Electronic Supplementary Material for CrystEngComm
This Journal is (c) The Royal Society of Chemistry 2006

data_global

_journal_coden_Cambridge         1350

_publ_requested_journal          CrystEngComm

loop_
_publ_author_name
'Lars Ohrstrom'
'Cedric Borel'
'Mikael Hakansson'

_publ_contact_author_name        'Prof Lars Ohrstrom'
_publ_contact_author_address     
;
Department of Chemical & Biological Engineering
Chalmers University of Technology
Gothenburg
41296
SWEDEN
;

_publ_contact_author_email       'OHRSTROM@CHEM.CHALMERS.SE '

_publ_section_title              
;
Coordination bonds and strong hydrogen
bonds giving a framework material based on a 4- and 8-connected
net in [Ca[Co(en)(oxalato)2]2]n
;

# Attachment 'coenox2ca.cif'

data_coenox3
_database_code_depnum_ccdc_archive 'CCDC 605384'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H16 Ca Co2 N4 O16'
_chemical_formula_weight         630.23

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'
Co Co 0.3494 0.9721 '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'
Ca Ca 0.2262 0.3064 '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-4

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'

_cell_length_a                   8.898(3)
_cell_length_b                   8.898(3)
_cell_length_c                   7.679(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     608.0(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3741
_cell_measurement_theta_min      3.50
_cell_measurement_theta_max      25.0

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             318
_exptl_absorpt_coefficient_mu    1.654
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_process_details   REQAB

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'R-Axis IIc'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3741
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.50
_diffrn_reflns_theta_max         25.0
_reflns_number_total             1053
_reflns_number_gt                991
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_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^)+(0.1199P)^2^+0.8724P] 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     SHELXL
_refine_ls_extinction_coef       0.24(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(6)
_refine_ls_number_reflns         1053
_refine_ls_number_parameters     82
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0685
_refine_ls_wR_factor_ref         0.1823
_refine_ls_wR_factor_gt          0.1780
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_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
C1 C 0.0573(9) 0.7647(8) 0.1861(9) 0.0404(16) Uani 1 1 d . . .
C2 C -0.0822(9) 0.7057(8) 0.2787(9) 0.0435(16) Uani 1 1 d . . .
C3 C 0.076(3) 0.5054(15) -0.2964(14) 0.175(15) Uani 1 1 d . . .
H3A H 0.1067 0.6100 -0.3023 0.210 Uiso 1 1 calc R . .
H3B H 0.1177 0.4532 -0.3964 0.210 Uiso 1 1 calc R . .
Co1 Co 0.0000 0.5000 0.04855(17) 0.0506(7) Uani 1 2 d S . .
N1 N 0.1321(18) 0.4362(9) -0.1328(12) 0.106(5) Uani 1 1 d . . .
H1A H 0.2267 0.4666 -0.1106 0.127 Uiso 1 1 calc R . .
H1B H 0.1316 0.3353 -0.1416 0.127 Uiso 1 1 calc R . .
O1 O 0.1019(8) 0.6843(7) 0.0583(8) 0.0574(15) Uani 1 1 d . . .
O2 O 0.1161(6) 0.8832(6) 0.2375(7) 0.0483(14) Uani 1 1 d . . .
O3 O -0.1303(7) 0.5805(7) 0.2253(8) 0.0554(15) Uani 1 1 d . . .
O4 O -0.1397(7) 0.7818(6) 0.3975(8) 0.0521(15) Uani 1 1 d . . .
Ca1 Ca 0.0000 1.0000 0.5000 0.0382(8) Uani 1 4 d S . .

