# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 186/1474

data_CRYSTALS_cif
_audit_creation_date        99-02-26
_audit_creation_method CRYSTALS_ver_07-07-97
_publ_contact_author_name                       'Ann Chippindale'
_publ_contact_author_address
;
Chemical Crystallography Laboratory
9 Parks Road
OXFORD OX1 3PD
;
_publ_contact_author_phone                      ' 01865 270 824 '
_publ_contact_author_fax                        ' 01865 272 699 '
_publ_contact_author_email 'ann.chippindale@chem.ox.ac.uk '
#=======================================================================
# Diffractometer details
#=======================================================================
_diffrn_radiation_monochromator      graphite
_diffrn_measurement_device-type     '  Enraf-nonius DIP2000 '
_computing_data_collection 'DIP2000 software Xpress (MAC Science, 1989)'
_computing_data_reduction
;
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_cell_refinement
;
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)
;
#=======================================================================
# General computing
#=======================================================================

_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)'
 
#=======================================================================

 
_chemical_melting_point                    'not measured'
_refine_ls_matrix_type                   full
_atom_sites_solution_primary   Direct_Methods
_atom_sites_solution_hydrogens       Geometric
_refine_ls_hydrogen_treatment
# choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed'
;
 mixed
;
#***********************************************************************

_cell_length_a 5.210(1)
_cell_angle_alpha 90.
_cell_length_b 12.693(1)
_cell_angle_beta  90.
_cell_length_c 15.518(1)
_cell_angle_gamma 90.
_cell_volume  1026.21
_symmetry_cell_setting 'Orthorhombic '
_symmetry_space_group_name_H-M 'P 21 21 21 '
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 'x+1/2,-y+1/2,-z'
 '-x,y+1/2,-z+1/2'
 '-x+1/2,-y,z+1/2'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
 'C   '    0.0020    0.0020    2.3100   20.8439
    1.0200   10.2075    1.5886    0.5687    0.8650   51.6512    0.2156
'International_Tables_Vol_IV_Table_2.2B'
 'H   '    0.0000    0.0000    0.4930   10.5109
    0.3229   26.1257    0.1402    3.1424    0.0408   57.7997    0.0030
'International_Tables_Vol_IV_Table_2.2B'
 'Co  '    0.2990    0.9730   12.2841    4.2791
    7.3409    0.2784    4.0034   13.5359    2.3488   71.1692    1.0118
'International_Tables_Vol_IV_Table_2.2B'
 'N   '    0.0040    0.0030   12.2126    0.0057
    3.1322    9.8933    2.0125   28.9975    1.1663    0.5826  -11.5290
'International_Tables_Vol_IV_Table_2.2B'
 'O   '    0.0080    0.0060    3.0485   13.2771
    2.2868    5.7011    1.5463    0.3239    0.8670   32.9089    0.2508
'International_Tables_Vol_IV_Table_2.2B'
 'P   '    0.0900    0.0950    6.4345    1.9067
    4.1791   27.1570    1.7800    0.5260    1.4908   68.1645    1.1149
'International_Tables_Vol_IV_Table_2.2B'
_chemical_formula_sum
' C3 H14 Co1 P2 O8 N2 '
_chemical_formula_moiety
' C3 H14 Co1 P2 O8 N2 '
_chemical_formula_weight   327.03
_cell_measurement_reflns_used        6003
_cell_measurement_theta_min        1.31
_cell_measurement_theta_max        26.39
_cell_measurement_temperature        150
_cell_formula_units_Z     4.00
_exptl_crystal_description ' needle '
_exptl_crystal_colour ' dark blue '
_exptl_crystal_size_min 0.06
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_max 0.40
_exptl_crystal_density_diffrn 2.12
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_F_000 670.12
_exptl_absorpt_coefficient_mu 2.01
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(Otwinowski and Minor (1996))'
_exptl_absorpt_correction_T_min 0.48
_exptl_absorpt_correction_T_max 0.89
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_diffrn_standards_decay_% 0.00
_diffrn_ambient_temperature          150
_diffrn_reflns_number 6003
_reflns_number_total 2030
_diffrn_reflns_av_R_equivalents 0.045
_diffrn_measured_fraction_theta_max 0.96
_reflns_number_observed 1721
_diffrn_reflns_theta_min 1.31
_diffrn_reflns_theta_max 26.39
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_reflns_limit_h_min 0
_reflns_limit_h_max 6
_reflns_limit_k_min 0
_reflns_limit_k_max 15
_reflns_limit_l_min 0
_reflns_limit_l_max 19
_reflns_observed_criterion  >3.00\s(I)
_refine_diff_density_min -0.80
_refine_diff_density_max 0.67
_refine_ls_number_reflns 1721
_refine_ls_number_parameters 153
_refine_ls_R_factor_obs 0.0324
_refine_ls_wR_factor_obs 0.0370
_refine_ls_goodness_of_fit_obs 1.1387
_refine_ls_shift/su_max 0.007298
_refine_ls_abs_structure_Flack '0.55(2)'
_refine_ls_abs_structure_details 'Flack, 416 Friedel-pairs'
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
 Chebychev polynomial with   3 parameters (Carruthers & Watkin, 1979)
 1.46 -0.150 0.995
;
_diffrn_radiation_type       'Mo K\a'
_diffrn_radiation_wavelength      0.71069
_diffrn_measurement_method \w
 
# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3
 
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_thermal_displace_type
 Co1 -0.11434(9) 0.12928(4) 0.45535(3) 0.0085 1.0000 Uani
 P1 0.38250(17) 0.12759(7) 0.56901(5) 0.0077 1.0000 Uani
 P2 0.10397(18) -0.08363(7) 0.36631(5) 0.0087 1.0000 Uani
 O1 0.4740(5) 0.0458(2) 0.63791(17) 0.0111 1.0000 Uani
 O2 0.5238(5) 0.0987(2) 0.48536(16) 0.0117 1.0000 Uani
 O3 0.0933(5) 0.1179(2) 0.55906(15) 0.0129 1.0000 Uani
 O4 0.4592(5) 0.2366(2) 0.60077(17) 0.0122 1.0000 Uani
 O5 0.3342(5) -0.0845(2) 0.43295(17) 0.0141 1.0000 Uani
 O6 -0.0426(5) 0.0187(2) 0.37314(18) 0.0140 1.0000 Uani
 O7 -0.0575(5) -0.1788(2) 0.39075(17) 0.0126 1.0000 Uani
 O8 0.2184(5) -0.0951(2) 0.27661(17) 0.0140 1.0000 Uani
 N1 -0.2825(6) -0.1425(3) 0.5600(2) 0.0130 1.0000 Uani
 N2 0.1605(6) -0.2827(3) 0.7624(2) 0.0155 1.0000 Uani
 C1 -0.0494(7) -0.1492(3) 0.6159(2) 0.0134 1.0000 Uani
 C2 -0.1243(8) -0.1396(3) 0.7102(2) 0.0155 1.0000 Uani
 C3 0.0918(8) -0.1689(3) 0.7703(2) 0.0153 1.0000 Uani
 H1 0.408(12) 0.062(5) 0.699(4) 0.0300 1.0000 Uiso
 H2 0.384(12) -0.025(5) 0.447(4) 0.0300 1.0000 Uiso
 H3 -0.2308 -0.1489 0.4982 0.0300 1.0000 Uiso
 H4 -0.4033 -0.2009 0.5751 0.0300 1.0000 Uiso
 H5 -0.3693 -0.0732 0.5694 0.0300 1.0000 Uiso
 H6 0.3040 -0.2994 0.8030 0.0300 1.0000 Uiso
 H7 0.0077 -0.3269 0.7770 0.0300 1.0000 Uiso
 H8 0.2160 -0.2979 0.7020 0.0300 1.0000 Uiso
 H9 0.0372 -0.2185 0.6063 0.0300 1.0000 Uiso
 H10 0.0712 -0.0908 0.6006 0.0300 1.0000 Uiso
 H11 -0.2732 -0.1873 0.7215 0.0300 1.0000 Uiso
 H12 -0.1757 -0.0651 0.7219 0.0300 1.0000 Uiso
 H13 0.0375 -0.1543 0.8309 0.0300 1.0000 Uiso
 H14 0.2458 -0.1253 0.7559 0.0300 1.0000 Uiso
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 0.0070(2) 0.0080(2) 0.0107(2) -0.00020(18) 0.00061(18) -0.0008(2)
 P1 0.0058(4) 0.0081(4) 0.0090(4) -0.0002(3) -0.0003(3) 0.0006(4)
 P2 0.0090(4) 0.0080(4) 0.0090(4) -0.0013(3) -0.0004(4) 0.0002(4)
 O1 0.0130(13) 0.0082(15) 0.0120(12) 0.003(1) -0.002(1) 0.003(1)
 O2 0.0087(12) 0.0127(14) 0.0136(12) -0.0008(9) 0.0038(9) -0.003(1)
 O3 0.0062(11) 0.0204(15) 0.0122(11) -0.000(1) -0.000(1) -0.0017(11
 O4 0.0132(14) 0.0085(15) 0.0150(13) 0.001(1) -0.004(1) 0.0012(9)
 O5 0.0121(13) 0.0125(14) 0.0176(13) 0.0000(11) -0.006(1) 0.0006(11
 O6 0.0157(15) 0.0112(15) 0.0149(13) -0.002(1) -0.0035(11) 0.003(1)
 O7 0.0107(14) 0.0103(14) 0.0167(13) 0.0016(11) -0.001(1) -0.001(1)
 O8 0.0129(12) 0.0141(15) 0.0149(13) 0.0001(11) 0.003(1) 0.004(1)
 N1 0.0120(14) 0.0133(18) 0.0137(15) 0.0015(12) -0.0016(12) -0.0007(13
 N2 0.0092(17) 0.0215(19) 0.0157(16) 0.0031(13) -0.0006(13) 0.0037(13
 C1 0.0084(17) 0.018(2) 0.0134(17) 0.0039(14) -0.0023(12) 0.0003(13
 C2 0.0136(17) 0.015(2) 0.0176(18) -0.0040(14) -0.0017(15) 0.0008(19
