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

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_jco209_mk1

_audit_update_record
;
2012-07-12 # Formatted by publCIF
;
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C4 H12 Co3 F6 N3 O8 P2'
_chemical_formula_weight          582.90
 
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'
 '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'
 'Cu'  'Cu'   0.3201   1.2651
 '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'
 '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    P21/c
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    10.335(7)
_cell_length_b                    10.772(7)
_cell_length_c                    7.353(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  100.180(13)
_cell_angle_gamma                 90.00
_cell_volume                      805.7(9)
_cell_formula_units_Z             2
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     1447
_cell_measurement_theta_min       2.8
_cell_measurement_theta_max       27.5
 
_exptl_crystal_description        needle
_exptl_crystal_colour             purple
_exptl_crystal_size_max           0.30
_exptl_crystal_size_mid           0.05
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.369
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              556
_exptl_absorpt_coefficient_mu     3.358
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.4324
_exptl_absorpt_correction_T_max   0.8501
_exptl_absorpt_process_details    ?
 
_exptl_special_details
?
_diffrn_special_details
?
_diffrn_ambient_temperature             100(2)
_diffrn_source_power                    2.5
_diffrn_source_voltage                  45.0
_diffrn_source_current                  55.0
_diffrn_radiation_wavelength            0.71075
_diffrn_radiation_type                  'Mo K\a'
_diffrn_source                          'Rotating Anode'
_diffrn_radiation_monochromator         'Confocal'
_diffrn_measurement_specimen_support    'Mitegen'
_diffrn_detector                        'CCD'
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean        28.5714
_diffrn_measurement_method              'profile data from ω-scans'
_diffrn_reflns_number                   4344
_diffrn_reflns_av_R_equivalents         0.086
_diffrn_reflns_av_unetI/netI            0.128
_diffrn_reflns_theta_full               27.5
_diffrn_measured_fraction_theta_max     0.991
_diffrn_measured_fraction_theta_full    0.991
_diffrn_reflns_theta_min                2.8
_diffrn_reflns_theta_max                27.5
_diffrn_reflns_limit_h_min              -9
_diffrn_reflns_limit_h_max              9
_diffrn_reflns_limit_k_min              -13
_diffrn_reflns_limit_k_max              13
_diffrn_reflns_limit_l_min              -8
_diffrn_reflns_limit_l_max              13
_diffrn_measurement_details
;
scan:
	Number of images: 105
	           Slice: -88.0000 - 17.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -70.0000
	             Phi: 135.0000
	             XTD: 45.0371
	          2theta: -20.0790
scan:
	Number of images: 82
	           Slice: -74.0000 - 8.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -60.0000
	             Phi: 315.0000
	             XTD: 45.0371
	          2theta: -20.0790
scan:
	Number of images: 45
	           Slice: -110.0000 - -65.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -15.0000
	             Phi: 270.0000
	             XTD: 45.0371
	          2theta: -20.0790

;
_diffrn_orient_matrix_UB_11             0.078682
_diffrn_orient_matrix_UB_12             -0.113586
_diffrn_orient_matrix_UB_13             0.000747
_diffrn_orient_matrix_UB_21             -0.012695
_diffrn_orient_matrix_UB_22             -0.009395
_diffrn_orient_matrix_UB_23             -0.091479
_diffrn_orient_matrix_UB_31             0.088326
_diffrn_orient_matrix_UB_32             0.039940
_diffrn_orient_matrix_UB_33             -0.016359
_diffrn_orient_matrix_type              'd*Trek' 

_reflns_number_total              1828
_reflns_number_gt                 1292
_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)+(0.1937P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          1828
_refine_ls_number_parameters      103
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1628
_refine_ls_R_factor_gt            0.1243
_refine_ls_wR_factor_ref          0.3545
_refine_ls_wR_factor_gt           0.3141
_refine_ls_goodness_of_fit_ref    1.110
_refine_ls_restrained_S_all       1.110
_refine_ls_shift/su_max           0.048
_refine_ls_shift/su_mean          0.007
 