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
C1 0.055(4) 0.040(4) 0.027(3) -0.001(3) -0.005(3) 0.000(3)
C2 0.059(5) 0.037(3) 0.034(3) -0.007(3) -0.006(3) -0.008(3)
C3 0.44(4) 0.036(5) 0.051(5) -0.022(5) 0.075(12) -0.105(14)
Co1 0.0804(12) 0.0378(9) 0.0337(8) 0.000 0.000 0.0004(7)
N1 0.215(14) 0.037(4) 0.066(6) -0.017(4) 0.042(8) -0.017(6)
O1 0.077(4) 0.054(3) 0.041(3) 0.001(3) 0.016(3) 0.010(3)
O2 0.050(3) 0.051(3) 0.044(3) -0.008(2) 0.010(3) -0.006(2)
O3 0.057(3) 0.048(3) 0.061(4) -0.004(3) -0.006(3) -0.005(3)
O4 0.054(3) 0.046(3) 0.056(3) -0.018(3) 0.009(3) -0.008(2)
Ca1 0.0420(10) 0.0420(10) 0.0305(14) 0.000 0.000 0.000

_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
C1 O2 1.241(10) . ?
C1 O1 1.277(9) . ?
C1 C2 1.524(11) . ?
C1 Ca1 3.233(7) . ?
C2 O4 1.245(9) . ?
C2 O3 1.262(9) . ?
C2 Ca1 3.206(7) . ?
C3 C3 1.36(5) 2_565 ?
C3 N1 1.48(2) . ?
Co1 O1 1.876(7) . ?
Co1 O1 1.876(7) 2_565 ?
Co1 N1 1.909(11) . ?
Co1 N1 1.909(11) 2_565 ?
Co1 O3 1.923(6) 2_565 ?
Co1 O3 1.923(6) . ?
O2 Ca1 2.492(5) . ?
O4 Ca1 2.436(5) . ?
Ca1 O4 2.436(5) 2_575 ?
Ca1 O4 2.436(5) 4_666 ?
Ca1 O4 2.436(5) 3_466 ?
Ca1 O2 2.492(5) 4_666 ?
Ca1 O2 2.492(5) 3_466 ?
Ca1 O2 2.492(5) 2_575 ?
Ca1 C2 3.206(7) 4_666 ?
Ca1 C2 3.206(7) 2_575 ?
Ca1 C2 3.206(7) 3_466 ?

