# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'R. Morris'
_publ_contact_author_email       REM1@ST-ANDREWS.AC.UK

_publ_section_title              
;
A Novel Non-centrosymmetric
Metallophosphate-Borate Compound via Ionothermal Synthesis
;
loop_
_publ_author_name
'R. Morris'
'Philip Lightfoot'
'Zhuojia Lin.'
'David Wragg'

# Attachment 'borate.cif'

data_new
_database_code_depnum_ccdc_archive 'CCDC 722597'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4(Co O4 P), B5 H4 O10, C4 H12 N, 4(C H6 N)'
_chemical_formula_sum            'C8 H40 B5 Co4 N5 O26 P4'
_chemical_formula_weight         1036.10

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'
B B 0.0013 0.0007 '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'
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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'I 2 2 2'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'

_cell_length_a                   6.7601(6)
_cell_length_b                   7.5422(6)
_cell_length_c                   34.822(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1775.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    3685
_cell_measurement_theta_min      1.14
_cell_measurement_theta_max      28.38

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1048
_exptl_absorpt_coefficient_mu    2.115
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.69390
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_monochromator  silicon
_diffrn_measurement_method       'profile data'
_diffrn_measurement_device_type  
;
;
_diffrn_detector_area_resol_mean 7.353
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?

_diffrn_reflns_number            7218
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_theta_min         2.70
_diffrn_reflns_theta_max         30.15
_reflns_number_total             2774
_reflns_number_gt                2263
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0585P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.47(5)
_refine_ls_number_reflns         2774
_refine_ls_number_parameters     123
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.0994
_refine_ls_wR_factor_gt          0.0953
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_restrained_S_all      0.957
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 1.0000 0.0000 0.244294(17) 0.01415(15) Uani 1 2 d S . .
Co2 Co 1.0000 -0.5000 0.255975(17) 0.01488(16) Uani 1 2 d S . .
P1 P 1.25404(17) -0.20351(7) 0.301174(16) 0.01358(13) Uani 1 1 d . . .
O4 O 1.0689(3) -0.3131(4) 0.29238(7) 0.0229(6) Uani 1 1 d . . .
O1 O 1.2498(4) -0.0400(2) 0.27277(4) 0.0152(3) Uani 1 1 d . . .
O7 O 1.2502(6) 0.7807(3) 0.41744(6) 0.0482(7) Uani 1 1 d . . .
H7A H 1.2494 0.8100 0.3938 0.058 Uiso 1 1 d R . .
C1 C 1.2593(8) 0.3430(5) 0.37669(9) 0.0393(8) Uani 1 1 d . . .
H1C H 1.2831 0.4656 0.3686 0.047 Uiso 1 1 calc R . .
H1B H 1.3688 0.3029 0.3930 0.047 Uiso 1 1 calc R . .
H1A H 1.1353 0.3368 0.3912 0.047 Uiso 1 1 calc R . .
O3 O 1.4439(3) -0.3045(4) 0.29100(6) 0.0221(6) Uani 1 1 d . . .
N1 N 1.2456(7) 0.2300(3) 0.34309(6) 0.0231(4) Uani 1 1 d . . .
H1D H 1.2306 0.1204 0.3503 0.028 Uiso 1 1 calc R . .
H1E H 1.3534 0.2397 0.3296 0.028 Uiso 1 1 calc R . .
H1F H 1.1447 0.2622 0.3292 0.028 Uiso 1 1 calc R . .
O2 O 1.2584(6) -0.1391(2) 0.34192(5) 0.0224(4) Uani 1 1 d . . .
O6 O 1.0000 1.0000 0.41694(10) 0.0422(10) Uani 1 2 d S . .
B1 B 1.0000 1.0000 0.5000 0.052(3) Uani 1 4 d S . .
O5 O 1.1244(6) 0.8874(4) 0.47611(7) 0.0593(10) Uani 1 1 d . . .
N2 N 1.5000 -0.5000 0.5000 0.062(2) Uani 1 4 d S . .
B2 B 1.1278(8) 0.8898(7) 0.43741(12) 0.0410(11) Uani 1 1 d . . .
C2 C 1.6271(11) -0.6096(10) 0.52600(14) 0.113(3) Uani 1 1 d . . .
H2A H 1.5430 -0.6830 0.5425 0.170 Uiso 1 1 calc R . .
H2B H 1.7086 -0.5314 0.5420 0.170 Uiso 1 1 calc R . .
H2C H 1.7130 -0.6862 0.5105 0.170 Uiso 1 1 calc R . .

