#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:40:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179150 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/11/4311186.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_4311186
loop_
_publ_author_name
'Wei Liu'
'Minghui Ge'
'Xinxin Yang'
'Haohong Chen'
'Manrong Li'
'Jingtai Zhao'
_publ_section_title
;
 Hydrothermal Synthesis and Characterization of Two Organically Templated
 Cadmium Borophosphates with Novel Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3910
_journal_page_last               3914
_journal_paper_doi               10.1021/ic0498034
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'B2 Cd Cl H O13 P3, C4 H16 N3'
_chemical_formula_sum            'C4 H17 B2 Cd Cl N3 O13 P3'
_chemical_formula_weight         577.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.470(2)
_cell_length_b                   12.307(3)
_cell_length_c                   27.311(6)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.01
_cell_measurement_theta_min      1.49
_cell_volume                     3183.0(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            13778
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    1.920
_exptl_absorpt_correction_T_max  0.7616
_exptl_absorpt_correction_T_min  0.5139
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0095P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0581
_reflns_number_gt                2154
_reflns_number_total             3127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0498034si20040216_033138_1.cif
_cod_data_source_block           (C4H16N3)[CdClB2P3O12(OH)]
_cod_database_code               4311186
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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
Cd1 Cd 0.13293(4) 0.20263(3) 0.117592(14) 0.01277(10) Uani 1 1 d . . .
Cl1 Cl -0.01542(14) 0.18813(11) 0.04323(5) 0.0279(3) Uani 1 1 d . . .
P1 P 0.48789(14) 0.24254(11) 0.09827(5) 0.0146(3) Uani 1 1 d . . .
P2 P 0.21814(13) 0.46672(10) 0.15012(5) 0.0125(3) Uani 1 1 d . . .
P3 P -0.03919(13) 0.23864(10) 0.22519(5) 0.0118(3) Uani 1 1 d . . .
B1 B 0.3992(6) 0.1625(4) 0.1859(2) 0.0124(14) Uani 1 1 d . . .
B2 B 0.2397(5) 0.3066(5) 0.2195(2) 0.0147(13) Uani 1 1 d . . .
O1 O 0.2622(3) 0.2133(2) 0.19009(12) 0.0113(8) Uani 1 1 d . . .
O2 O 0.3456(3) 0.2110(3) 0.07875(12) 0.0195(8) Uani 1 1 d . . .
O3 O 0.1431(3) 0.3872(2) 0.11748(13) 0.0202(8) Uani 1 1 d . . .
O4 O -0.0396(3) 0.1928(3) 0.17490(12) 0.0159(8) Uani 1 1 d . . .
O5 O 0.1541(3) 0.0188(2) 0.12550(13) 0.0166(8) Uani 1 1 d . . .
O6 O 0.4964(3) 0.2278(2) 0.15535(12) 0.0158(8) Uani 1 1 d . . .
O7 O 0.6104(3) 0.1892(3) 0.07455(12) 0.0208(8) Uani 1 1 d . . .
O8 O 0.5122(3) 0.3689(3) 0.08974(14) 0.0211(9) Uani 1 1 d . . .
H8 H 0.4470 0.4031 0.1021 0.032 Uiso 1 1 calc R . .
O9 O 0.2772(3) 0.4112(2) 0.19692(13) 0.0149(8) Uani 1 1 d . . .
O10 O 0.0864(3) 0.3163(2) 0.23416(12) 0.0152(8) Uani 1 1 d . . .
O11 O 0.1087(3) 0.5529(2) 0.16564(12) 0.0156(8) Uani 1 1 d . . .
O12 O -0.0348(3) 0.1490(2) 0.26463(13) 0.0141(8) Uani 1 1 d . . .
O13 O -0.1752(3) 0.3042(3) 0.23474(12) 0.0139(8) Uani 1 1 d . . .
C1 C 0.7450(6) 0.0062(4) 0.1759(2) 0.0258(15) Uani 1 1 d . . .
H11 H 0.7428 0.0842 0.1707 0.031 Uiso 1 1 calc R . .
H12 H 0.6804 -0.0105 0.2024 0.031 Uiso 1 1 calc R . .
C2 C 0.6951(5) -0.0497(4) 0.1301(2) 0.0236(15) Uani 1 1 d . . .
H21 H 0.7265 -0.1247 0.1307 0.028 Uiso 1 1 calc R . .
H22 H 0.5927 -0.0499 0.1297 0.028 Uiso 1 1 calc R . .
C3 C 0.6877(6) -0.0455(4) 0.0398(2) 0.0307(16) Uani 1 1 d . . .
