#============================================================================== 

data_New_Global_Publ_Block

# Added by publCIF - use a unique identifier for each data block

#==============================================================================


# SUBMISSION DETAILS

_publ_contact_author_name            
'Mark T Weller'   # Name of author for correspondence
_publ_contact_author_address             # Address of author for correspondence

;
School of Chemistry
University of Southampton
Southampton
SO17 1BJ
UK
;

_publ_contact_author_email           'mtw@soton.ac.uk'
_publ_contact_author_fax             ?
_publ_contact_author_phone           ?

_publ_contact_letter
;
Please consider this CIF for publication. I certify that this contibution is the
original work of those listed as authors; that it has not been published
before (in any language or medium) and is not being considered for publication
elsewhere; that all authors concur with and are aware of the submission; that
all workers involved in the study are listed as authors or given proper credit
in the acknowledgements; that I have obtained permission for and acknowledged
the source of any excerpts from other copyright works; and that to the best of
my knowledge the paper contains no statements which are libellous, unlawful or
in any way actionable. All coauthors have made significant scientific
contributions to the work reported, including the ideas and their execution,
and share responsibility and accountability for the results.
;
   
_publ_requested_journal              'Dalton Transactions'
_publ_requested_category             ?   

#==============================================================================

# TITLE AND AUTHOR LIST

_publ_section_title
;
Cobalt(II) fluorophosphate frameworks
;
_publ_section_title_footnote  # remove if not required
; ?
;         
 
# The loop structure below should contain the names and addresses of all 
# authors, in the required order of publication. Repeat as necessary.

# NB if using publCIF, the Author database tool might prove useful
# (see the Tools menu in publCIF)

loop_
_publ_author_name
_publ_author_address
_publ_author_footnote
_publ_author_email
'Armstrong, Jennifer A'
;
School of Chemistry
University of Southampton
Southampton
SO17 1BJ
UK
;
;
?
;
.
'Williams, Edward R'
;
School of Chemistry
University of Southampton
Southampton
SO17 1BJ
UK
;
.
.
'Weller, Mark T'
;
School of Chemistry
University of Southampton
Southampton
SO17 1BJ
UK
;
.
;
mtw@soton.ac.uk
;



#==============================================================================

# TEXT

_publ_section_synopsis
;
?
;
_publ_section_abstract
;
?
;
_publ_section_comment
;
?
;
_publ_section_acknowledgements 	# remove if not required
;
?
;
_publ_section_references
;
?
;
_publ_section_figure_captions
;
?
;
_publ_section_exptl_prep
;
?
;
_publ_section_exptl_refinement
;
?
;
#==============================================================================


data_2010jaa0055

_audit_update_record
;
2012-06-08 # Formatted by publCIF
;
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Co3 F2 H4 K O12 P3'
_chemical_formula_weight          542.83
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 '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'
 'K'  'K'   0.2009   0.2494
 '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'
 'F'  'F'   0.0171   0.0103
 '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'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    C2/c
 
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'
 
_cell_length_a                    19.987(2)
_cell_length_b                    7.4105(7)
_cell_length_c                    7.4952(8)
_cell_angle_alpha                 90.00
_cell_angle_beta                  102.129(6)
_cell_angle_gamma                 90.00
_cell_volume                      1085.39(19)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     11845
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        plate
_exptl_crystal_colour             purple
_exptl_crystal_size_max           0.02
_exptl_crystal_size_mid           0.01
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.322
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              558
_exptl_absorpt_coefficient_mu     5.456
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9407
_exptl_absorpt_correction_T_max   0.9697
_exptl_absorpt_process_details    ?
 