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
F2 F 0.4278(7) 0.6375(7) 0.1380(10) 0.0163(16) Uani 1 1 d . . .
F3 F 0.5234(7) 0.3879(7) 0.2212(10) 0.0153(16) Uiso 1 1 d . . .
F1 F 0.5957(6) 0.8288(7) -0.0209(9) 0.0120(15) Uiso 1 1 d . . .
O1 O 0.7635(8) 0.8473(8) 0.3257(13) 0.0157(19) Uani 1 1 d . . .
O4 O 0.3139(8) 0.4088(8) -0.1186(12) 0.0148(18) Uani 1 1 d . . .
O2 O 0.8849(9) 1.0118(10) 0.5299(13) 0.023(2) Uani 1 1 d . . .
O3 O 0.8958(9) 0.7920(10) 0.6334(13) 0.024(2) Uani 1 1 d . . .
N1 N 0.6693(10) 0.0608(10) 0.0536(16) 0.020(2) Uani 1 1 d . . .
H1A H 0.6685 -0.0188 0.0209 0.030 Uiso 1 1 calc R . .
H1B H 0.6173 0.1039 -0.0334 0.030 Uiso 1 1 calc R . .
H1C H 0.6404 0.0680 0.1602 0.030 Uiso 1 1 calc R . .
C2 C 0.8072(16) 0.1102(16) 0.076(2) 0.033(4) Uiso 1 1 d . . .
N2 N 0.802(2) 0.243(2) 0.322(3) 0.021(5) Uiso 0.50 1 d P . .
H2A H 0.7151 0.2382 0.3211 0.025 Uiso 0.50 1 calc PR . .
H2B H 0.8402 0.1791 0.3903 0.025 Uiso 0.50 1 calc PR . .
C4 C 0.826(2) 0.227(2) 0.124(3) 0.009(4) Uiso 0.50 1 d P . .
H4A H 0.7661 0.2790 0.0411 0.011 Uiso 0.50 1 calc PR . .
H4B H 0.9152 0.2509 0.1163 0.011 Uiso 0.50 1 calc PR . .
C5 C 0.850(4) 0.142(3) -0.085(4) 0.029(7) Uani 0.50 1 d P . .
H5A H 0.8274 0.0748 -0.1724 0.035 Uiso 0.50 1 calc PR . .
H5B H 0.9453 0.1468 -0.0576 0.035 Uiso 0.50 1 calc PR . .
Co2 Co 0.5000 0.5000 0.0000 0.0112(6) Uani 1 2 d S . .
Co1 Co 0.59487(15) 0.74461(15) 0.2267(2) 0.0117(6) Uani 1 1 d . . .
P3 P 0.8025(3) 0.8915(3) 0.5222(5) 0.0141(8) Uiso 1 1 d . . .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
F2 0.018(3) 0.020(4) 0.015(4) 0.001(3) 0.015(3) 0.003(3)
O1 0.015(4) 0.013(4) 0.022(5) -0.002(4) 0.012(4) -0.002(4)
O4 0.015(4) 0.018(4) 0.014(4) 0.000(4) 0.009(3) 0.005(4)
O2 0.022(5) 0.033(6) 0.016(5) -0.007(4) 0.011(4) -0.009(4)
O3 0.021(5) 0.040(6) 0.015(5) 0.012(5) 0.010(4) 0.013(5)
N1 0.018(5) 0.018(5) 0.029(6) 0.009(5) 0.018(5) 0.002(5)
C5 0.057(19) 0.018(13) 0.013(13) -0.011(11) 0.008(13) -0.020(14)
Co2 0.0183(12) 0.0112(12) 0.0071(11) -0.0017(9) 0.0104(9) -0.0020(9)
Co1 0.0193(10) 0.0109(9) 0.0078(9) -0.0011(6) 0.0101(7) 0.0005(6)
 
_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
F2 Co2 2.011(7) . ?
F2 Co1 2.083(8) . ?
F3 Co2 2.006(7) . ?
F3 Co1 2.046(7) 2_645 ?
F1 Co1 2.016(7) 4_575 ?
F1 Co1 2.035(7) . ?
O1 P3 1.508(10) . ?
O1 Co1 2.084(8) . ?
O4 P3 1.512(9) 2_645 ?
O4 Co1 2.125(9) 3_665 ?
O4 Co2 2.198(9) . ?
O2 P3 1.546(11) . ?
O3 P3 1.571(10) . ?
N1 C2 1.502(19) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C2 C4 1.31(3) . ?
C2 C5 1.38(3) . ?
N2 C5 1.45(4) 4_566 ?
N2 C4 1.53(3) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
C4 C5 1.84(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.45(4) 4_565 ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
Co2 F3 2.006(7) 3_665 ?
Co2 F2 2.011(7) 3_665 ?
Co2 O4 2.198(9) 3_665 ?
Co1 F1 2.016(7) 4_576 ?
Co1 F3 2.046(7) 2_655 ?
Co1 O4 2.125(9) 3_665 ?
P3 O4 1.512(9) 2_655 ?
 
