#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:35:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179147 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/08/4310849.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_4310849
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(C4H4N2)(HPO4)2F2]'
_chemical_formula_sum            'C4 H6 Co3 F2 N2 O8 P2'
_chemical_formula_weight         486.84
_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                 103.753(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.809(4)
_cell_length_b                   7.3695(13)
_cell_length_c                   7.3954(13)
_cell_measurement_temperature    293(2)
_cell_volume                     1154.5(4)
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXTL programs, version 5.1'
_computing_structure_solution    'SHELXTL programs, version 5.1'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0933
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3591
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    4.609
_exptl_absorpt_correction_type   'empirical based on symmetry equivalents'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.801
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.437
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.224
_refine_ls_extinction_coef       0.0007(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0534
_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)+(0.0523P)²+14.2201P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1378
_reflns_number_gt                1252
_reflns_number_total             1402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0353460si20031120_081115_1.cif
_cod_data_source_block           cfp02m
_cod_database_code               4310849
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 0.2500 0.2500 0.0000 0.0125(3) Uani 1 2 d S . .
Co2 Co 0.16696(4) 0.52273(10) 0.07944(10) 0.0129(2) Uani 1 1 d . . .
P1 P 0.32288(7) 0.6266(2) 0.17689(18) 0.0116(3) Uani 1 1 d . . .
O1 O 0.2653(2) 0.5110(6) 0.1009(6) 0.0173(9) Uani 1 1 d . . .
O2 O 0.3466(2) 0.7233(6) 0.0266(5) 0.0172(9) Uani 1 1 d . . .
O3 O 0.3784(2) 0.4955(7) 0.2718(6) 0.0236(10) Uani 1 1 d . . .
O4 O 0.3107(2) 0.7575(6) 0.3242(5) 0.0173(9) Uani 1 1 d . . .
F1 F 0.32911(16) 0.1159(5) 0.1628(4) 0.0161(7) Uani 1 1 d . . .
N1 N 0.0658(3) 0.5063(8) 0.0331(8) 0.0225(11) Uani 1 1 d . . .
C1 C 0.0310(6) 0.644(2) 0.079(2) 0.028(3) Uani 0.50 1 d P . .
C1A C 0.0302(7) 0.651(2) -0.038(2) 0.028(3) Uani 0.50 1 d P . .
C2 C 0.0361(7) 0.356(2) 0.060(3) 0.029(3) Uani 0.50 1 d P . .
C2A C 0.0351(7) 0.360(2) -0.044(2) 0.027(3) Uani 0.50 1 d P . .
H3O H 0.4233 0.5232 0.3149 0.050 Uiso 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
O1 Co1 O1 180.0(3) . 7 ?
O1 Co1 O4 100.35(18) . 6_565 ?
O1 Co1 O4 79.65(18) 7 6_565 ?
O1 Co1 O4 79.65(18) . 4_545 ?
O1 Co1 O4 100.35(18) 7 4_545 ?
O4 Co1 O4 180.00(15) 6_565 4_545 ?
O1 Co1 F1 79.00(15) . 7 ?
O1 Co1 F1 101.00(16) 7 7 ?
O4 Co1 F1 102.33(15) 6_565 7 ?
O4 Co1 F1 77.67(15) 4_545 7 ?
O1 Co1 F1 101.00(15) . . ?
O1 Co1 F1 79.00(15) 7 . ?
O4 Co1 F1 77.67(15) 6_565 . ?
O4 Co1 F1 102.33(15) 4_545 . ?
F1 Co1 F1 180.0(3) 7 . ?
O1 Co1 Co2 132.39(13) . 7 ?
O1 Co1 Co2 47.61(13) 7 7 ?
O4 Co1 Co2 47.12(12) 6_565 7 ?
O4 Co1 Co2 132.88(12) 4_545 7 ?
F1 Co1 Co2 133.39(9) 7 7 ?
F1 Co1 Co2 46.61(9) . 7 ?
O1 Co1 Co2 47.61(13) . . ?
O1 Co1 Co2 132.39(13) 7 . ?
O4 Co1 Co2 132.88(12) 6_565 . ?
O4 Co1 Co2 47.12(12) 4_545 . ?
F1 Co1 Co2 46.61(9) 7 . ?
F1 Co1 Co2 133.39(9) . . ?
Co2 Co1 Co2 180.00(2) 7 . ?
F1 Co2 O2 91.18(15) 4 7_565 ?
F1 Co2 F1 169.50(11) 4 7 ?
O2 Co2 F1 98.79(14) 7_565 7 ?
F1 Co2 O4 92.41(15) 4 4_545 ?
O2 Co2 O4 173.80(16) 7_565 4_545 ?
F1 Co2 O4 77.37(14) 7 4_545 ?
F1 Co2 O1 97.43(16) 4 . ?
O2 Co2 O1 96.86(17) 7_565 . ?
F1 Co2 O1 78.22(16) 7 . ?
O4 Co2 O1 77.67(16) 4_545 . ?
F1 Co2 N1 88.92(18) 4 . ?
O2 Co2 N1 86.6(2) 7_565 . ?
F1 Co2 N1 94.91(18) 7 . ?