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
Co1 0.0118(3) 0.0135(3) 0.0172(3) 0.000 0.000 -0.0022(4)
Co2 0.0115(3) 0.0149(3) 0.0182(3) 0.000 0.000 -0.0015(4)
P1 0.0157(3) 0.0096(2) 0.0155(2) -0.00043(18) -0.0009(5) -0.0021(6)
O4 0.0220(13) 0.0195(13) 0.0271(11) -0.0050(11) 0.0067(11) -0.0096(12)
O1 0.0147(7) 0.0125(7) 0.0184(8) 0.0033(5) -0.0003(13) 0.0009(14)
O7 0.069(2) 0.0507(14) 0.0245(10) 0.0097(10) 0.005(2) 0.024(3)
C1 0.0384(19) 0.0436(17) 0.0357(15) -0.0148(13) -0.001(3) -0.007(3)
O3 0.0191(12) 0.0177(12) 0.0295(11) -0.0115(11) -0.0069(11) 0.0062(12)
N1 0.0223(11) 0.0186(10) 0.0283(10) -0.0012(8) -0.001(2) -0.002(2)
O2 0.0360(11) 0.0149(7) 0.0162(7) -0.0019(6) 0.0004(17) -0.0008(19)
O6 0.064(3) 0.037(2) 0.0255(17) 0.000 0.000 0.015(2)
B1 0.070(8) 0.070(7) 0.018(4) 0.000 0.000 0.000
O5 0.093(3) 0.062(2) 0.0228(13) 0.0072(14) -0.0009(16) 0.022(2)
N2 0.083(7) 0.064(6) 0.040(4) 0.000 0.000 0.000
B2 0.052(3) 0.040(3) 0.031(2) 0.0088(19) -0.006(2) 0.007(2)
C2 0.126(7) 0.156(7) 0.057(3) -0.005(4) -0.009(4) 0.070(6)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds 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
Co1 O3 1.956(2) 7_445 ?
Co1 O3 1.956(2) 8_755 ?
Co1 O1 1.981(3) . ?
Co1 O1 1.981(3) 2_755 ?
Co2 O4 1.952(3) . ?
Co2 O4 1.952(3) 2_745 ?
Co2 O1 1.989(3) 7_445 ?
Co2 O1 1.989(3) 8_745 ?
P1 O2 1.5001(17) . ?
P1 O4 1.531(3) . ?
P1 O3 1.534(3) . ?
P1 O1 1.5809(16) . ?
O1 Co2 1.989(3) 7_545 ?
O7 B2 1.358(6) . ?
O7 H7A 0.8530 . ?
C1 N1 1.450(3) . ?
C1 H1C 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1A 0.9800 . ?
O3 Co1 1.956(2) 7_545 ?
N1 H1D 0.8701 . ?
N1 H1E 0.8701 . ?
N1 H1F 0.8701 . ?
O6 B2 1.395(5) . ?
O6 B2 1.395(5) 2_775 ?
B1 O5 1.456(3) 3_576 ?
B1 O5 1.456(3) . ?
B1 O5 1.456(3) 4_756 ?
B1 O5 1.456(3) 2_775 ?
O5 B2 1.348(5) . ?
N2 C2 1.497(6) 4_856 ?
N2 C2 1.497(6) 3_546 ?
N2 C2 1.497(6) . ?
N2 C2 1.497(6) 2_845 ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?

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
O3 Co1 O3 102.16(15) 7_445 8_755 ?
O3 Co1 O1 111.39(9) 7_445 . ?
O3 Co1 O1 105.32(9) 8_755 . ?
O3 Co1 O1 105.32(9) 7_445 2_755 ?
O3 Co1 O1 111.39(9) 8_755 2_755 ?
O1 Co1 O1 119.94(12) . 2_755 ?
O4 Co2 O4 99.01(15) . 2_745 ?
O4 Co2 O1 114.85(9) . 7_445 ?
O4 Co2 O1 103.50(8) 2_745 7_445 ?
O4 Co2 O1 103.50(8) . 8_745 ?
O4 Co2 O1 114.85(9) 2_745 8_745 ?
O1 Co2 O1 119.55(12) 7_445 8_745 ?
O2 P1 O4 112.35(19) . . ?
O2 P1 O3 111.3(2) . . ?
O4 P1 O3 111.69(11) . . ?
O2 P1 O1 109.86(9) . . ?
O4 P1 O1 106.33(14) . . ?
O3 P1 O1 104.96(14) . . ?
P1 O4 Co2 135.65(15) . . ?
P1 O1 Co1 116.58(15) . . ?
P1 O1 Co2 114.70(14) . 7_545 ?
Co1 O1 Co2 116.73(8) . 7_545 ?
B2 O7 H7A 109.5 . . ?
N1 C1 H1C 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1C C1 H1B 109.5 . . ?
N1 C1 H1A 109.5 . . ?
H1C C1 H1A 109.5 . . ?
H1B C1 H1A 109.5 . . ?
P1 O3 Co1 132.95(15) . 7_545 ?
C1 N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C1 N1 H1F 109.5 . . ?
H1D N1 H1F 109.5 . . ?
H1E N1 H1F 109.5 . . ?
B2 O6 B2 118.6(5) . 2_775 ?
O5 B1 O5 109.4(3) 3_576 . ?
O5 B1 O5 110.3(2) 3_576 4_756 ?
O5 B1 O5 108.7(3) . 4_756 ?
O5 B1 O5 108.7(3) 3_576 2_775 ?
O5 B1 O5 110.3(2) . 2_775 ?
O5 B1 O5 109.4(3) 4_756 2_775 ?
B2 O5 B1 125.0(3) . . ?
C2 N2 C2 105.6(4) 4_856 3_546 ?
C2 N2 C2 113.0(6) 4_856 . ?
C2 N2 C2 109.9(6) 3_546 . ?
C2 N2 C2 109.9(6) 4_856 2_845 ?
C2 N2 C2 113.0(6) 3_546 2_845 ?
C2 N2 C2 105.6(4) . 2_845 ?
O5 B2 O7 121.0(4) . . ?
O5 B2 O6 120.5(4) . . ?
O7 B2 O6 118.5(3) . . ?
N2 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        30.15
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.106