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 F2 Co1 101.8(3) . . ?
Co2 F3 Co1 128.0(4) . 2_645 ?
Co1 F1 Co1 130.5(4) 4_575 . ?
P3 O1 Co1 124.6(5) . . ?
P3 O4 Co1 121.5(5) 2_645 3_665 ?
P3 O4 Co2 125.6(5) 2_645 . ?
Co1 O4 Co2 94.6(3) 3_665 . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C4 C2 C5 86.5(19) . . ?
C4 C2 N1 117.5(16) . . ?
C5 C2 N1 116.1(18) . . ?
C5 N2 C4 116(2) 4_566 . ?
C5 N2 H2A 108.2 4_566 . ?
C4 N2 H2A 108.2 . . ?
C5 N2 H2B 108.2 4_566 . ?
C4 N2 H2B 108.2 . . ?
H2A N2 H2B 107.3 . . ?
C2 C4 N2 109(2) . . ?
C2 C4 C5 48.3(14) . . ?
N2 C4 C5 157(2) . . ?
C2 C4 H4A 109.8 . . ?
N2 C4 H4A 109.8 . . ?
C5 C4 H4A 85.9 . . ?
C2 C4 H4B 109.8 . . ?
N2 C4 H4B 109.8 . . ?
C5 C4 H4B 79.2 . . ?
H4A C4 H4B 108.3 . . ?
C2 C5 N2 119(3) . 4_565 ?
C2 C5 C4 45.2(13) . . ?
N2 C5 C4 83.5(19) 4_565 . ?
C2 C5 H5A 107.6 . . ?
N2 C5 H5A 107.7 4_565 . ?
C4 C5 H5A 150.4 . . ?
C2 C5 H5B 107.7 . . ?
N2 C5 H5B 107.6 4_565 . ?
C4 C5 H5B 94.8 . . ?
H5A C5 H5B 107.1 . . ?
F3 Co2 F3 180.0(3) . 3_665 ?
F3 Co2 F2 92.1(3) . . ?
F3 Co2 F2 87.9(3) 3_665 . ?
F3 Co2 F2 87.9(3) . 3_665 ?
F3 Co2 F2 92.1(3) 3_665 3_665 ?
F2 Co2 F2 180.0(4) . 3_665 ?
F3 Co2 O4 88.6(3) . 3_665 ?
F3 Co2 O4 91.4(3) 3_665 3_665 ?
F2 Co2 O4 81.2(3) . 3_665 ?
F2 Co2 O4 98.8(3) 3_665 3_665 ?
F3 Co2 O4 91.4(3) . . ?
F3 Co2 O4 88.6(3) 3_665 . ?
F2 Co2 O4 98.8(3) . . ?
F2 Co2 O4 81.2(3) 3_665 . ?
O4 Co2 O4 180.0 3_665 . ?
F1 Co1 F1 176.60(19) 4_576 . ?
F1 Co1 F3 91.7(3) 4_576 2_655 ?
F1 Co1 F3 85.9(3) . 2_655 ?
F1 Co1 O1 91.1(3) 4_576 . ?
F1 Co1 O1 86.6(3) . . ?
F3 Co1 O1 91.4(3) 2_655 . ?
F1 Co1 F2 86.5(3) 4_576 . ?
F1 Co1 F2 95.8(3) . . ?
F3 Co1 F2 89.3(3) 2_655 . ?
O1 Co1 F2 177.6(3) . . ?
F1 Co1 O4 96.3(3) 4_576 3_665 ?
F1 Co1 O4 86.5(3) . 3_665 ?
F3 Co1 O4 167.3(3) 2_655 3_665 ?
O1 Co1 O4 98.3(3) . 3_665 ?
F2 Co1 O4 81.4(3) . 3_665 ?
O1 P3 O4 112.8(5) . 2_655 ?
O1 P3 O2 110.6(5) . . ?
O4 P3 O2 111.0(5) 2_655 . ?
O1 P3 O3 108.6(5) . . ?
O4 P3 O3 107.8(5) 2_655 . ?
O2 P3 O3 105.7(6) . . ?

_refine_diff_density_max    1.642
_refine_diff_density_min   -4.986
_refine_diff_density_rms    0.565

