#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:35:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179147 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/08/4310850.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_4310850
loop_
_publ_author_name
'Wei-Kuo Chang'
'Ray-Kuang Chiang'
'Yau-Chen Jiang'
'Sue-Lein Wang'
'Shang-Fan Lee'
'Kwang-Hwa Lii'
_publ_section_title
;
 Metamagnetism in Cobalt Phosphates with Pillared Layer Structures:
 [Co3(pyz)(HPO4)2F2] and [Co3(4,4'-bpy)(HPO4)2F2].xH2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2564
_journal_page_last               2568
_journal_paper_doi               10.1021/ic0353460
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '[Co3(4,4'-bpy)(HPO4)2F2].xH2O'
_chemical_formula_sum            'C10 H10 Co3 F2 N2 O8 P2'
_chemical_formula_weight         562.93
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.4440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.940(2)
_cell_length_b                   7.4421(5)
_cell_length_c                   7.4170(5)
_cell_measurement_temperature    297(2)
_cell_volume                     1649.65(19)
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXTL programs, version 5.1'
_computing_structure_solution    'SHELXTL programs, version 5.1'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Siemens Smart 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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7797
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    3.24
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   'empirical based on symmetry equivalents'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.310
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.430
_refine_ls_extinction_coef       0.0058(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         1893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.215
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0383
_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)+(0.0753P)²+0.4178P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                1745
_reflns_number_total             1893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0353460si20031120_081115_2.cif
_cod_data_source_block           cobipym
_cod_original_cell_volume        1649.6(2)
_cod_database_code               4310850
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
Co1 Co 0.309750(12) 0.47996(5) 0.15094(5) 0.01239(18) Uani 1 1 d . . .
Co2 Co 0.2500 0.7500 0.0000 0.01279(19) Uani 1 2 d S . .
P1 P 0.19859(2) 0.37385(9) 0.11274(9) 0.0115(2) Uani 1 1 d . . .
F1 F 0.30648(5) 0.6167(2) -0.0950(2) 0.0175(4) Uani 1 1 d . . .
O1 O 0.23956(7) 0.4892(3) 0.0858(3) 0.0172(5) Uani 1 1 d . . .
O2 O 0.18143(8) 0.2773(3) -0.0579(3) 0.0186(5) Uani 1 1 d . . .
O3 O 0.15897(7) 0.5050(3) 0.1588(3) 0.0180(5) Uani 1 1 d . . .
O4 O 0.20682(7) 0.2448(3) 0.2710(3) 0.0167(5) Uani 1 1 d . . .
O5 O 0.4295(4) 0.0019(16) 0.023(2) 0.092(7) Uani 0.365(17) 1 d P . .
N1 N 0.38117(10) 0.5038(5) 0.1917(4) 0.0314(8) Uani 1 1 d . . .
C1 C 0.4030(2) 0.6727(10) 0.1495(12) 0.0236(14) Uani 0.50 1 d P . .
C1A C 0.4035(2) 0.6263(11) 0.2518(14) 0.0300(16) Uani 0.50 1 d P . .
C2 C 0.4054(2) 0.3892(9) 0.2689(11) 0.0256(14) Uani 0.50 1 d P . .
C2A C 0.4060(2) 0.3357(9) 0.1489(11) 0.0248(14) Uani 0.50 1 d P . .
C3 C 0.4497(2) 0.6899(11) 0.1721(13) 0.0280(15) Uani 0.50 1 d P . .
C3A C 0.4504(2) 0.6323(11) 0.2768(13) 0.0313(16) Uani 0.50 1 d P . .
C4 C 0.4518(2) 0.3899(10) 0.2897(11) 0.0274(15) Uani 0.50 1 d P . .
C4A C 0.4522(2) 0.3295(10) 0.1741(12) 0.0285(15) Uani 0.50 1 d P . .
C5 C 0.47537(13) 0.5140(8) 0.2400(6) 0.0505(14) Uani 1 1 d . . .
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'
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'
F F 0.0171 0.0103 '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'
Co Co 0.3494 0.9721 '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
F1 Co1 O2 89.76(8) 6_566 7 ?
F1 Co1 F1 169.99(6) 6_566 . ?
O2 Co1 F1 99.26(8) 7 . ?
F1 Co1 O4 92.92(8) 6_566 4 ?
O2 Co1 O4 173.16(8) 7 4 ?
F1 Co1 O4 77.65(8) . 4 ?
F1 Co1 O1 96.91(8) 6_566 . ?
O2 Co1 O1 95.67(9) 7 . ?
F1 Co1 O1 78.00(8) . . ?
O4 Co1 O1 77.77(8) 4 . ?
F1 Co1 N1 90.09(10) 6_566 . ?
O2 Co1 N1 88.71(11) 7 . ?
