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

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
;
Water molecule with unresolved H-atoms
;
_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_2010jaa0137_p-4n2

# start Validation Reply Form

_vrf_PLAT306_2010jaa0137_p-4n2
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        OW1     
RESPONSE: Water molecule
;
# end Validation Reply Form

#Added by publCIF (Tue 3. Jul 14:51:28 2012)


_audit_update_record
;
2012-06-14 # Formatted by publCIF
;
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C10 H18 Co4 F5 N6 O21 P6'
_chemical_formula_weight          1074.84
 
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'
 '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'
 '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'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            tetragonal
_symmetry_space_group_name_H-M    P-4n2
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, z'
 'y, -x, -z'
 '-y, x, -z'
 'x+1/2, -y+1/2, z+1/2'
 '-x+1/2, y+1/2, z+1/2'
 'y+1/2, x+1/2, -z+1/2'
 '-y+1/2, -x+1/2, -z+1/2'
 
_cell_length_a                    12.9145(2)
_cell_length_b                    12.9145(2)
_cell_length_c                    9.8482(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      1642.53(5)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     10760
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             blue
_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     2.328
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1104
_exptl_absorpt_coefficient_mu     2.397
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9508
_exptl_absorpt_correction_T_max   0.9668
_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             11625
_diffrn_reflns_av_R_equivalents   0.0333
_diffrn_reflns_av_sigmaI/netI     0.0283
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          3.04
_diffrn_reflns_theta_max          27.47
_reflns_number_total              1860
_reflns_number_gt                 1827
_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)+(0.1204P)²+10.2450P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     .
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.00(1)
_refine_ls_number_reflns          1860
_refine_ls_number_parameters      99
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0683
_refine_ls_R_factor_gt            0.0672
_refine_ls_wR_factor_ref          0.1994
_refine_ls_wR_factor_gt           0.1974
_refine_ls_goodness_of_fit_ref    1.104
_refine_ls_restrained_S_all       1.104
_refine_ls_shift/su_max           0.113
_refine_ls_shift/su_mean          0.009
 
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
O10 O 0.2549(6) 0.1095(9) 0.2505(8) 0.063(3) Uani 1 1 d . . .
F20 F 0.1046(5) -0.2637(5) 0.2802(6) 0.0439(13) Uani 1 1 d . . .
OW1 O 0.0000 0.0000 0.5000 0.065(5) Uani 1 4 d S . .
P1 P 0.3652(2) 0.1348(2) 0.2500 0.0648(16) Uani 1 2 d S . .
P2 P 0.07235(15) -0.17586(15) 0.1837(2) 0.0245(4) Uani 1 1 d . . .
N2 N 0.627(3) 0.179(3) 0.143(4) 0.108(10) Uiso 0.50 1 d P . .
C2 C 0.6286(15) 0.2574(16) 0.003(2) 0.039(4) Uiso 0.50 1 d P . .
N1 N 0.5230(12) 0.2902(12) 0.0144(16) 0.035(3) Uiso 0.50 1 d P . .
C5 C 0.5997(15) 0.1022(14) -0.1498(19) 0.081(4) Uiso 1 1 d . . .
N6 N 0.6504(7) 0.1504(7) -0.2500 0.044(3) Uiso 1 2 d S . .
C7 C 0.6376(17) 0.1893(19) 0.007(2) 0.098(6) Uiso 1 1 d . . .
O6 O 0.3883(12) 0.1111(12) 0.0699(14) 0.098(4) Uiso 1 1 d . . .
O1 O 0.1381(5) -0.0817(5) 0.2141(8) 0.0421(17) Uani 1 1 d . . .
O3 O 0.2106(5) 0.0857(5) -0.0369(6) 0.0307(12) Uani 1 1 d . . .
O5 O 0.0428(5) 0.1543(4) 0.2146(6) 0.0302(12) Uani 1 1 d . . .
F1 F 0.0000 0.0000 0.0000 0.0258(18) Uani 1 4 d S . .
Co1 Co 0.13619(7) 0.05480(7) 0.13118(11) 0.0221(3) Uani 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
O10 0.044(4) 0.114(7) 0.032(3) -0.014(4) -0.007(3) -0.030(4)
F20 0.048(3) 0.041(3) 0.043(3) 0.010(2) 0.004(3) 0.007(2)
OW1 0.073(8) 0.073(8) 0.047(9) 0.000 0.000 0.000
P1 0.0247(10) 0.0247(10) 0.145(5) -0.0046(15) -0.0046(15) -0.0062(11)
P2 0.0228(8) 0.0221(9) 0.0286(9) 0.0085(7) 0.0012(7) -0.0002(7)
O1 0.036(3) 0.034(3) 0.056(4) 0.019(3) -0.019(3) -0.016(2)
O3 0.029(3) 0.036(3) 0.027(3) -0.007(2) 0.007(2) -0.008(2)
O5 0.027(3) 0.028(3) 0.035(3) -0.009(2) -0.006(2) 0.003(2)
F1 0.023(3) 0.023(3) 0.032(4) 0.000 0.000 0.000
Co1 0.0225(5) 0.0208(5) 0.0231(5) 0.0021(4) 0.0002(4) -0.0029(3)
 
