#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:15:23 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179960 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/54/7025411.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_7025411
loop_
_publ_author_name
'Liu, Wei'
'Zhang, Lan'
'Su, Ge'
'Cao, Li-Xin'
'Wang, Yong-Gang'
_publ_section_title
;
 A novel polyoxochromium borophosphate with new 6-membered ring
 crown-shaped clusters.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7262
_journal_page_last               7265
_journal_paper_doi               10.1039/c000515k
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'B4 Cr8 H8 K5 Na11 O70 P12'
_chemical_formula_weight         2407.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2'
_symmetry_space_group_name_H-M   'P m n n'
_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            2
_cell_length_a                   10.4633(9)
_cell_length_b                   15.0491(11)
_cell_length_c                   18.7214(15)
_cell_measurement_reflns_used    479
_cell_measurement_temperature    293(2)
_cell_volume                     2947.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  ω
_diffrn_measurement_method       ccd
_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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19921
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    2.333
_exptl_absorpt_correction_T_max  0.8923
_exptl_absorpt_correction_T_min  0.8002
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.679
_refine_diff_density_min         -1.377
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1128P)²+25.9734P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2004
_refine_ls_wR_factor_ref         0.2031
_reflns_number_gt                3401
_reflns_number_total             3581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c000515k.txt
_cod_data_source_block           cr
_cod_original_sg_symbol_H-M      Pmnn
_cod_database_code               7025411
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x, -y, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x, y, 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
Cr1 Cr 0.14060(8) 0.19801(6) 0.45810(5) 0.0172(3) Uani 1 1 d .
Cr2 Cr 0.14018(8) -0.10712(6) 0.36287(5) 0.0166(3) Uani 1 1 d .
P1 P 0.25541(12) 0.08096(10) 0.33433(7) 0.0176(3) Uani 1 1 d .
P2 P 0.25401(13) -0.29093(9) 0.40535(8) 0.0188(3) Uani 1 1 d .
P3 P 0.0000 0.32481(19) 0.34510(13) 0.0324(5) Uani 1 2 d S
P4 P 0.0000 -0.11460(14) 0.21209(11) 0.0206(4) Uani 1 2 d S
B1 B 0.0000 0.0736(5) 0.3536(4) 0.0146(15) Uani 1 2 d S
B2 B 0.0000 -0.2700(6) 0.4145(5) 0.0189(16) Uani 1 2 d S
Na1 Na 0.0000 0.0000 0.5000 0.0192(9) Uani 1 4 d S
O1 O 0.0000 -0.0209(3) 0.3711(3) 0.0167(10) Uani 1 2 d S
O2 O 0.0000 -0.1920(4) 0.3705(3) 0.0183(11) Uani 1 2 d S
O3 O 0.0000 0.2528(4) 0.5100(3) 0.0169(10) Uani 1 2 d S
O4 O 0.0000 0.1289(4) 0.4163(3) 0.0196(11) Uani 1 2 d S
O5 O 0.2680(4) -0.2068(3) 0.3587(2) 0.0217(8) Uani 1 1 d .
O6 O 0.1130(4) 0.0939(3) 0.3079(2) 0.0202(8) Uani 1 1 d .
O7 O 0.1640(4) 0.1028(3) 0.5317(2) 0.0189(8) Uani 1 1 d .
O8 O 0.3451(4) -0.3616(3) 0.3816(2) 0.0255(9) Uani 1 1 d .
O9 O 0.1126(4) -0.3272(3) 0.3949(2) 0.0203(8) Uani 1 1 d .
O10 O 0.1216(4) 0.2921(3) 0.3838(2) 0.0269(9) Uani 1 1 d .
O11 O 0.2760(4) 0.1377(3) 0.4007(2) 0.0291(10) Uani 1 1 d .
O12 O 0.3381(4) 0.1129(3) 0.2740(2) 0.0323(10) Uani 1 1 d .
O13 O 0.2699(4) 0.2688(3) 0.5143(2) 0.0220(8) Uani 1 1 d .
O14 O 0.2765(4) -0.0158(3) 0.3525(3) 0.0278(9) Uani 1 1 d .
O15 O 0.1228(4) -0.1123(3) 0.2575(2) 0.0284(10) Uani 1 1 d .
