# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5K_neutron_bgCo
_database_code_depnum_ccdc_archive 'CCDC 1876541'
_audit_update_record             
;
2018-11-27 deposited with the CCDC.
2018-11-28 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_formula_sum            'C4 H6 Co1 O6'
_chemical_formula_weight         209

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

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x+1/2,-y+1/2,z+1/2

_cell_length_a                   5.143(3)
_cell_length_b                   7.656(5)
_cell_length_c                   8.653(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.429(8)
_cell_angle_gamma                90
_cell_volume                     330.0(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    73
_cell_measurement_theta_min      3.38
_cell_measurement_theta_max      57.06
_cell_measurement_temperature    5.0(5)

_exptl_crystal_density_diffrn    2.104
_exptl_crystal_F_000             210
_exptl_absorpt_coefficient_mu    0
_exptl_crystal_description       prism
_exptl_crystal_size_max          5
_exptl_crystal_size_mid          2
_exptl_crystal_size_min          2
_exptl_crystal_colour            orange
_exptl_absorpt_correction_type   none

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

# 7. EXPERIMENTAL DATA

_diffrn_ambient_temperature      5.0(5)
_diffrn_radiation_type           neutron
_diffrn_radiation_source         'J-PARC neutron spallation source'
_diffrn_radiation_wavelength     '0.4 - 4.4'
_diffrn_radiation_wavelength_details 'Based on neutron time of flight'
_diffrn_measurement_device       '2-cirle goniometer'
_diffrn_measurement_device_type  
'single-crystal diffractometer SENJU at the BL18 in the MLF of the J-PARC'
_diffrn_detector_area_resol_mean '4 mm'
_diffrn_measurement_method       'time-of-flight Laue'
_diffrn_reflns_number            4726
_diffrn_reflns_theta_min         3.38
_diffrn_reflns_theta_max         57.06
_diffrn_reflns_theta_full        20.29
_diffrn_measured_fraction_theta_max 0.46
_diffrn_measured_fraction_theta_full 0.69
_diffrn_reflns_av_R_equivalents  0.094
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_radiation_probe          neutron

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

# 8. REFINEMENT DATA

_refine_special_details          
; The neutron diffraction data was collected using a closed-cycle helium refrigerator equipped with the 2-axes piezo-motor goniometer (omega, phi and 45 deg. fixed chi). The crystal structure was refined using the result of the X-ray structural analysis as initial parameters. Anisotropic displacement parameters were applied for all atoms inclusing hydrogen atoms.
;

_reflns_number_total             4726
_reflns_number_gt                4100
_reflns_threshold_expression     I>3σ(I)
_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.0683
_refine_ls_wR_factor_gt          0.1234
_refine_ls_R_factor_all          0.0767
_refine_ls_wR_factor_ref         0.1387
_refine_ls_goodness_of_fit_ref   1.31
_refine_ls_goodness_of_fit_gt    1.24
_refine_ls_number_reflns         4726
_refine_ls_number_parameters     87
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(F)+0.0081F²)
_refine_ls_hydrogen_treatment    refall
_refine_ls_shift/su_max          0.0060
_refine_ls_shift/su_mean         0.0012
_refine_diff_density_max         12.20
_refine_diff_density_min         -5.20
_refine_ls_extinction_method     
'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_extinction_coef       17.1(8)

loop_
_atom_type_symbol
_atom_type_scat_length_neutron
_atom_type_scat_source
C 6.646 International_Tables_Vol_C
H -3.739 International_Tables_Vol_C
Co 2.490 International_Tables_Vol_C
O 5.803 International_Tables_Vol_C

_computing_data_collection       STARGazer
_computing_cell_refinement       STARGazer
_computing_data_reduction        'JANA2006(Petricek et al., 2006)'
_computing_structure_solution    'JANA2006(Petricek et al., 2006)'
_computing_structure_refinement  'JANA2006(Petricek et al., 2006)'
_computing_molecular_graphics    'VESTA(Momma & Izumi, 2011)'
_computing_publication_material  'JANA2006(Petricek et al., 2006)'