H31 H 0.7046 -0.1233 0.0402 0.037 Uiso 1 1 calc R . .
H32 H 0.5863 -0.0343 0.0398 0.037 Uiso 1 1 calc R . .
C4 C 0.7471(6) 0.0000(4) -0.0059(2) 0.0328(16) Uani 1 1 d . . .
H41 H 0.7131 -0.0429 -0.0333 0.039 Uiso 1 1 calc R . .
H42 H 0.8490 -0.0074 -0.0049 0.039 Uiso 1 1 calc R . .
N1 N 0.8910(4) -0.0264(3) 0.19071(16) 0.0264(12) Uani 1 1 d . . .
H13 H 0.8956 -0.0984 0.1931 0.040 Uiso 1 1 calc R . .
H14 H 0.9118 0.0034 0.2195 0.040 Uiso 1 1 calc R . .
H15 H 0.9524 -0.0036 0.1683 0.040 Uiso 1 1 calc R . .
N2 N 0.7474(4) 0.0026(3) 0.08489(15) 0.0206(11) Uani 1 1 d . . .
H23 H 0.8421 -0.0031 0.0839 0.025 Uiso 1 1 calc R . .
H24 H 0.7256 0.0738 0.0858 0.025 Uiso 1 1 calc R . .
N3 N 0.7117(4) 0.1162(3) -0.01509(16) 0.0243(12) Uani 1 1 d . . .
H33 H 0.6517 0.1394 0.0077 0.036 Uiso 1 1 calc R . .
H34 H 0.6721 0.1228 -0.0445 0.036 Uiso 1 1 calc R . .
H35 H 0.7902 0.1559 -0.0140 0.036 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 0.0033 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'
B B 0.0013 0.0007 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
_geom_angle_publ_flag
O4 Cd1 O3 94.87(12) . . ?
O4 Cd1 O2 164.03(11) . . ?
O3 Cd1 O2 85.22(12) . . ?
O4 Cd1 O5 86.83(12) . . ?
O3 Cd1 O5 170.81(11) . . ?
O2 Cd1 O5 90.66(12) . . ?
O4 Cd1 O1 78.18(11) . . ?
O3 Cd1 O1 85.57(12) . . ?
O2 Cd1 O1 85.91(11) . . ?
O5 Cd1 O1 85.95(11) . . ?
O4 Cd1 Cl1 98.83(9) . . ?
O3 Cd1 Cl1 95.44(10) . . ?
O2 Cd1 Cl1 97.06(9) . . ?
O5 Cd1 Cl1 93.21(9) . . ?
O1 Cd1 Cl1 176.92(8) . . ?
O7 P1 O2 115.7(2) . . ?
O7 P1 O6 110.0(2) . . ?
O2 P1 O6 111.64(19) . . ?
O7 P1 O8 104.85(19) . . ?
O2 P1 O8 109.3(2) . . ?
O6 P1 O8 104.52(19) . . ?
O3 P2 O5 112.80(19) . 8_665 ?
O3 P2 O11 107.03(19) . . ?
O5 P2 O11 111.43(18) 8_665 . ?
O3 P2 O9 111.83(19) . . ?
O5 P2 O9 105.18(19) 8_665 . ?
O11 P2 O9 108.57(19) . . ?
O4 P3 O13 110.66(19) . . ?
O4 P3 O12 111.96(19) . . ?
O13 P3 O12 106.17(18) . . ?
O4 P3 O10 112.58(19) . . ?
O13 P3 O10 107.03(18) . . ?
O12 P3 O10 108.10(19) . . ?
O1 B1 O11 112.6(4) . 8_655 ?
O1 B1 O6 111.6(4) . . ?
O11 B1 O6 108.7(4) 8_655 . ?
O1 B1 O12 110.5(4) . 6_656 ?
O11 B1 O12 105.1(4) 8_655 6_656 ?
O6 B1 O12 108.0(4) . 6_656 ?
O1 B2 O9 115.8(4) . . ?
O1 B2 O13 112.2(4) . 6_656 ?
O9 B2 O13 103.8(4) . 6_656 ?
O1 B2 O10 111.0(4) . . ?
O9 B2 O10 105.9(4) . . ?
O13 B2 O10 107.4(4) 6_656 . ?
B2 O1 B1 122.1(4) . . ?
B2 O1 Cd1 116.6(3) . . ?
B1 O1 Cd1 112.3(3) . . ?
P1 O2 Cd1 129.8(2) . . ?
P2 O3 Cd1 132.1(2) . . ?
P3 O4 Cd1 128.06(18) . . ?