O4 Co2 N1 98.54(19) 4_545 . ?
O1 Co2 N1 172.69(19) . . ?
F1 Co2 Co1 123.32(10) 4 . ?
O2 Co2 Co1 127.76(12) 7_565 . ?
F1 Co2 Co1 47.18(9) 7 . ?
O4 Co2 Co1 46.14(11) 4_545 . ?
O1 Co2 Co1 46.03(11) . . ?
N1 Co2 Co1 127.06(16) . . ?
O1 P1 O2 113.1(3) . . ?
O1 P1 O4 110.6(2) . . ?
O2 P1 O4 112.1(2) . . ?
O1 P1 O3 107.6(3) . . ?
O2 P1 O3 104.8(2) . . ?
O4 P1 O3 108.4(3) . . ?
P1 O1 Co1 135.2(3) . . ?
P1 O1 Co2 138.0(3) . . ?
Co1 O1 Co2 86.36(16) . . ?
P1 O2 Co2 132.6(3) . 7_565 ?
P1 O3 H3O 128.4(4) . . ?
P1 O4 Co1 132.8(3) . 4 ?
P1 O4 Co2 140.0(3) . 4 ?
Co1 O4 Co2 86.74(15) 4 4 ?
Co2 F1 Co2 130.37(18) 4_545 7 ?
Co2 F1 Co1 123.26(17) 4_545 . ?
Co2 F1 Co1 86.21(11) 7 . ?
C2 N1 C2A 33.7(8) . . ?
C2 N1 C1A 117.5(10) . . ?
C2A N1 C1A 106.8(10) . . ?
C2 N1 C1 105.3(11) . . ?
C2A N1 C1 117.5(10) . . ?
C1A N1 C1 37.2(8) . . ?
C2 N1 Co2 123.0(7) . . ?
C2A N1 Co2 120.5(7) . . ?
C1A N1 Co2 119.4(7) . . ?
C1 N1 Co2 122.0(7) . . ?
C1A C1 N1 70.7(15) . . ?
C1A C1 C2A 92.5(17) . 5_565 ?
N1 C1 C2A 123.3(12) . 5_565 ?
C1A C1 C2 63.4(15) . 5_565 ?
N1 C1 C2 108.8(12) . 5_565 ?
C2A C1 C2 29.1(8) 5_565 5_565 ?
C1 C1A N1 72.0(15) . . ?
C1 C1A C2 83.6(16) . 5_565 ?
N1 C1A C2 119.5(12) . 5_565 ?
C1 C1A C2A 56.6(13) . 5_565 ?
N1 C1A C2A 106.3(11) . 5_565 ?
C2 C1A C2A 27.0(8) 5_565 5_565 ?
C2A C2 N1 73.4(17) . . ?
C2A C2 C1A 95.9(19) . 5_565 ?
N1 C2 C1A 122.5(13) . 5_565 ?
C2A C2 C1 62.9(16) . 5_565 ?
N1 C2 C1 108.4(12) . 5_565 ?
C1A C2 C1 33.0(8) 5_565 5_565 ?
C2 C2A N1 72.9(16) . . ?
C2 C2A C1 88.0(18) . 5_565 ?
N1 C2A C1 119.3(13) . 5_565 ?
C2 C2A C1A 57.1(16) . 5_565 ?
N1 C2A C1A 105.5(11) . 5_565 ?
C1 C2A C1A 30.9(8) 5_565 5_565 ?
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 O1 2.061(4) . ?
Co1 O1 2.061(4) 7 ?
Co1 O4 2.064(4) 6_565 ?
Co1 O4 2.064(4) 4_545 ?
Co1 F1 2.101(3) 7 ?
Co1 F1 2.101(3) . ?
Co1 Co2 2.8583(9) 7 ?
Co1 Co2 2.8583(9) . ?
Co2 F1 2.009(3) 4 ?
Co2 O2 2.024(4) 7_565 ?
Co2 F1 2.082(3) 7 ?
Co2 O4 2.098(4) 4_545 ?
Co2 O1 2.115(5) . ?
Co2 N1 2.154(6) . ?
P1 O1 1.510(4) . ?
P1 O2 1.512(4) . ?
P1 O4 1.525(4) . ?
P1 O3 1.577(5) . ?
O2 Co2 2.024(4) 7_565 ?
O3 H3O 0.977(5) . ?
O4 Co1 2.064(4) 4 ?
O4 Co2 2.098(4) 4 ?
F1 Co2 2.009(3) 4_545 ?
F1 Co2 2.082(3) 7 ?
N1 C2 1.321(15) . ?
N1 C2A 1.324(16) . ?
N1 C1A 1.348(16) . ?
N1 C1 1.358(16) . ?
C1 C1A 0.864(19) . ?
C1 C2A 1.404(19) 5_565 ?
C1 C2 1.58(2) 5_565 ?
C1A C2 1.42(2) 5_565 ?
C1A C2A 1.68(2) 5_565 ?
C2 C2A 0.767(18) . ?
C2 C1A 1.42(2) 5_565 ?
C2 C1 1.58(2) 5_565 ?
C2A C1 1.404(19) 5_565 ?
C2A C1A 1.68(2) 5_565 ?