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

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0 0 0 Uani 0.0015(3) 2 1 d . . .
O2 O 0.18321(11) -0.35656(5) 0.35513(6) Uani 0.00356(13) 4 1 d . . .
O3 O -0.02464(11) -0.15547(5) 0.18683(6) Uani 0.00307(13) 4 1 d . . .
O4 O 0.27801(11) -0.19410(5) -0.01116(6) Uani 0.00348(13) 4 1 d . . .
C5 C 0.15720(9) -0.26635(4) 0.23018(5) Uani 0.00224(11) 4 1 d . . .
C6 C 0.35533(10) -0.29484(5) 0.13025(6) Uani 0.00477(12) 4 1 d . . .
H7 H 0.4326(3) -0.17860(14) -0.05915(18) Uani 0.0155(4) 4 1 d . . .
H8 H 0.5534(4) -0.25571(19) 0.1995(2) Uani 0.0244(5) 4 1 d . . .
H9 H 0.3597(4) -0.43379(13) 0.1026(2) Uani 0.0239(5) 4 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co1 Co 0.0027(6) 0.0010(2) 0.0008(3) 0.0007(2) 0.0006(3) 0.0007(2)
O2 O 0.0041(2) 0.00434(12) 0.0024(2) 0.00162(9) 0.00116(13) 0.00223(9)
O3 O 0.0029(2) 0.00315(12) 0.0033(2) 0.00134(8) 0.00152(12) 0.00153(8)
O4 O 0.0043(2) 0.00384(13) 0.0027(2) 0.00121(9) 0.00191(13) 0.00121(9)
C5 C 0.0029(2) 0.00224(11) 0.0018(2) 0.00062(7) 0.00087(11) 0.00092(7)
C6 C 0.0046(2) 0.00599(12) 0.0048(2) 0.00298(9) 0.00289(13) 0.00283(9)
H7 H 0.0155(7) 0.0187(3) 0.0134(6) 0.0020(3) 0.0075(4) 0.0045(3)
H8 H 0.0116(8) 0.0406(7) 0.0181(9) -0.0021(5) -0.0003(4) 0.0072(6)
H9 H 0.0382(10) 0.0118(3) 0.0269(8) 0.0096(4) 0.0183(6) 0.0051(4)

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

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 O2 . 2_555 2.101(2) ?
Co1 O2 . 4_444 2.101(2) ?
Co1 O3 . . 2.0367(18) ?
Co1 O3 . 3_555 2.0367(18) ?
Co1 O4 . . 2.0811(19) ?
Co1 O4 . 3_555 2.0811(19) ?
O2 C5 . . 1.2616(13) ?
O3 C5 . . 1.2495(13) ?
O4 C6 . . 1.4169(15) ?
C5 C6 . . 1.5075(13) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Co1 O2 2_555 . 4_444 180.0(5) ?
O2 Co1 O3 2_555 . . 91.39(4) ?
O2 Co1 O3 2_555 . 3_555 88.61(4) ?
O2 Co1 O4 2_555 . . 87.78(5) ?
O2 Co1 O4 2_555 . 3_555 92.22(5) ?
O2 Co1 O3 4_444 . . 88.61(4) ?
O2 Co1 O3 4_444 . 3_555 91.39(4) ?
O2 Co1 O4 4_444 . . 92.22(5) ?
O2 Co1 O4 4_444 . 3_555 87.78(5) ?
O3 Co1 O3 . . 3_555 180.0(5) ?
O3 Co1 O4 . . . 78.40(4) ?
O3 Co1 O4 . . 3_555 101.60(4) ?
O3 Co1 O4 3_555 . . 101.60(4) ?
O3 Co1 O4 3_555 . 3_555 78.40(4) ?
O4 Co1 O4 . . 3_555 180.0(5) ?
Co1 O2 C5 2_545 . . 134.29(5) ?
Co1 O3 C5 . . . 116.45(5) ?
Co1 O4 C6 . . . 113.38(5) ?
O2 C5 O3 . . . 122.74(6) ?
O2 C5 C6 . . . 118.02(5) ?
O3 C5 C6 . . . 119.24(5) ?
O4 C6 C5 . . . 109.40(5) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O4 H7 O2 . . 4_544 0.992(2) 1.661(2) 2.652(2) 176.92(11) ?
O4 H7 C5 . . 4_544 0.992(2) 2.426(3) 3.329(2) 151.11(11) ?
C6 H8 O3 . . 1_655 1.088(2) 2.330(3) 3.282(4) 145.14(16) ?
C6 H9 O3 . . 2_545 1.0918(18) 2.480(3) 3.194(3) 121.86(13) ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_298K_neutron_bgCo
_database_code_depnum_ccdc_archive 'CCDC 1876543'
_audit_update_record             
;
2018-11-27 deposited with the CCDC.
2018-11-28 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_formula_sum            'C4 H6 Co1 O6'
_chemical_formula_weight         209

