1 calc R . .
H8B H 0.3098 0.3417 -0.0429 0.304 Uiso 1 1 calc R . .
H8C H 0.3576 0.2925 -0.0013 0.304 Uiso 1 1 calc R . .
C9 C 0.3688(4) 0.3305(4) -0.1818(7) 0.106(3) Uani 1 1 d . . .
H9A H 0.3442 0.3458 -0.2589 0.127 Uiso 1 1 calc R . .
H9B H 0.3920 0.2965 -0.2175 0.127 Uiso 1 1 calc R . .
C10 C 0.3896(3) 0.4389(4) -0.1198(13) 0.144(4) Uani 1 1 d . . .
H10 H 0.3503 0.4470 -0.1413 0.173 Uiso 1 1 calc R . .
C11 C 0.4233(3) 0.4853(4) -0.0771(14) 0.154(5) Uani 1 1 d . . .
H11 H 0.4084 0.5255 -0.0787 0.185 Uiso 1 1 calc R . .
C12 C 0.4814(3) 0.4752(3) -0.0291(8) 0.097(3) Uani 1 1 d . . .
C13 C 0.5002(3) 0.4147(3) -0.0418(7) 0.087(2) Uani 1 1 d . . .
H13 H 0.5383 0.4046 -0.0137 0.105 Uiso 1 1 calc R . .
C14 C 0.4645(4) 0.3697(4) -0.0942(6) 0.093(2) Uani 1 1 d . . .
H14 H 0.4790 0.3295 -0.1029 0.111 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Be Be 0.0038 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O1 P1 O4 110.51(17) . .
O1 P1 O2 111.11(14) . .
O4 P1 O2 109.76(18) . .
O1 P1 O3 109.75(19) . .
O4 P1 O3 108.1(3) . .
O2 P1 O3 107.48(19) . .
O5 P2 O5 111.3(2) . 2_655
O5 P2 O6 106.49(17) . 2_655
O5 P2 O6 111.00(17) 2_655 2_655
O5 P2 O6 111.00(17) . .
O5 P2 O6 106.49(17) 2_655 .
O6 P2 O6 110.7(4) 2_655 .
O7 P3 O10 111.08(14) . .
O7 P3 O8 110.73(17) . .
O10 P3 O8 111.18(19) . .
O7 P3 O9 108.76(19) . .
O10 P3 O9 106.67(17) . .
O8 P3 O9 108.3(3) . .
O14 P4 O12 122.5(3) . .
O14 P4 O13' 53.6(4) . .
O12 P4 O13' 123.2(3) . .
O14 P4 O11 114.7(2) . .
O12 P4 O11 113.57(14) . .
O13' P4 O11 116.5(3) . .
O14 P4 O13 101.5(4) . .
O12 P4 O13 95.2(2) . .
O13' P4 O13 48.2(4) . .
O11 P4 O13 104.1(2) . .
O14 P4 O14' 47.4(4) . .
O12 P4 O14' 92.9(2) . .
O13' P4 O14' 100.4(4) . .
O11 P4 O14' 102.9(2) . .
O13 P4 O14' 145.7(4) . .
P5 P5 O17 97.7(5) 2_656 2_656
P5 P5 O15 89.8(10) 2_656 .
O17 P5 O15 133.5(4) 2_656 .
P5 P5 O15 70.4(10) 2_656 2_656
O17 P5 O15 113.1(5) 2_656 2_656
O15 P5 O15 112.7(2) . 2_656
P5 P5 O17 62.9(5) 2_656 .
O17 P5 O17 40.9(7) 2_656 .
O15 P5 O17 109.3(4) . .
O15 P5 O17 115.4(4) 2_656 .
P5 P5 O16 164.1(9) 2_656 .
O17 P5 O16 67.9(5) 2_656 .
O15 P5 O16 104.9(3) . .
O15 P5 O16 108.1(4) 2_656 .
O17 P5 O16 105.7(6) . .
P5 P5 O16 11.9(7) 2_656 2_656
O17 P5 O16 89.5(5) 2_656 2_656
O15 P5 O16 89.3(3) . 2_656
O15 P5 O16 81.5(2) 2_656 2_656
O17 P5 O16 52.2(5) . 2_656
O16 P5 O16 157.3(6) . 2_656
O12 Be1 O1 106.6(3) 6_566 .
O12 Be1 O7 108.2(3) 6_566 .
O1 Be1 O7 111.9(3) . .
O12 Be1 O11 109.5(2) 6_566 .
O1 Be1 O11 111.2(2) . .
O7 Be1 O11 109.5(2) . .
O5 Be2 O15 111.6(3) . .
O5 Be2 O10 105.4(3) . 7_556
O15 Be2 O10 110.1(3) . 7_556
O5 Be2 O2 110.5(3) . .
O15 Be2 O2 105.3(3) . .
O10 Be2 O2 114.0(2) 7_556 .
P1 O1 Be1 141.7(2) . .
P1 O2 Be2 139.8(2) . .
P1 O3 H3 109.5 . .
P2 O5 Be2 137.3(2) . .
P2 O6 H6 109.5 . .
P3 O7 Be1 147.0(2) . .
P3 O9 H9 109.5 . .
P3 O10 Be2 137.1(2) . 7_556
P4 O11 Be1 141.1(2) . .
P4 O12 Be1 146.1(2) . 6_565
P5 O15 P5 19.75(17) . 2_656
P5 O15 Be2 145.8(3) . .