 C3 0.0132(18) 0.0178(19) 0.0147(18) -0.0036(14) 0.0010(16) 0.0009(17
_refine_ls_extinction_method
    'None'
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Co1 . O2 1_455 1.980(3)    yes
Co1 . O3 . 1.945(2)    yes
Co1 . O4 2_456 1.950(3)    yes
Co1 . O6 . 1.933(3)    yes
P1 . O1 . 1.565(3)    yes
P1 . O2 . 1.537(3)    yes
P1 . O3 . 1.519(3)    yes
P1 . O4 . 1.523(3)    yes
P2 . O5 . 1.584(3)    yes
P2 . O6 . 1.510(3)    yes
P2 . O7 . 1.521(3)    yes
P2 . O8 . 1.521(3)    yes
O1 . H1 . 1.03(6)    yes
O5 . H2 . 0.82(6)    yes
N1 . C1 . 1.495(5)    yes
N1 . H3 . 1.000(3)    no
N1 . H4 . 1.000(3)    no
N1 . H5 . 1.000(4)    no
N2 . C3 . 1.492(5)    yes
N2 . H6 . 1.000(3)    no
N2 . H7 . 1.000(3)    no
N2 . H8 . 1.000(3)    no
C1 . C2 . 1.519(5)    yes
C1 . H9 . 1.000(4)    no
C1 . H10 . 1.000(4)    no
C2 . C3 . 1.508(6)    yes
C2 . H11 . 1.000(4)    no
C2 . H12 . 1.000(4)    no
C3 . H13 . 1.000(4)    no
C3 . H14 . 1.000(4)    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O2 1_455 Co1 . O3 . 108.7(1)    yes
O2 1_455 Co1 . O4 2_456 117.61(12)    yes
O3 . Co1 . O4 2_456 108.99(11)    yes
O2 1_455 Co1 . O6 . 101.34(12)    yes
O3 . Co1 . O6 . 112.61(12)    yes
O4 2_456 Co1 . O6 . 107.52(12)    yes
O1 . P1 . O2 . 105.83(16)    yes
O1 . P1 . O3 . 108.53(15)    yes
O2 . P1 . O3 . 111.71(15)    yes
O1 . P1 . O4 . 107.56(15)    yes
O2 . P1 . O4 . 111.39(16)    yes
O3 . P1 . O4 . 111.54(16)    yes
O5 . P2 . O6 . 110.09(16)    yes
O5 . P2 . O7 . 104.50(15)    yes
O6 . P2 . O7 . 112.71(16)    yes
O5 . P2 . O8 . 107.46(16)    yes
O6 . P2 . O8 . 110.16(16)    yes
O7 . P2 . O8 . 111.65(16)    yes
P1 . O1 . H1 . 112.9(33)    yes
Co1 1_655 O2 . P1 . 127.44(16)    yes
Co1 . O3 . P1 . 129.03(15)    yes
Co1 2_556 O4 . P1 . 126.67(16)    yes
P2 . O5 . H2 . 114.1(43)    yes
Co1 . O6 . P2 . 140.21(18)    yes
C1 . N1 . H3 . 109.5(3)    no
C1 . N1 . H4 . 109.5(3)    no
H3 . N1 . H4 . 109.5(3)    no
C1 . N1 . H5 . 109.5(3)    no
H3 . N1 . H5 . 109.5(3)    no
H4 . N1 . H5 . 109.5(3)    no
C3 . N2 . H6 . 109.5(3)    no
C3 . N2 . H7 . 109.5(3)    no
H6 . N2 . H7 . 109.5(3)    no
C3 . N2 . H8 . 109.5(3)    no
H6 . N2 . H8 . 109.5(3)    no
H7 . N2 . H8 . 109.5(3)    no
N1 . C1 . C2 . 110.2(3)    yes
N1 . C1 . H9 . 109.3(3)    no
C2 . C1 . H9 . 109.3(3)    no
N1 . C1 . H10 . 109.3(3)    no
C2 . C1 . H10 . 109.3(3)    no
H9 . C1 . H10 . 109.5(3)    no
C1 . C2 . C3 . 112.6(3)    yes
C1 . C2 . H11 . 108.7(3)    no
C3 . C2 . H11 . 108.7(3)    no
C1 . C2 . H12 . 108.7(3)    no
C3 . C2 . H12 . 108.7(3)    no
H11 . C2 . H12 . 109.5(4)    no
N2 . C3 . C2 . 111.5(3)    yes
N2 . C3 . H13 . 109.0(3)    no
C2 . C3 . H13 . 109.0(4)    no
N2 . C3 . H14 . 109.0(3)    no
C2 . C3 . H14 . 109.0(3)    no
H13 . C3 . H14 . 109.5(4)    no