P2 O5 Cd1 121.87(17) 8_655 . ?
B1 O6 P1 126.1(3) . . ?
P1 O8 H8 109.5 . . ?
B2 O9 P2 130.0(3) . . ?
B2 O10 P3 130.4(3) . . ?
B1 O11 P2 140.7(3) 8_665 . ?
B1 O12 P3 122.6(3) 6_556 . ?
B2 O13 P3 127.2(3) 6_556 . ?
N1 C1 C2 113.1(4) . . ?
N1 C1 H11 109.0 . . ?
C2 C1 H11 109.0 . . ?
N1 C1 H12 109.0 . . ?
C2 C1 H12 109.0 . . ?
H11 C1 H12 107.8 . . ?
N2 C2 C1 112.9(4) . . ?
N2 C2 H21 109.0 . . ?
C1 C2 H21 109.0 . . ?
N2 C2 H22 109.0 . . ?
C1 C2 H22 109.0 . . ?
H21 C2 H22 107.8 . . ?
C4 C3 N2 114.0(5) . . ?
C4 C3 H31 108.8 . . ?
N2 C3 H31 108.8 . . ?
C4 C3 H32 108.8 . . ?
N2 C3 H32 108.8 . . ?
H31 C3 H32 107.7 . . ?
C3 C4 N3 114.8(5) . . ?
C3 C4 H41 108.6 . . ?
N3 C4 H41 108.6 . . ?
C3 C4 H42 108.6 . . ?
N3 C4 H42 108.6 . . ?
H41 C4 H42 107.5 . . ?
C1 N1 H13 109.5 . . ?
C1 N1 H14 109.5 . . ?
H13 N1 H14 109.5 . . ?
C1 N1 H15 109.5 . . ?
H13 N1 H15 109.5 . . ?
H14 N1 H15 109.5 . . ?
C2 N2 C3 113.2(4) . . ?
C2 N2 H23 108.9 . . ?
C3 N2 H23 108.9 . . ?
C2 N2 H24 108.9 . . ?
C3 N2 H24 108.9 . . ?
H23 N2 H24 107.8 . . ?
C4 N3 H33 109.5 . . ?
C4 N3 H34 109.5 . . ?
H33 N3 H34 109.5 . . ?
C4 N3 H35 109.5 . . ?
H33 N3 H35 109.5 . . ?
H34 N3 H35 109.5 . . ?
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
Cd1 O4 2.266(3) . ?
Cd1 O3 2.273(3) . ?
Cd1 O2 2.278(3) . ?
Cd1 O5 2.281(3) . ?
Cd1 O1 2.332(3) . ?
Cd1 Cl1 2.4758(14) . ?
P1 O7 1.483(3) . ?
P1 O2 1.500(3) . ?
P1 O6 1.572(4) . ?
P1 O8 1.589(3) . ?
P2 O3 1.503(3) . ?
P2 O5 1.526(3) 8_665 ?
P2 O11 1.543(3) . ?
P2 O9 1.553(3) . ?
P3 O4 1.485(3) . ?
P3 O13 1.542(3) . ?
P3 O12 1.542(3) . ?
P3 O10 1.545(3) . ?
B1 O1 1.445(6) . ?
B1 O11 1.460(6) 8_655 ?
B1 O6 1.480(6) . ?
B1 O12 1.499(7) 6_656 ?
B2 O1 1.417(6) . ?
B2 O9 1.471(6) . ?
B2 O13 1.488(6) 6_656 ?
B2 O10 1.511(6) . ?
O5 P2 1.526(3) 8_655 ?
O8 H8 0.8200 . ?
O11 B1 1.460(6) 8_665 ?
O12 B1 1.499(7) 6_556 ?
O13 B2 1.488(6) 6_556 ?
C1 N1 1.495(6) . ?
C1 C2 1.504(7) . ?
C1 H11 0.9700 . ?
C1 H12 0.9700 . ?
C2 N2 1.479(6) . ?
C2 H21 0.9700 . ?
C2 H22 0.9700 . ?
C3 C4 1.479(7) . ?
C3 N2 1.479(6) . ?
C3 H31 0.9700 . ?
C3 H32 0.9700 . ?
C4 N3 1.491(6) . ?
C4 H41 0.9700 . ?
C4 H42 0.9700 . ?
N1 H13 0.8900 . ?
N1 H14 0.8900 . ?
N1 H15 0.8900 . ?
N2 H23 0.9000 . ?
N2 H24 0.9000 . ?
N3 H33 0.8900 . ?
N3 H34 0.8900 . ?
N3 H35 0.8900 . ?