_exptl_special_details
?
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode' 
_diffrn_radiation_monochromator   '10cm confocal mirrors'
_diffrn_measurement_device_type   'Bruker-Nonius APEX II CCD camera on κ-goniostat' 
_diffrn_measurement_method        'φ & ω scans'
_diffrn_detector_area_resol_mean  '4096x4096pixels / 62x62mm'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             4987
_diffrn_reflns_av_R_equivalents   0.0801
_diffrn_reflns_av_sigmaI/netI     0.0698
_diffrn_reflns_limit_h_min        -25
_diffrn_reflns_limit_h_max        25
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        7
_diffrn_reflns_theta_min          2.94
_diffrn_reflns_theta_max          27.55
_reflns_number_total              1247
_reflns_number_gt                 1016
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0001P)²+48.1408P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          1247
_refine_ls_number_parameters      106
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0831
_refine_ls_R_factor_gt            0.0624
_refine_ls_wR_factor_ref          0.1309
_refine_ls_wR_factor_gt           0.1206
_refine_ls_goodness_of_fit_ref    1.098
_refine_ls_restrained_S_all       1.098
_refine_ls_shift/su_max           0.025
_refine_ls_shift/su_mean          0.002
 
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
F1 F 0.1607(2) 0.6350(6) 0.0541(6) 0.0114(9) Uani 1 1 d . . .
O4 O 0.2370(3) 0.0234(7) 0.0636(7) 0.0106(11) Uani 1 1 d . . .
O1 O 0.1181(3) 0.0012(7) 0.1252(7) 0.0108(11) Uani 1 1 d . . .
O2 O 0.1415(3) 0.2257(7) -0.0973(7) 0.0115(11) Uani 1 1 d . . .
O3 O 0.1929(3) 0.2684(7) 0.2391(7) 0.0115(11) Uani 1 1 d . . .
O11 O 0.0580(3) 0.4832(8) 0.2074(7) 0.0136(12) Uani 1 1 d . . .
O10 O 0.0294(3) 0.2389(8) 0.4089(8) 0.0145(12) Uani 1 1 d . . .
H1 H 0.076(6) 0.269(15) 0.461(15) 0.04(3) Uiso 1 1 d . . .
H2 H 0.025(10) 0.13(3) 0.39(2) 0.12(7) Uiso 1 1 d . . .
Co1 Co 0.2500 0.2500 0.5000 0.0094(3) Uani 1 2 d S . .
Co2 Co 0.15856(5) 0.52173(14) 0.30861(14) 0.0095(3) Uani 1 1 d . . .
P1 P 0.17455(10) 0.1347(3) 0.0821(3) 0.0096(4) Uani 1 1 d . . .
P2 P 0.0000 0.3755(4) 0.2500 0.0099(6) Uani 1 2 d S . .
K5 K 0.0000 0.8598(4) 0.2500 0.0169(5) Uani 1 2 d S . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
 
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
F1 Co2 2.092(4) . ?
F1 Co1 2.094(4) 4 ?
F1 Co2 2.169(4) 6_565 ?
O4 P1 1.527(6) . ?
O4 Co2 2.106(5) 4_545 ?
O4 Co1 2.110(5) 4_545 ?
O1 P1 1.585(5) . ?
O1 K5 2.910(5) 1_545 ?
O1 K5 3.428(5) 5_565 ?
O2 P1 1.525(5) . ?
O2 Co2 2.054(5) 6_565 ?
O2 K5 2.889(5) 5_565 ?
O3 P1 1.523(6) . ?
O3 Co1 2.051(5) . ?
O3 Co2 2.102(5) . ?
O11 P2 1.496(6) . ?
O11 Co2 2.015(5) . ?
O11 K5 3.064(6) . ?
O10 P2 1.579(6) . ?
O10 K5 2.837(6) 5_566 ?
O10 K5 3.060(7) 1_545 ?
Co1 O3 2.051(5) 7_556 ?
Co1 F1 2.094(4) 4_545 ?
Co1 F1 2.094(4) 6_566 ?
Co1 O4 2.110(5) 4 ?
Co1 O4 2.110(5) 6_556 ?
Co1 Co2 2.8899(11) . ?
Co1 Co2 2.8899(11) 7_556 ?
Co2 O2 2.054(5) 6_566 ?
Co2 O4 2.106(5) 4 ?
Co2 F1 2.169(4) 6_566 ?
Co2 K5 3.991(2) . ?
P1 K5 3.8367(19) 5_565 ?
P2 O11 1.496(6) 2 ?
P2 O10 1.579(6) 2 ?
P2 K5 3.590(4) . ?
P2 K5 3.821(4) 1_545 ?
K5 O10 2.837(6) 5_566 ?
K5 O10 2.837(6) 6_565 ?
K5 O2 2.889(5) 5_565 ?
K5 O2 2.889(5) 6_566 ?
K5 O1 2.910(5) 1_565 ?
K5 O1 2.910(5) 2_565 ?
K5 O10 3.060(7) 1_565 ?
K5 O10 3.060(7) 2_565 ?
K5 O11 3.064(6) 2 ?
K5 O1 3.428(5) 6_566 ?
K5 O1 3.428(5) 5_565 ?
 