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

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x+1/2,-y+1/2,z+1/2

_cell_length_a                   5.180(3)
_cell_length_b                   7.860(5)
_cell_length_c                   8.659(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.129(8)
_cell_angle_gamma                90
_cell_volume                     340.3(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    27
_cell_measurement_theta_min      4.66
_cell_measurement_theta_max      59.18
_cell_measurement_temperature    298(1)

_exptl_crystal_density_diffrn    2.0397
_exptl_crystal_F_000             210
_exptl_absorpt_coefficient_mu    0
_exptl_crystal_description       prism
_exptl_crystal_size_max          5
_exptl_crystal_size_mid          2
_exptl_crystal_size_min          2
_exptl_crystal_colour            orange
_exptl_absorpt_correction_type   none

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

# 7. EXPERIMENTAL DATA

_diffrn_ambient_temperature      298(1)
_diffrn_radiation_type           neutron
_diffrn_radiation_source         'J-PARC neutron spallation source'
_diffrn_radiation_wavelength     '0.4 - 4.4'
_diffrn_radiation_wavelength_details 'Based on neutron time of flight'
_diffrn_measurement_device       '2-cirle goniometer'
_diffrn_measurement_device_type  
'single-crystal diffractometer SENJU at the BL18 in the MLF of the J-PARC'
_diffrn_measurement_method       'time-of-flight Laue'
_diffrn_reflns_number            6757
_diffrn_reflns_theta_min         4.66
_diffrn_reflns_theta_max         59.18
_diffrn_reflns_theta_full        20.49
_diffrn_measured_fraction_theta_max 0.53
_diffrn_measured_fraction_theta_full 0.85
_diffrn_reflns_av_R_equivalents  0.124
_diffrn_reflns_av_unetI/netI     0.1669
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_radiation_probe          neutron

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

# 8. REFINEMENT DATA

_refine_special_details          
; The neutron diffraction data was collected using a closed-cycle helium refrigerator equipped with the 2-axes piezo-motor goniometer (omega, phi and 45 deg. fixed chi). The crystal structure was refined using the result of the X-ray structural analysis as initial parameters. Anisotropic displacement parameters were applied for all atoms inclusing hydrogen atoms.
;

_reflns_number_total             6757
_reflns_number_gt                3083
_reflns_threshold_expression     I>3σ(I)
_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.0783
_refine_ls_wR_factor_gt          0.1070
_refine_ls_R_factor_all          0.1976
_refine_ls_wR_factor_ref         0.1392
_refine_ls_goodness_of_fit_ref   1.11
_refine_ls_goodness_of_fit_gt    1.24
_refine_ls_number_reflns         6757
_refine_ls_number_parameters     90
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(F)+0.0049F²)
_refine_ls_hydrogen_treatment    refall
_refine_ls_shift/su_max          0.0051
_refine_ls_shift/su_mean         0.0010
_refine_diff_density_max         8.27
_refine_diff_density_min         -5.12
_refine_ls_extinction_method     
'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_extinction_coef       26.0(9)

loop_
_atom_type_symbol
_atom_type_scat_length_neutron
_atom_type_scat_source
C 6.646 International_Tables_Vol_C
H -3.739 International_Tables_Vol_C
Co 2.490 International_Tables_Vol_C
O 5.803 International_Tables_Vol_C

_computing_data_collection       STARGazer
_computing_cell_refinement       STARGazer
_computing_data_reduction        'JANA2006(Petricek et al., 2006)'
_computing_structure_solution    'JANA2006(Petricek et al., 2006)'
_computing_structure_refinement  'JANA2006(Petricek et al., 2006)'
_computing_molecular_graphics    'VESTA(Momma & Izumi, 2011)'
_computing_publication_material  'JANA2006(Petricek et al., 2006)'