F1 Co1 N1 94.41(10) . . ?
O4 Co1 N1 97.57(11) 4 . ?
O1 Co1 N1 171.74(11) . . ?
F1 Co1 Co2 123.19(5) 6_566 . ?
O2 Co1 Co2 127.58(6) 7 . ?
F1 Co1 Co2 47.36(5) . . ?
O4 Co1 Co2 46.05(6) 4 . ?
O1 Co1 Co2 46.04(6) . . ?
N1 Co1 Co2 126.03(9) . . ?
O4 Co2 O4 180.00(15) 4 6_565 ?
O4 Co2 O1 99.85(9) 4 7_565 ?
O4 Co2 O1 80.15(9) 6_565 7_565 ?
O4 Co2 O1 80.15(9) 4 . ?
O4 Co2 O1 99.85(9) 6_565 . ?
O1 Co2 O1 180.0 7_565 . ?
O4 Co2 F1 78.03(7) 4 . ?
O4 Co2 F1 101.97(7) 6_565 . ?
O1 Co2 F1 101.45(8) 7_565 . ?
O1 Co2 F1 78.55(8) . . ?
O4 Co2 F1 101.97(7) 4 7_565 ?
O4 Co2 F1 78.03(7) 6_565 7_565 ?
O1 Co2 F1 78.55(8) 7_565 7_565 ?
O1 Co2 F1 101.45(8) . 7_565 ?
F1 Co2 F1 180.00(13) . 7_565 ?
O4 Co2 Co1 47.48(6) 4 . ?
O4 Co2 Co1 132.52(6) 6_565 . ?
O1 Co2 Co1 132.30(6) 7_565 . ?
O1 Co2 Co1 47.70(6) . . ?
F1 Co2 Co1 46.44(4) . . ?
F1 Co2 Co1 133.56(4) 7_565 . ?
O4 Co2 Co1 132.52(6) 4 7_565 ?
O4 Co2 Co1 47.48(6) 6_565 7_565 ?
O1 Co2 Co1 47.70(6) 7_565 7_565 ?
O1 Co2 Co1 132.30(6) . 7_565 ?
F1 Co2 Co1 133.56(4) . 7_565 ?
F1 Co2 Co1 46.44(4) 7_565 7_565 ?
Co1 Co2 Co1 180.000(11) . 7_565 ?
O2 P1 O1 113.14(14) . . ?
O2 P1 O4 112.01(12) . . ?
O1 P1 O4 111.25(12) . . ?
O2 P1 O3 104.50(12) . . ?
O1 P1 O3 107.46(12) . . ?
O4 P1 O3 108.01(13) . . ?
Co1 F1 Co1 129.67(9) 6_565 . ?
Co1 F1 Co2 124.09(8) 6_565 . ?
Co1 F1 Co2 86.21(6) . . ?
P1 O1 Co2 135.00(13) . . ?
P1 O1 Co1 138.18(13) . . ?
Co2 O1 Co1 86.26(8) . . ?
P1 O2 Co1 132.53(13) . 7 ?
P1 O4 Co2 133.07(12) . 4_545 ?
P1 O4 Co1 139.95(13) . 4_545 ?
Co2 O4 Co1 86.47(8) 4_545 4_545 ?
C1A N1 C2 93.1(6) . . ?
C1A N1 C1 34.8(5) . . ?
C2 N1 C1 115.8(5) . . ?
C1A N1 C2A 116.1(5) . . ?
C2 N1 C2A 40.4(5) . . ?
C1 N1 C2A 116.0(4) . . ?
C1A N1 Co1 130.0(4) . . ?
C2 N1 Co1 123.9(4) . . ?
C1 N1 Co1 119.7(3) . . ?
C2A N1 Co1 113.8(3) . . ?
C1A C1 C3 88.1(9) . . ?
C1A C1 N1 55.3(7) . . ?
C3 C1 N1 120.6(6) . . ?
C1A C1 C3A 56.5(8) . . ?
C3 C1 C3A 31.7(4) . . ?
N1 C1 C3A 95.7(6) . . ?
C1 C1A N1 89.9(9) . . ?
C1 C1A C3A 93.9(10) . . ?
N1 C1A C3A 127.1(7) . . ?
C1 C1A C3 60.7(8) . . ?
N1 C1A C3 124.0(7) . . ?
C3A C1A C3 33.3(4) . . ?
C1 C1A C2 118.5(9) . . ?
N1 C1A C2 44.3(4) . . ?
C3A C1A C2 89.7(6) . . ?
C3 C1A C2 107.2(5) . . ?
C2A C2 N1 84.4(7) . . ?
C2A C2 C4 91.7(7) . . ?
N1 C2 C4 127.1(6) . . ?
C2A C2 C4A 56.2(6) . . ?
N1 C2 C4A 118.2(6) . . ?
