# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_co_calc-topas-35
_database_code_depnum_ccdc_archive 'CCDC 1951490'
loop_
_audit_author_name
_audit_author_address
'Artem Dmitrienko'
;INEOS RAS
Russia
;
_audit_update_record             
;
2019-09-04 deposited with the CCDC.	2020-04-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT341_co_calc-topas-35    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04875 Ang.
RESPONSE: Bond precision is typical for Rietveld refined structures
;
# Added during the CSD deposition process: Wednesday 04 September 2019 02:47 PM
# end Validation Reply Form


# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H14 Co N8 O4'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' 
_chemical_formula_structural     ?
_chemical_formula_sum            'C20 H14 Co N8 O4'
_chemical_formula_iupac          ?
_chemical_formula_weight         489.32
_chemical_compound_source        'see text'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0179 0.0091 'S.Brennan & P.L.Cowan (1992).Rev.Sci.Instr.,63,650'
H H 0.0000 0.0000 'S.Brennan & P.L.Cowan (1992).Rev.Sci.Instr.,63,650'
Co Co -2.3614 3.6150 'S.Brennan & P.L.Cowan (1992).Rev.Sci.Instr.,63,650'
N N 0.0311 0.0180 'S.Brennan & P.L.Cowan (1992).Rev.Sci.Instr.,63,650'
O O 0.0495 0.0323 'S.Brennan & P.L.Cowan (1992).Rev.Sci.Instr.,63,650'

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


# 6. CRYSTAL DATA (replace F000 and xyz with PLATON data, fill exp. details)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_Int_Tables_number      15

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z


_cell_length_a                   13.2282(8)
_cell_length_b                   11.9400(7)
_cell_length_c                   13.5364(8)
_cell_angle_alpha                90
_cell_angle_beta                 100.2941(15)
_cell_angle_gamma                90
_cell_volume                     2103.6(2)
_cell_formula_units_Z            4
_exptl_crystal_description       powder
_diffrn_radiation_wavelength     1.540596


_exptl_crystal_density_diffrn    1.545
_exptl_absorpt_coefficient_mu    6.799
_exptl_crystal_F_000             996



_cell_measurement_temperature    298

_pd_spec_mounting                
; 
deposited on sticky tape 
;
_pd_spec_mount_mode              transmission # options are reflection
# or transmission

_pd_spec_shape                   flat_sheet # options are cylinder
# flat_sheet OR irregular

_pd_char_particle_morphology     round
_pd_char_colour                  white # use ICDD colour descriptions




_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?


_exptl_absorpt_correction_type   analytical

_exptl_absorpt_process_details   
;
International Tables Vol C Tables 2.3.1.20
 A(Th) = (t/cos(Th)) exp(-s/cos(Th))
refined coefficients are
 s =  ??
 t =  ??
;
#===============================================================================

# 7. EXPERIMENTAL DATA (leave as is)


_exptl_special_details           ?

_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a~1~
_diffrn_radiation_source         ?
_diffrn_radiation_monochromator  
;
Ge 111
;
_diffrn_ambient_temperature      298
_diffrn_source                   
;
sealed X-ray tube
;
_diffrn_source_target            Cu
_diffrn_measurement_device_type  
;
Bruker D8 Advance Vario
;
_diffrn_detector                 
;
1D linear
;
_diffrn_detector_type            
;
Bruker LynxEye compound silicon strip 1D linear detector 
;
_pd_meas_scan_method             cont

_computing_data_collection       
;
Bruker XRD Commander 2.6 (Bruker, 2007)
;
_computing_cell_refinement       
;
TOPAS 4.2 (Coelho, 2003; Bruker, 2009)
;
_computing_data_reduction        
;
TOPAS 4.2 (Coelho, 2003; Bruker, 2009)
;
_computing_structure_solution    
;
FOX 1.9.7.0 (Favre-Nicolin, Cerny, 2002)
;
_computing_structure_refinement  
;
TOPAS 4.2 (Coelho, 2003; Bruker, 2009)
;
_computing_molecular_graphics    
;
OLEX2 1.2 (Dolomanov et al., 2009, 2)
;
_computing_publication_material  
;
PLATON (Spek, 2003)
;

#Beware: these are values as defined by start_X and finish_X.
# Real measurerement range may differ
_pd_meas_number_of_points        39126
_pd_meas_2theta_range_min        8.002353
_pd_meas_2theta_range_max        89.998965
_pd_meas_2theta_range_inc        0.002096
#===============================================================================

# 8. REFINEMENT DATA (fill in the blanks, here PLATON will not help)

_pd_proc_ls_special_details      ?
_pd_proc_ls_profile_function     'fundamental parameters'
_pd_proc_ls_background_function  
;
16th order Chebyshev polynomial 
;
_pd_proc_ls_pref_orient_corr     
;

6th order hkl dependent symmetrized spherical harmonics series (Jarvinen 1993).