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

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0 0 0 Uani 0.0111(5) 2 1 d . . .
O2 O 0.18864(19) -0.35091(11) 0.35666(9) Uani 0.0201(2) 4 1 d . . .
O3 O -0.01555(19) -0.15002(10) 0.19119(9) Uani 0.0172(2) 4 1 d . . .
O4 O 0.28566(18) -0.18588(10) -0.00742(9) Uani 0.0179(2) 4 1 d . . .
C5 C 0.16304(13) -0.26071(7) 0.23275(7) Uani 0.01324(16) 4 1 d . . .
C6 C 0.3561(2) -0.28807(12) 0.13063(10) Uani 0.0277(3) 4 1 d . . .
H7 H 0.4376(4) -0.1754(2) -0.0573(2) Uani 0.0279(5) 4 1 d . . .
H8 H 0.5552(5) -0.2565(5) 0.2015(3) Uani 0.0869(15) 4 1 d . . .
H9 H 0.3521(10) -0.4216(3) 0.0987(4) Uani 0.0870(17) 4 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co1 Co 0.0125(10) 0.0118(8) 0.0088(8) 0.0010(5) 0.0028(6) 0.0013(5)
O2 O 0.0183(4) 0.0281(4) 0.0165(3) 0.0085(3) 0.0093(3) 0.0105(3)
O3 O 0.0198(4) 0.0189(3) 0.0162(3) 0.0060(2) 0.0108(3) 0.0067(2)
O4 O 0.0190(4) 0.0224(4) 0.0156(3) 0.0063(2) 0.0104(3) 0.0054(2)
C5 C 0.0118(3) 0.0170(3) 0.0123(2) 0.00235(16) 0.00563(18) 0.00401(17)
C6 C 0.0267(5) 0.0375(4) 0.0257(4) 0.0190(3) 0.0191(3) 0.0186(3)
H7 H 0.0301(10) 0.0333(7) 0.0257(7) 0.0027(6) 0.0168(6) 0.0028(5)
H8 H 0.0229(15) 0.194(4) 0.0453(15) 0.0169(19) 0.0115(11) 0.0537(19)
H9 H 0.158(4) 0.0442(13) 0.098(2) 0.0499(17) 0.103(3) 0.0342(14)

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

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 O2 . 2_555 2.114(2) ?
Co1 O2 . 4_444 2.114(2) ?
Co1 O3 . . 2.051(2) ?
Co1 O3 . 3_555 2.051(2) ?
Co1 O4 . . 2.092(2) ?
Co1 O4 . 3_555 2.092(2) ?
O2 C5 . . 1.2638(16) ?
O3 C5 . . 1.2524(15) ?
O4 C6 . . 1.4069(18) ?
C5 C6 . . 1.5133(16) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Co1 O2 2_555 . 4_444 180.0(5) ?
O2 Co1 O3 2_555 . . 91.69(5) ?
O2 Co1 O3 2_555 . 3_555 88.31(5) ?
O2 Co1 O4 2_555 . . 88.16(6) ?
O2 Co1 O4 2_555 . 3_555 91.84(6) ?
O2 Co1 O3 4_444 . . 88.31(5) ?
O2 Co1 O3 4_444 . 3_555 91.69(5) ?
O2 Co1 O4 4_444 . . 91.84(6) ?
O2 Co1 O4 4_444 . 3_555 88.16(6) ?
O3 Co1 O3 . . 3_555 180.0(5) ?
O3 Co1 O4 . . . 78.49(4) ?
O3 Co1 O4 . . 3_555 101.51(4) ?
O3 Co1 O4 3_555 . . 101.51(4) ?
O3 Co1 O4 3_555 . 3_555 78.49(4) ?
O4 Co1 O4 . . 3_555 180.0(5) ?
Co1 O2 C5 2_545 . . 134.77(8) ?
Co1 O3 C5 . . . 116.72(7) ?
Co1 O4 C6 . . . 113.66(7) ?
O2 C5 O3 . . . 122.66(9) ?
O2 C5 C6 . . . 118.52(8) ?
O3 C5 C6 . . . 118.82(8) ?
O4 C6 C5 . . . 110.54(8) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O4 H7 O2 . . 4_544 0.995(3) 1.672(3) 2.666(2) 177.52(16) ?
O4 H7 C5 . . 4_544 0.995(3) 2.456(3) 3.370(3) 152.52(14) ?
C6 H8 O3 . . 1_655 1.082(3) 2.399(4) 3.340(4) 144.5(2) ?
C6 H9 O3 . . 2_545 1.085(3) 2.539(4) 3.239(4) 121.4(2) ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_20K_neutron_bgCo
_database_code_depnum_ccdc_archive 'CCDC 1876542'
_audit_update_record             
;
2018-11-27 deposited with the CCDC.
2018-11-28 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_formula_sum            'C4 H6 Co1 O6'
_chemical_formula_weight         209