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
Co2 F1 Co1 121.4(2) . 4 ?
Co2 F1 Co2 123.9(2) . 6_565 ?
Co1 F1 Co2 85.35(16) 4 6_565 ?
P1 O4 Co2 135.5(3) . 4_545 ?
P1 O4 Co1 133.0(3) . 4_545 ?
Co2 O4 Co1 86.5(2) 4_545 4_545 ?
P1 O1 K5 162.0(3) . 1_545 ?
P1 O1 K5 92.4(2) . 5_565 ?
K5 O1 K5 84.66(13) 1_545 5_565 ?
P1 O2 Co2 129.3(3) . 6_565 ?
P1 O2 K5 117.3(3) . 5_565 ?
Co2 O2 K5 106.5(2) 6_565 5_565 ?
P1 O3 Co1 133.5(3) . . ?
P1 O3 Co2 137.2(3) . . ?
Co1 O3 Co2 88.2(2) . . ?
P2 O11 Co2 138.7(3) . . ?
P2 O11 K5 97.9(3) . . ?
Co2 O11 K5 101.6(2) . . ?
P2 O10 K5 136.9(3) . 5_566 ?
P2 O10 K5 106.5(3) . 1_545 ?
K5 O10 K5 93.13(18) 5_566 1_545 ?
O3 Co1 O3 180.000(1) . 7_556 ?
O3 Co1 F1 99.71(19) . 4_545 ?
O3 Co1 F1 80.29(19) 7_556 4_545 ?
O3 Co1 F1 80.29(19) . 6_566 ?
O3 Co1 F1 99.71(19) 7_556 6_566 ?
F1 Co1 F1 180.00(11) 4_545 6_566 ?
O3 Co1 O4 77.9(2) . 4 ?
O3 Co1 O4 102.1(2) 7_556 4 ?
F1 Co1 O4 101.33(19) 4_545 4 ?
F1 Co1 O4 78.67(19) 6_566 4 ?
O3 Co1 O4 102.1(2) . 6_556 ?
O3 Co1 O4 77.9(2) 7_556 6_556 ?
F1 Co1 O4 78.67(19) 4_545 6_556 ?
F1 Co1 O4 101.33(19) 6_566 6_556 ?
O4 Co1 O4 180.0 4 6_556 ?
O3 Co1 Co2 46.63(15) . . ?
O3 Co1 Co2 133.37(15) 7_556 . ?
F1 Co1 Co2 131.58(12) 4_545 . ?
F1 Co1 Co2 48.42(12) 6_566 . ?
O4 Co1 Co2 46.67(14) 4 . ?
O4 Co1 Co2 133.33(14) 6_556 . ?
O3 Co1 Co2 133.37(15) . 7_556 ?
O3 Co1 Co2 46.63(15) 7_556 7_556 ?
F1 Co1 Co2 48.42(12) 4_545 7_556 ?
F1 Co1 Co2 131.58(12) 6_566 7_556 ?
O4 Co1 Co2 133.33(14) 4 7_556 ?
O4 Co1 Co2 46.67(14) 6_556 7_556 ?
Co2 Co1 Co2 180.00(4) . 7_556 ?
O11 Co2 O2 91.9(2) . 6_566 ?
O11 Co2 F1 85.6(2) . . ?
O2 Co2 F1 89.1(2) 6_566 . ?
O11 Co2 O3 97.6(2) . . ?
O2 Co2 O3 170.3(2) 6_566 . ?
F1 Co2 O3 93.56(19) . . ?
O11 Co2 O4 171.0(2) . 4 ?
O2 Co2 O4 93.4(2) 6_566 4 ?
F1 Co2 O4 101.79(19) . 4 ?
O3 Co2 O4 76.9(2) . 4 ?