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
O2 C1 O1 126.1(7) . . ?
O2 C1 C2 119.2(6) . . ?
O1 C1 C2 114.7(7) . . ?
O1 C1 Ca1 169.8(6) . . ?
C2 C1 Ca1 75.3(4) . . ?
O4 C2 O3 125.4(8) . . ?
O4 C2 C1 119.3(7) . . ?
O3 C2 C1 115.4(7) . . ?
O3 C2 Ca1 166.1(6) . . ?
C1 C2 Ca1 77.3(4) . . ?
C3 C3 N1 107.7(9) 2_565 . ?
O1 Co1 O1 175.4(4) . 2_565 ?
O1 Co1 N1 89.5(3) . . ?
O1 Co1 N1 93.8(4) 2_565 . ?
O1 Co1 N1 93.8(4) . 2_565 ?
O1 Co1 N1 89.5(3) 2_565 2_565 ?
N1 Co1 N1 86.3(9) . 2_565 ?
O1 Co1 O3 90.3(3) . 2_565 ?
O1 Co1 O3 86.4(2) 2_565 2_565 ?
N1 Co1 O3 91.9(4) . 2_565 ?
N1 Co1 O3 175.4(3) 2_565 2_565 ?
O1 Co1 O3 86.4(2) . . ?
O1 Co1 O3 90.3(3) 2_565 . ?
N1 Co1 O3 175.4(3) . . ?
N1 Co1 O3 91.9(4) 2_565 . ?
O3 Co1 O3 90.2(4) 2_565 . ?
C3 N1 Co1 106.8(13) . . ?
C1 O1 Co1 111.8(5) . . ?
C1 O2 Ca1 115.9(5) . . ?
C2 O3 Co1 110.7(6) . . ?
C2 O4 Ca1 117.4(5) . . ?
O4 Ca1 O4 142.3(3) . 2_575 ?
O4 Ca1 O4 96.00(9) . 4_666 ?
O4 Ca1 O4 96.00(9) 2_575 4_666 ?
O4 Ca1 O4 96.00(9) . 3_466 ?
O4 Ca1 O4 96.00(9) 2_575 3_466 ?
O4 Ca1 O4 142.3(3) 4_666 3_466 ?
O4 Ca1 O2 143.57(19) . 4_666 ?
O4 Ca1 O2 73.6(2) 2_575 4_666 ?
O4 Ca1 O2 67.52(18) 4_666 4_666 ?
O4 Ca1 O2 81.9(2) 3_466 4_666 ?
O4 Ca1 O2 67.52(18) . . ?
O4 Ca1 O2 81.9(2) 2_575 . ?
O4 Ca1 O2 73.6(2) 4_666 . ?
O4 Ca1 O2 143.57(19) 3_466 . ?
O2 Ca1 O2 130.87(17) 4_666 . ?
O4 Ca1 O2 73.6(2) . 3_466 ?
O4 Ca1 O2 143.57(19) 2_575 3_466 ?
O4 Ca1 O2 81.9(2) 4_666 3_466 ?
O4 Ca1 O2 67.52(18) 3_466 3_466 ?
O2 Ca1 O2 72.0(3) 4_666 3_466 ?
O2 Ca1 O2 130.87(17) . 3_466 ?
O4 Ca1 O2 81.9(2) . 2_575 ?
O4 Ca1 O2 67.52(18) 2_575 2_575 ?
O4 Ca1 O2 143.57(19) 4_666 2_575 ?
O4 Ca1 O2 73.6(2) 3_466 2_575 ?
O2 Ca1 O2 130.87(17) 4_666 2_575 ?
O2 Ca1 O2 72.0(3) . 2_575 ?
O2 Ca1 O2 130.87(17) 3_466 2_575 ?
O4 Ca1 C2 20.2(2) . . ?
O4 Ca1 C2 126.6(2) 2_575 . ?
O4 Ca1 C2 86.4(2) 4_666 . ?
O4 Ca1 C2 114.0(2) 3_466 . ?
O2 Ca1 C2 149.58(18) 4_666 . ?
O2 Ca1 C2 47.57(18) . . ?
O2 Ca1 C2 89.72(19) 3_466 . ?
O2 Ca1 C2 79.47(18) 2_575 . ?
O4 Ca1 C2 114.0(2) . 4_666 ?
O4 Ca1 C2 86.4(2) 2_575 4_666 ?
O4 Ca1 C2 20.2(2) 4_666 4_666 ?
O4 Ca1 C2 126.6(2) 3_466 4_666 ?
O2 Ca1 C2 47.57(18) 4_666 4_666 ?
O2 Ca1 C2 89.72(19) . 4_666 ?
O2 Ca1 C2 79.47(18) 3_466 4_666 ?
O2 Ca1 C2 149.58(18) 2_575 4_666 ?
C2 Ca1 C2 106.31(12) . 4_666 ?
O4 Ca1 C2 126.6(2) . 2_575 ?
O4 Ca1 C2 20.2(2) 2_575 2_575 ?
O4 Ca1 C2 114.0(2) 4_666 2_575 ?
O4 Ca1 C2 86.4(2) 3_466 2_575 ?
O2 Ca1 C2 89.72(19) 4_666 2_575 ?
O2 Ca1 C2 79.47(18) . 2_575 ?
O2 Ca1 C2 149.58(18) 3_466 2_575 ?
O2 Ca1 C2 47.57(18) 2_575 2_575 ?
C2 Ca1 C2 116.0(3) . 2_575 ?
C2 Ca1 C2 106.31(12) 4_666 2_575 ?
O4 Ca1 C2 86.4(2) . 3_466 ?
O4 Ca1 C2 114.0(2) 2_575 3_466 ?
O4 Ca1 C2 126.6(2) 4_666 3_466 ?
O4 Ca1 C2 20.2(2) 3_466 3_466 ?
O2 Ca1 C2 79.47(18) 4_666 3_466 ?
O2 Ca1 C2 149.58(18) . 3_466 ?
O2 Ca1 C2 47.57(18) 3_466 3_466 ?
O2 Ca1 C2 89.72(19) 2_575 3_466 ?
C2 Ca1 C2 106.31(12) . 3_466 ?
C2 Ca1 C2 116.0(3) 4_666 3_466 ?
C2 Ca1 C2 106.31(12) 2_575 3_466 ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.123