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

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x+1/2,-y+1/2,z+1/2

_cell_length_a                   5.170(3)
_cell_length_b                   7.697(5)
_cell_length_c                   8.701(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.492(8)
_cell_angle_gamma                90
_cell_volume                     335.2(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    90
_cell_measurement_theta_min      5.08
_cell_measurement_theta_max      68.8
_cell_measurement_temperature    20.0(5)

_exptl_crystal_density_diffrn    2.0707
_exptl_crystal_F_000             210
_exptl_absorpt_coefficient_mu    0
_exptl_crystal_description       prism
_exptl_crystal_size_max          5
_exptl_crystal_size_mid          2
_exptl_crystal_size_min          2
_exptl_crystal_colour            orange
_exptl_absorpt_correction_type   none

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

# 7. EXPERIMENTAL DATA

_diffrn_ambient_temperature      20.0(5)
_diffrn_radiation_type           neutron
_diffrn_radiation_source         'J-PARC neutron spallation source'
_diffrn_radiation_wavelength     '0.4 - 4.4'
_diffrn_radiation_wavelength_details 'Based on neutron time of flight'
_diffrn_measurement_device       '2-cirle goniometer'
_diffrn_measurement_device_type  
'single-crystal diffractometer SENJU at the BL18 in the MLF of the J-PARC'
_diffrn_detector_area_resol_mean '4 mm'
_diffrn_measurement_method       'time-of-flight Laue'
_diffrn_reflns_number            5477
_diffrn_reflns_theta_min         5.08
_diffrn_reflns_theta_max         68.85
_diffrn_reflns_theta_full        25.87
_diffrn_measured_fraction_theta_max 0.52
_diffrn_measured_fraction_theta_full 0.79
_diffrn_reflns_av_R_equivalents  0.0811
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_radiation_probe          neutron

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

# 8. REFINEMENT DATA

_refine_special_details          
; The neutron diffraction data was collected using a closed-cycle helium refrigerator equipped with the 2-axes piezo-motor goniometer (omega, phi and 45 deg. fixed chi). The crystal structure was refined using the result of the X-ray structural analysis as initial parameters. Anisotropic displacement parameters were applied for all atoms inclusing hydrogen atoms.
;

_reflns_number_total             5477
_reflns_number_gt                4204
_reflns_threshold_expression     I>3σ(I)
_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.0680
_refine_ls_wR_factor_gt          0.1116
_refine_ls_R_factor_all          0.0889
_refine_ls_wR_factor_ref         0.1242
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_goodness_of_fit_gt    1.11
_refine_ls_number_reflns         5477
_refine_ls_number_parameters     89
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(F)+0.0081F²)
_refine_ls_hydrogen_treatment    refall
_refine_ls_shift/su_max          0.0067
_refine_ls_shift/su_mean         0.0009
_refine_diff_density_max         11.88
_refine_diff_density_min         -4.96
_refine_ls_extinction_method     
'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_extinction_coef       22.6(8)

loop_
_atom_type_symbol
_atom_type_scat_length_neutron
_atom_type_scat_source
C 6.646 International_Tables_Vol_C
H -3.739 International_Tables_Vol_C
Co 2.490 International_Tables_Vol_C
O 5.803 International_Tables_Vol_C

_computing_data_collection       STARGazer
_computing_cell_refinement       STARGazer
_computing_data_reduction        'JANA2006(Petricek et al., 2006)'
_computing_structure_solution    'JANA2006(Petricek et al., 2006)'
_computing_structure_refinement  'JANA2006(Petricek et al., 2006)'
_computing_molecular_graphics    'VESTA(Momma & Izumi, 2011)'
_computing_publication_material  'JANA2006(Petricek et al., 2006)'