O11 Co2 F1 94.8(2) . 6_566 ?
O2 Co2 F1 99.88(19) 6_566 6_566 ?
F1 Co2 F1 171.00(13) . 6_566 ?
O3 Co2 F1 77.47(19) . 6_566 ?
O4 Co2 F1 77.10(19) 4 6_566 ?
O11 Co2 Co1 124.42(16) . . ?
O2 Co2 Co1 126.73(15) 6_566 . ?
F1 Co2 Co1 126.89(13) . . ?
O3 Co2 Co1 45.19(14) . . ?
O4 Co2 Co1 46.78(14) 4 . ?
F1 Co2 Co1 46.24(11) 6_566 . ?
O11 Co2 K5 48.76(17) . . ?
O2 Co2 K5 43.96(15) 6_566 . ?
F1 Co2 K5 79.36(13) . . ?
O3 Co2 K5 145.76(15) . . ?
O4 Co2 K5 137.29(15) 4 . ?
F1 Co2 K5 107.63(12) 6_566 . ?
Co1 Co2 K5 153.74(4) . . ?
O3 P1 O2 112.5(3) . . ?
O3 P1 O4 110.7(3) . . ?
O2 P1 O4 111.7(3) . . ?
O3 P1 O1 108.4(3) . . ?
O2 P1 O1 105.1(3) . . ?
O4 P1 O1 108.2(3) . . ?
O3 P1 K5 122.2(2) . 5_565 ?
O2 P1 K5 42.0(2) . 5_565 ?
O4 P1 K5 126.6(2) . 5_565 ?
O1 P1 K5 63.2(2) . 5_565 ?
O11 P2 O11 115.4(5) . 2 ?
O11 P2 O10 111.3(3) . 2 ?
O11 P2 O10 108.7(3) 2 2 ?
O11 P2 O10 108.7(3) . . ?
O11 P2 O10 111.3(3) 2 . ?
O10 P2 O10 100.3(5) 2 . ?
O11 P2 K5 57.7(2) . . ?
O11 P2 K5 57.7(2) 2 . ?
O10 P2 K5 129.8(2) 2 . ?
O10 P2 K5 129.8(2) . . ?
O11 P2 K5 122.3(2) . 1_545 ?
O11 P2 K5 122.3(2) 2 1_545 ?
O10 P2 K5 50.2(2) 2 1_545 ?
O10 P2 K5 50.2(2) . 1_545 ?
K5 P2 K5 180.0 . 1_545 ?
O10 K5 O10 150.1(3) 5_566 6_565 ?
O10 K5 O2 85.96(17) 5_566 5_565 ?
O10 K5 O2 87.55(16) 6_565 5_565 ?
O10 K5 O2 87.55(17) 5_566 6_566 ?
O10 K5 O2 85.96(17) 6_565 6_566 ?
O2 K5 O2 154.6(2) 5_565 6_566 ?
O10 K5 O1 135.90(17) 5_566 1_565 ?
O10 K5 O1 57.84(16) 6_565 1_565 ?
O2 K5 O1 138.07(15) 5_565 1_565 ?
O2 K5 O1 54.14(15) 6_566 1_565 ?
O10 K5 O1 57.84(16) 5_566 2_565 ?
O10 K5 O1 135.90(16) 6_565 2_565 ?
O2 K5 O1 54.14(15) 5_565 2_565 ?
O2 K5 O1 138.07(15) 6_566 2_565 ?
O1 K5 O1 137.8(2) 1_565 2_565 ?
O10 K5 O10 86.87(18) 5_566 1_565 ?
O10 K5 O10 121.90(18) 6_565 1_565 ?
O2 K5 O10 116.60(17) 5_565 1_565 ?