_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
O10 P1 1.461(8) . ?
O10 Co1 2.057(7) . ?
F20 P2 1.538(6) . ?
P1 O10 1.461(8) 8 ?
P1 O6 1.824(14) . ?
P1 O6 1.824(14) 8 ?
P2 O1 1.514(6) . ?
P2 O3 1.523(6) 3 ?
P2 O5 1.543(6) 2 ?
N2 C7 1.36(4) . ?
N2 C2 1.72(4) . ?
C2 C7 0.89(3) . ?
C2 N1 1.43(2) . ?
N1 C7 1.97(3) . ?
C5 N6 1.34(2) . ?
C5 C7 1.97(3) . ?
C5 C5 1.98(4) 7_544 ?
N6 C5 1.34(2) 7_544 ?
O1 Co1 1.943(7) . ?
O3 P2 1.523(6) 4 ?
O3 Co1 1.955(6) . ?
O5 P2 1.543(6) 2 ?
O5 Co1 1.944(6) . ?
F1 Co1 2.2942(10) 4 ?
F1 Co1 2.2942(10) . ?
F1 Co1 2.2942(10) 3 ?
F1 Co1 2.2942(10) 2 ?
 
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
P1 O10 Co1 143.3(5) . . ?
O10 P1 O10 115.9(9) 8 . ?
O10 P1 O6 97.1(6) 8 . ?
O10 P1 O6 97.2(6) . . ?
O10 P1 O6 97.2(6) 8 8 ?
O10 P1 O6 97.1(6) . 8 ?
O6 P1 O6 152.9(9) . 8 ?
O1 P2 O3 111.2(4) . 3 ?
O1 P2 F20 108.5(4) . . ?
O3 P2 F20 109.8(3) 3 . ?
O1 P2 O5 110.9(4) . 2 ?
O3 P2 O5 110.4(4) 3 2 ?
F20 P2 O5 105.8(3) . 2 ?
C7 N2 C2 30.9(15) . . ?
C7 C2 N1 114(2) . . ?
C7 C2 N2 52(2) . . ?
N1 C2 N2 95.5(17) . . ?
C2 N1 C7 24.2(11) . . ?
N6 C5 C7 101.0(12) . . ?
N6 C5 C5 42.5(9) . 7_544 ?
C7 C5 C5 142.0(10) . 7_544 ?
C5 N6 C5 95.1(17) . 7_544 ?
C2 C7 N2 97(3) . . ?
C2 C7 C5 120(3) . . ?
N2 C7 C5 134(3) . . ?
C2 C7 N1 41.4(18) . . ?
N2 C7 N1 87(2) . . ?
C5 C7 N1 102.7(13) . . ?
P2 O1 Co1 129.7(4) . . ?
P2 O3 Co1 129.5(4) 4 . ?
P2 O5 Co1 129.3(4) 2 . ?
Co1 F1 Co1 108.49(2) 4 . ?
Co1 F1 Co1 111.46(5) 4 3 ?
Co1 F1 Co1 108.49(2) . 3 ?
Co1 F1 Co1 108.49(2) 4 2 ?
Co1 F1 Co1 111.46(5) . 2 ?
Co1 F1 Co1 108.49(2) 3 2 ?
O1 Co1 O5 115.5(3) . . ?
O1 Co1 O3 122.3(3) . . ?
O5 Co1 O3 121.9(3) . . ?
O1 Co1 O10 93.5(4) . . ?
O5 Co1 O10 89.7(3) . . ?
O3 Co1 O10 92.7(3) . . ?
O1 Co1 F1 88.09(18) . . ?
O5 Co1 F1 88.06(17) . . ?
O3 Co1 F1 87.88(18) . . ?
O10 Co1 F1 177.6(3) . . ?
 
_diffrn_measured_fraction_theta_max    0.990
_diffrn_reflns_theta_full              27.47
_diffrn_measured_fraction_theta_full   0.990
_refine_diff_density_max    1.880
_refine_diff_density_min   -1.501
_refine_diff_density_rms    0.212