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

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0 0 0 Uani 0.0015(3) 2 1 d . . .
O2 O 0.18337(12) -0.35653(6) 0.35518(6) Uani 0.00387(12) 4 1 d . . .
O3 O -0.02483(12) -0.15520(6) 0.18689(6) Uani 0.00361(13) 4 1 d . . .
O4 O 0.27822(13) -0.19389(6) -0.01113(6) Uani 0.00381(13) 4 1 d . . .
C5 C 0.15715(10) -0.26626(5) 0.23034(5) Uani 0.00260(11) 4 1 d . . .
C6 C 0.35566(12) -0.29444(6) 0.13024(6) Uani 0.00516(12) 4 1 d . . .
H7 H 0.4322(3) -0.17879(16) -0.05971(17) Uani 0.0158(3) 4 1 d . . .
H8 H 0.5555(4) -0.2563(2) 0.2008(2) Uani 0.0253(5) 4 1 d . . .
H9 H 0.3586(4) -0.43374(16) 0.1022(2) Uani 0.0260(5) 4 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co1 Co 0.0023(7) 0.0019(4) 0.0005(4) 0.0000(3) 0.0003(3) -0.0003(3)
O2 O 0.0044(3) 0.00481(14) 0.00251(18) 0.00134(11) 0.00109(13) 0.00216(10)
O3 O 0.0043(3) 0.00350(15) 0.00342(19) 0.00155(11) 0.00170(13) 0.00142(9)
O4 O 0.0046(3) 0.00435(15) 0.00303(18) 0.00118(11) 0.00201(13) 0.00094(10)
C5 C 0.0035(2) 0.00225(12) 0.00233(16) 0.00050(9) 0.00118(11) 0.00065(8)
C6 C 0.0052(3) 0.00667(14) 0.00454(18) 0.00304(11) 0.00293(13) 0.00300(9)
H7 H 0.0144(7) 0.0203(4) 0.0149(5) 0.0026(4) 0.0078(4) 0.0040(3)
H8 H 0.0116(10) 0.0448(8) 0.0177(6) -0.0020(6) 0.0002(5) 0.0078(5)
H9 H 0.0444(13) 0.0125(4) 0.0272(7) 0.0108(5) 0.0206(7) 0.0047(4)

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

# 10. MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 O2 . 2_555 2.111(2) ?
Co1 O2 . 4_444 2.111(2) ?
Co1 O3 . . 2.0475(18) ?
Co1 O3 . 3_555 2.0475(18) ?
Co1 O4 . . 2.0916(19) ?
Co1 O4 . 3_555 2.0916(19) ?
O2 C5 . . 1.2679(13) ?
O3 C5 . . 1.2573(13) ?
O4 C6 . . 1.4234(15) ?
C5 C6 . . 1.5187(13) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Co1 O2 2_555 . 4_444 180.0(5) ?
O2 Co1 O3 2_555 . . 91.40(4) ?
O2 Co1 O3 2_555 . 3_555 88.60(4) ?
O2 Co1 O4 2_555 . . 87.78(5) ?
O2 Co1 O4 2_555 . 3_555 92.22(5) ?
O2 Co1 O3 4_444 . . 88.60(4) ?
O2 Co1 O3 4_444 . 3_555 91.40(4) ?
O2 Co1 O4 4_444 . . 92.22(5) ?
O2 Co1 O4 4_444 . 3_555 87.78(5) ?
O3 Co1 O3 . . 3_555 180.0(5) ?
O3 Co1 O4 . . . 78.52(4) ?
O3 Co1 O4 . . 3_555 101.48(4) ?
O3 Co1 O4 3_555 . . 101.48(4) ?
O3 Co1 O4 3_555 . 3_555 78.52(4) ?
O4 Co1 O4 . . 3_555 180.0(5) ?
Co1 O2 C5 2_545 . . 134.34(5) ?
Co1 O3 C5 . . . 116.40(5) ?
Co1 O4 C6 . . . 113.32(5) ?
O2 C5 O3 . . . 122.81(6) ?
O2 C5 C6 . . . 118.06(5) ?
O3 C5 C6 . . . 119.13(5) ?
O4 C6 C5 . . . 109.49(6) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O4 H7 O2 . . 4_544 0.997(2) 1.670(2) 2.667(2) 176.99(12) ?
O4 H7 C5 . . 4_544 0.997(2) 2.436(2) 3.346(2) 151.57(11) ?
C6 H8 O3 . . 1_655 1.101(2) 2.337(3) 3.295(4) 144.43(15) ?
C6 H9 O3 . . 2_545 1.1005(19) 2.495(3) 3.211(3) 121.58(12) ?