O2 K5 O10 87.44(16) 6_566 1_565 ?
O1 K5 O10 72.06(16) 1_565 1_565 ?
O1 K5 O10 69.32(16) 2_565 1_565 ?
O10 K5 O10 121.90(18) 5_566 2_565 ?
O10 K5 O10 86.87(18) 6_565 2_565 ?
O2 K5 O10 87.44(16) 5_565 2_565 ?
O2 K5 O10 116.60(17) 6_566 2_565 ?
O1 K5 O10 69.32(16) 1_565 2_565 ?
O1 K5 O10 72.06(16) 2_565 2_565 ?
O10 K5 O10 46.7(2) 1_565 2_565 ?
O10 K5 O11 61.10(17) 5_566 2 ?
O10 K5 O11 90.76(17) 6_565 2 ?
O2 K5 O11 58.76(15) 5_565 2 ?
O2 K5 O11 96.82(16) 6_566 2 ?
O1 K5 O11 135.34(16) 1_565 2 ?
O1 K5 O11 86.82(15) 2_565 2 ?
O10 K5 O11 147.32(15) 1_565 2 ?
O10 K5 O11 146.19(15) 2_565 2 ?
O10 K5 O11 90.76(17) 5_566 . ?
O10 K5 O11 61.10(17) 6_565 . ?
O2 K5 O11 96.82(16) 5_565 . ?
O2 K5 O11 58.76(15) 6_566 . ?
O1 K5 O11 86.82(15) 1_565 . ?
O1 K5 O11 135.34(16) 2_565 . ?
O10 K5 O11 146.19(15) 1_565 . ?
O10 K5 O11 147.32(15) 2_565 . ?
O11 K5 O11 48.8(2) 2 . ?
O10 K5 O1 64.87(15) 5_566 6_566 ?
O10 K5 O1 125.42(15) 6_565 6_566 ?
O2 K5 O1 147.00(14) 5_565 6_566 ?
O2 K5 O1 45.03(13) 6_566 6_566 ?
O1 K5 O1 71.98(10) 1_565 6_566 ?
O1 K5 O1 95.34(13) 2_565 6_566 ?
O10 K5 O1 50.35(14) 1_565 6_566 ?
O10 K5 O1 94.96(15) 2_565 6_566 ?
O11 K5 O1 113.47(14) 2 6_566 ?
O11 K5 O1 98.56(14) . 6_566 ?
O10 K5 O1 125.42(15) 5_566 5_565 ?
O10 K5 O1 64.87(15) 6_565 5_565 ?
O2 K5 O1 45.03(14) 5_565 5_565 ?
O2 K5 O1 147.00(14) 6_566 5_565 ?
O1 K5 O1 95.34(13) 1_565 5_565 ?
O1 K5 O1 71.98(10) 2_565 5_565 ?
O10 K5 O1 94.96(15) 1_565 5_565 ?
O10 K5 O1 50.35(14) 2_565 5_565 ?
O11 K5 O1 98.56(14) 2 5_565 ?
O11 K5 O1 113.47(14) . 5_565 ?
O1 K5 O1 145.04(19) 6_566 5_565 ?
 
_diffrn_measured_fraction_theta_max    0.992
_diffrn_reflns_theta_full              27.55
_diffrn_measured_fraction_theta_full   0.992
_refine_diff_density_max    1.105
_refine_diff_density_min   -0.959
_refine_diff_density_rms    0.265