O16 O 0.0000 0.2901(7) 0.2690(4) 0.051(2) Uani 1 2 d S
O17 O 0.0000 0.4244(7) 0.3453(6) 0.066(3) Uani 1 2 d S
O18 O 0.0000 -0.2030(8) 0.1737(7) 0.082(4) Uani 1 2 d S
O19 O 0.0000 -0.0330(7) 0.1662(6) 0.070(3) Uani 1 2 d S
K1 K 0.0000 0.3940(3) 0.1573(3) 0.0555(14) Uani 0.899(16) 2 d SP
K2 K 0.2277(3) -0.50101(18) 0.33024(15) 0.0579(7) Uani 0.75 1 d P
K3 K 0.0000 0.448(3) 0.198(3) 0.064(19) Uani 0.101(16) 2 d SP
Na2A Na 0.0000 0.1407(8) 0.2080(4) 0.035(3) Uani 0.79(3) 2 d SP
Na2B Na 0.0000 0.093(3) 0.1880(13) 0.034(7) Uani 0.21(3) 2 d SP
Na3 Na 0.0000 -0.2913(4) 0.0547(3) 0.0501(12) Uani 1 2 d S
Na4 Na 0.2599(3) -0.2341(2) 0.22728(17) 0.0461(8) Uani 1 1 d .
Na5 Na 0.0000 -0.3170(4) 0.2732(3) 0.0603(14) Uani 1 2 d S
O20 O 0.0000 0.0503(4) 0.0642(3) 0.0204(11) Uani 1 2 d S
O21 O 0.0000 -0.3235(9) 0.1149(8) 0.086(4) Uani 1 2 d S
O22 O 0.0000 0.4253(15) 0.4831(11) 0.076(7) Uani 0.50 2 d SP
023 O 0.0000 -0.4106 0.3051 0.065(5) Uani 0.50 2 d SP
024 O 0.0000 -0.335(2) -0.0088(14) 0.086(8) Uani 0.50 2 d SP
O25 O 0.0000 0.1678(3) -0.0011(10) 0.092(6) Uiso 0.50 2 d SP
O26A O 0.258(3) -0.555(2) 0.4418(17) 0.078(10) Uiso 0.28(2) 1 d P
O26B O 0.142(3) -0.0753(17) 0.0440(14) 0.042(8) Uiso 0.22(2) 1 d P
H1 H 0.0000 0.4354 0.3965 0.050 Uiso 1 2 d S
H2 H 0.0000 0.3362 0.2389 0.050 Uiso 1 2 d S
H3 H 0.0000 -0.0338 0.1172 0.050 Uiso 1 2 d S
H4 H 0.0000 -0.1928 0.1208 0.050 Uiso 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
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
O3 Cr1 O4 81.78(17) . .
O3 Cr1 O10 88.4(2) . .
O4 Cr1 O10 91.3(2) . .
O3 Cr1 O11 176.10(17) . .
O4 Cr1 O11 94.37(18) . .
O10 Cr1 O11 91.0(2) . .
O3 Cr1 O7 93.0(2) . .
O4 Cr1 O7 89.2(2) . .
O10 Cr1 O7 178.57(18) . .
O11 Cr1 O7 87.64(18) . .
O3 Cr1 O13 91.30(16) . .
O4 Cr1 O13 171.64(19) . .
O10 Cr1 O13 93.18(18) . .
O11 Cr1 O13 92.58(17) . .
O7 Cr1 O13 86.41(17) . .
O2 Cr2 O1 82.23(18) . .
O2 Cr2 O15 88.7(2) . .
O1 Cr2 O15 92.1(2) . .
O2 Cr2 O7 92.5(2) . 3_556
O1 Cr2 O7 89.63(19) . 3_556
O15 Cr2 O7 178.05(17) . 3_556
O2 Cr2 O14 176.80(18) . .
O1 Cr2 O14 95.00(17) . .
O15 Cr2 O14 89.8(2) . .
O7 Cr2 O14 89.10(18) 3_556 .
O2 Cr2 O5 90.84(17) . .
O1 Cr2 O5 172.83(18) . .
O15 Cr2 O5 89.60(18) . .
O7 Cr2 O5 88.85(16) 3_556 .
O14 Cr2 O5 91.99(18) . .
O12 P1 O14 113.2(3) . .
O12 P1 O11 110.7(3) . .
O14 P1 O11 109.6(3) . .
O12 P1 O6 105.5(2) . .
O14 P1 O6 109.1(2) . .
O11 P1 O6 108.6(2) . .
O8 P2 O5 110.7(2) . .
O8 P2 O13 111.9(2) . 3_556
O5 P2 O13 111.3(2) . 3_556
O8 P2 O9 108.2(2) . .
O5 P2 O9 107.5(2) . .