C4 C2 C4A 35.6(4) . . ?
C2A C2 C1A 110.1(7) . . ?
N1 C2 C1A 42.6(4) . . ?
C4 C2 C1A 91.8(5) . . ?
C4A C2 C1A 105.1(5) . . ?
C2 C2A C4A 88.0(7) . . ?
C2 C2A N1 55.2(5) . . ?
C4A C2A N1 120.2(6) . . ?
C2 C2A C4 53.8(6) . . ?
C4A C2A C4 34.3(4) . . ?
N1 C2A C4 93.6(5) . . ?
C3A C3 C1 91.8(8) . . ?
C3A C3 C5 48.4(6) . . ?
C1 C3 C5 115.0(6) . . ?
C3A C3 C1A 60.7(7) . . ?
C1 C3 C1A 31.2(4) . . ?
C5 C3 C1A 92.9(6) . . ?
C3 C3A C5 98.0(9) . . ?
C3 C3A C1A 85.9(9) . . ?
C5 C3A C1A 125.3(7) . . ?
C3 C3A C1 56.5(7) . . ?
C5 C3A C1 121.3(7) . . ?
C1A C3A C1 29.6(4) . . ?
C3 C3A C4 121.9(9) . . ?
C5 C3A C4 42.7(4) . . ?
C1A C3A C4 89.6(6) . . ?
C1 C3A C4 102.9(5) . . ?
C4A C4 C5 92.6(8) . . ?
C4A C4 C2 88.0(7) . . ?
C5 C4 C2 123.9(6) . . ?
C4A C4 C2A 53.5(6) . . ?
C5 C4 C2A 116.3(6) . . ?
C2 C4 C2A 34.6(4) . . ?
C4A C4 C3A 114.7(8) . . ?
C5 C4 C3A 41.2(4) . . ?
C2 C4 C3A 88.8(5) . . ?
C2A C4 C3A 100.8(5) . . ?
C4 C4A C2A 92.2(7) . . ?
C4 C4A C5 50.2(5) . . ?
C2A C4A C5 115.1(6) . . ?
C4 C4A C2 56.4(6) . . ?
C2A C4A C2 35.9(4) . . ?
C5 C4A C2 90.2(5) . . ?
C3A C5 C4 96.1(6) . . ?
C3A C5 C5 127.7(4) . 2_655 ?
C4 C5 C5 123.9(4) . 2_655 ?
C3A C5 C3 33.6(5) . . ?
C4 C5 C3 116.0(5) . . ?
C5 C5 C3 119.7(3) 2_655 . ?
C3A C5 C4A 115.8(5) . . ?
C4 C5 C4A 37.2(5) . . ?
C5 C5 C4A 116.3(3) 2_655 . ?
C3 C5 C4A 114.7(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
Co1 F1 2.0244(17) 6_566 ?
Co1 O2 2.058(2) 7 ?
Co1 F1 2.0861(17) . ?
Co1 O4 2.121(2) 4 ?
Co1 O1 2.129(2) . ?
Co1 N1 2.149(3) . ?
Co1 Co2 2.8726(4) . ?
Co2 O4 2.072(2) 4 ?
Co2 O4 2.072(2) 6_565 ?
Co2 O1 2.072(2) 7_565 ?
Co2 O1 2.072(2) . ?
Co2 F1 2.1177(17) . ?
Co2 F1 2.1177(16) 7_565 ?
Co2 Co1 2.8726(4) 7_565 ?
P1 O2 1.518(2) . ?
P1 O1 1.520(2) . ?
P1 O4 1.525(2) . ?
P1 O3 1.589(2) . ?
F1 Co1 2.0244(17) 6_565 ?
O2 Co1 2.058(2) 7 ?
O4 Co2 2.072(2) 4_545 ?
O4 Co1 2.121(2) 4_545 ?
N1 C1A 1.200(8) . ?
N1 C2 1.237(7) . ?
N1 C1 1.460(8) . ?
N1 C2A 1.499(8) . ?
C1 C1A 0.834(10) . ?
C1 C3 1.404(9) . ?
C1 C3A 1.684(11) . ?
C1A C3A 1.407(10) . ?
C1A C3 1.609(11) . ?
C1A C2 1.770(11) . ?
C2 C2A 0.976(10) . ?
C2 C4 1.389(9) . ?
C2 C4A 1.665(10) . ?
C2A C4A 1.384(9) . ?
C2A C4 1.721(10) . ?
C3 C3A 0.886(10) . ?
C3 C5 1.584(9) . ?
C3A C5 1.197(9) . ?
C3A C4 1.807(12) . ?
C4 C4A 0.969(10) . ?
C4 C5 1.232(8) . ?
C4A C5 1.602(9) . ?
C5 C5 1.473(8) 2_655 ?