P5 O15 Be2 143.7(3) 2_656 .
P5 O16 O17 51.4(3) . 2_656
P5 O16 P5 4.0(2) . 2_656
O17 O16 P5 47.9(3) 2_656 2_656
O17 O17 P5 77.7(3) 2_656 2_656
O17 O17 P5 61.4(4) 2_656 .
P5 O17 P5 19.41(19) 2_656 .
O17 O17 O16 132.6(6) 2_656 2_656
P5 O17 O16 60.7(4) 2_656 2_656
P5 O17 O16 80.0(4) . 2_656
C7 N1 C3 116.7(10) . .
C7 N1 C2 121.1(8) . .
C3 N1 C2 122.2(8) . .
C10 N2 C14 118.0(8) . .
C10 N2 C9 120.5(7) . .
C14 N2 C9 121.3(6) . .
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C1 C2 N1 112.6(8) . .
C1 C2 H2A 109.1 . .
N1 C2 H2A 109.1 . .
C1 C2 H2B 109.1 . .
N1 C2 H2B 109.1 . .
H2A C2 H2B 107.8 . .
C4 C3 N1 122.7(8) . .
C4 C3 H3A 118.7 . .
N1 C3 H3A 118.7 . .
C3 C4 C5 120.6(10) . .
C3 C4 H4 119.7 . .
C5 C4 H4 119.7 . .
C4 C5 C6 115.3(9) . .
C4 C5 C5 120.8(9) . 5_565
C6 C5 C5 123.8(7) . 5_565
C7 C6 C5 121.6(7) . .
C7 C6 H6A 119.2 . .
C5 C6 H6A 119.2 . .
C6 C7 N1 123.0(10) . .
C6 C7 H7 118.5 . .
N1 C7 H7 118.5 . .
C9 C8 H8A 109.5 . .
C9 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C9 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C8 C9 N2 113.4(7) . .
C8 C9 H9A 108.9 . .
N2 C9 H9A 108.9 . .
C8 C9 H9B 108.9 . .
N2 C9 H9B 108.9 . .
H9A C9 H9B 107.7 . .
C11 C10 N2 122.9(7) . .
C11 C10 H10 118.6 . .
N2 C10 H10 118.6 . .
C10 C11 C12 121.4(6) . .
C10 C11 H11 119.3 . .
C12 C11 H11 119.3 . .
C13 C12 C11 114.2(8) . .
C13 C12 C12 122.8(7) . 5_665
C11 C12 C12 122.9(7) . 5_665
C14 C13 C12 121.6(6) . .
C14 C13 H13 119.2 . .
C12 C13 H13 119.2 . .
N2 C14 C13 121.7(6) . .
N2 C14 H14 119.2 . .
C13 C14 H14 119.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 O1 1.496(2) .
P1 O4 1.500(3) .
P1 O2 1.501(2) .
P1 O3 1.532(3) .
P2 O5 1.494(2) .
P2 O5 1.494(2) 2_655
P2 O6 1.531(3) 2_655
P2 O6 1.531(3) .
P3 O7 1.490(3) .
P3 O10 1.497(2) .
P3 O8 1.505(3) .
P3 O9 1.548(3) .
P4 O14 1.441(6) .
P4 O12 1.449(2) .
P4 O13' 1.452(6) .
P4 O11 1.496(2) .
P4 O13 1.711(5) .
P4 O14' 1.743(6) .
P5 P5 0.515(4) 2_656
P5 O17 1.378(6) 2_656
P5 O15 1.435(5) .
P5 O15 1.523(5) 2_656
P5 O17 1.534(6) .
P5 O16 1.538(6) .
P5 O16 2.038(7) 2_656
Be1 O12 1.610(4) 6_566
Be1 O1 1.626(4) .
Be1 O7 1.626(4) .
Be1 O11 1.644(4) .
Be2 O5 1.624(4) .
Be2 O15 1.626(4) .
Be2 O10 1.629(5) 7_556
Be2 O2 1.634(5) .
O3 H3 0.8200 .
O6 H6 0.8200 .
O9 H9 0.8200 .
O10 Be2 1.629(5) 7_556
O12 Be1 1.610(4) 6_565
O15 P5 1.523(5) 2_656
O16 O17 1.634(13) 2_656
O16 P5 2.038(7) 2_656
O17 O17 1.028(17) 2_656
O17 P5 1.378(6) 2_656
O17 O16 1.634(13) 2_656
N1 C7 1.320(9) .
N1 C3 1.359(12) .
N1 C2 1.486(13) .
N2 C10 1.326(9) .
N2 C14 1.332(9) .
N2 C9 1.498(10) .
C1 C2 1.372(16) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.337(15) .
C3 H3A 0.9300 .
C4 C5 1.361(10) .
C4 H4 0.9300 .
C5 C6 1.407(12) .
C5 C5 1.463(17) 5_565
C6 C7 1.305(14) .
C6 H6A 0.9300 .
C7 H7 0.9300 .
C8 C9 1.375(14) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 C11 1.320(14) .
C10 H10 0.9300 .
C11 C12 1.408(11) .
C11 H11 0.9300 .
C12 C13 1.380(8) .
C12 C12 1.465(16) 5_665
C13 C14 1.355(10) .
C13 H13 0.9300 .
C14 H14 0.9300 .