O13 P2 O9 107.0(2) 3_556 .
O17 P3 O16 110.2(6) . .
O17 P3 O10 108.5(3) . .
O16 P3 O10 109.3(3) . .
O17 P3 O10 108.5(3) . 7
O16 P3 O10 109.3(3) . 7
O10 P3 O10 110.9(3) . 7
O19 P4 O18 116.6(8) . .
O19 P4 O15 107.4(3) . .
O18 P4 O15 106.4(3) . .
O19 P4 O15 107.4(3) . 7
O18 P4 O15 106.4(3) . 7
O15 P4 O15 112.9(3) . 7
O4 B1 O1 112.3(6) . .
O4 B1 O6 110.4(4) . 7
O1 B1 O6 109.2(4) . 7
O4 B1 O6 110.4(4) . .
O1 B1 O6 109.2(4) . .
O6 B1 O6 104.9(6) 7 .
O2 B2 O3 114.6(7) . 5_556
O2 B2 O9 109.2(4) . 7
O3 B2 O9 110.0(4) 5_556 7
O2 B2 O9 109.2(4) . .
O3 B2 O9 110.0(4) 5_556 .
O9 B2 O9 103.1(6) 7 .
O7 Na1 O7 180.00(19) 5_556 .
O7 Na1 O7 92.00(19) 5_556 3_556
O7 Na1 O7 88.00(19) . 3_556
O7 Na1 O7 88.00(19) 5_556 7
O7 Na1 O7 92.00(19) . 7
O7 Na1 O7 180.000(1) 3_556 7
O7 Na1 O1 70.66(12) 5_556 .
O7 Na1 O1 109.34(12) . .
O7 Na1 O1 70.66(12) 3_556 .
O7 Na1 O1 109.34(12) 7 .
O7 Na1 O1 109.34(12) 5_556 5_556
O7 Na1 O1 70.66(12) . 5_556
O7 Na1 O1 109.34(12) 3_556 5_556
O7 Na1 O1 70.66(12) 7 5_556
O1 Na1 O1 180.0 . 5_556
O7 Na1 O4 110.35(12) 5_556 .
O7 Na1 O4 69.65(12) . .
O7 Na1 O4 110.35(12) 3_556 .
O7 Na1 O4 69.65(12) 7 .
O1 Na1 O4 58.51(18) . .
O1 Na1 O4 121.49(18) 5_556 .
O7 Na1 O4 69.65(12) 5_556 5_556
O7 Na1 O4 110.35(12) . 5_556
O7 Na1 O4 69.65(12) 3_556 5_556
O7 Na1 O4 110.35(12) 7 5_556
O1 Na1 O4 121.49(18) . 5_556
O1 Na1 O4 58.51(18) 5_556 5_556
O4 Na1 O4 180.0 . 5_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 O3 1.946(3) .
Cr1 O4 1.964(4) .
Cr1 O10 1.994(4) .
Cr1 O11 1.996(4) .
Cr1 O7 2.004(4) .
Cr1 O13 2.018(4) .
Cr2 O2 1.950(4) .
Cr2 O1 1.964(4) .
Cr2 O15 1.982(4) .
Cr2 O7 1.990(4) 3_556
Cr2 O14 1.990(4) .
Cr2 O5 2.012(4) .
P1 O12 1.502(4) .
P1 O14 1.512(4) .
P1 O11 1.523(4) .
P1 O6 1.582(4) .
P2 O8 1.496(4) .
P2 O5 1.545(4) .
P2 O13 1.550(4) 3_556
P2 O9 1.590(4) .
P3 O17 1.498(10) .
P3 O16 1.518(8) .
P3 O10 1.545(5) .
P3 O10 1.545(5) 7
P3 K1 3.667(5) .
P4 O19 1.499(8) .
P4 O18 1.511(9) .
P4 O15 1.541(4) .
P4 O15 1.541(4) 7
B1 O4 1.440(9) .
B1 O1 1.460(10) .
B1 O6 1.492(6) 7
B1 O6 1.492(6) .
B2 O2 1.435(10) .
B2 O3 1.438(10) 5_556
B2 O9 1.504(7) 7
B2 O9 1.504(7) .
Na1 O7 2.385(4) 5_556
Na1 O7 2.385(4) .
Na1 O7 2.385(4) 3_556
Na1 O7 2.385(4) 7
Na1 O1 2.433(5) .
Na1 O1 2.433(5) 5_556
Na1 O4 2.494(6) .
Na1 O4 2.494(6) 5_556