The coefficients used were:

y00   =   1
y20   =   0.64352
y22m  =  -0.38554
y22p  =   0.47366
y40   =  -0.18585
y42m  =  -0.80079
y42p  =  -0.04380
y44m  =  -0.49765
y44p  =   0.07654
y60   =  -0.04866
y62m  =  -0.17992
y62p  =  -0.10668
y64m  =  -0.06465
y64p  =  -0.26717
y66m  =  -0.14348
y66p  =  -0.20678 

;

_pd_proc_ls_prof_R_factor        0.00462
_pd_proc_ls_prof_wR_factor       0.00717
_pd_proc_ls_prof_wR_expected     0.00089
_refine_ls_goodness_of_fit_all   8.014
_refine_ls_R_I_factor            0.0032

_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     1/Yi
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

_refine_ls_number_parameters     100
_refine_ls_number_restraints     32
_refine_ls_number_constraints    0

_pd_proc_2theta_range_min        8.002353
_pd_proc_2theta_range_max        89.998965
_pd_proc_2theta_range_inc        0.002096
_pd_proc_wavelength              1.540596

_pd_block_diffractogram_id       co_raw


# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co Uiso 0.75000 0.25000 0.00000 1.000 0.11(4) . . . .
O1 O Uiso 0.2875(15) 0.2131(16) 0.1097(13) 1.000 0.11(4) . . . .
O2 O Uiso 0.1861(14) 0.2002(15) 0.3622(14) 1.000 0.11(4) . . . .
N1 N Uiso 0.3886(19) 0.4751(17) 0.1536(17) 1.000 0.11(4) . . . .
N2 N Uiso 0.6218(15) 0.2940(15) 0.0496(16) 1.000 0.11(4) . . . .
N3 N Uiso 0.6068(14) 0.0262(17) 0.1583(15) 1.000 0.11(4) . . . .
N4 N Uiso 0.3148(19) -0.101(2) 0.0304(17) 1.000 0.11(4) . . . .
C1 C Uiso 0.418(2) 0.387(2) 0.134(2) 1.000 0.11(4) . . . .
C2 C Uiso 0.453(3) 0.283(2) 0.111(2) 1.000 0.11(4) . . . .
C3 C Uiso 0.546(2) 0.287(2) 0.077(2) 1.000 0.11(4) . . . .
C4 C Uiso 0.522(2) 0.048(2) 0.130(2) 1.000 0.11(4) . . . .
C5 C Uiso 0.420(3) 0.075(3) 0.097(2) 1.000 0.11(4) . . . .
C6 C Uiso 0.359(2) -0.018(3) 0.0611(19) 1.000 0.11(4) . . . .
C7 C Uiso 0.385(2) 0.186(4) 0.102(2) 1.000 0.11(4) . . . .
C8 C Uiso 0.2203(19) 0.131(2) 0.149(2) 1.000 0.11(4) . . . .
C9 C Uiso 0.1275(19) 0.193(3) 0.1767(19) 1.000 0.11(4) . . . .
C10 C Uiso 0.1520(19) 0.2657(19) 0.272(3) 1.000 0.11(4) . . . .
H1 H Uiso 0.10070 0.24700 0.12740 1.000 0.1393 . . . .
H2 H Uiso 0.07450 0.14000 0.17910 1.000 0.1393 . . . .
H3 H Uiso 0.19590 0.08900 0.09000 1.000 0.1393 . . . .
H4 H Uiso 0.25390 0.08400 0.20100 1.000 0.1393 . . . .
H5 H Uiso 0.09270 0.30160 0.28800 1.000 0.1393 . . . .
H6 H Uiso 0.20150 0.32250 0.26800 1.000 0.1393 . . . .
H7 H Uiso 0.14590 0.13240 0.36340 1.000 0.1393 . . . .

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

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N2 2.00(2) . . yes
Co1 O2 1.996(19) . 2_655 yes
Co1 N4 1.99(2) . 3_655 yes
Co1 N4 1.99(2) . 5_555 yes
Co1 N2 2.00(2) . 7_655 yes
Co1 O2 1.996(19) . 8_554 yes
O1 C7 1.35(3) . . yes
O1 C8 1.48(3) . . yes
O2 C10 1.45(4) . . yes
N1 C1 1.17(3) . . yes
N2 C3 1.13(3) . . yes
O2 H7 0.9700 . . no
N3 C4 1.15(3) . . yes
N4 C6 1.19(4) . . yes
C1 C2 1.38(4) . . no
C2 C7 1.46(5) . . no
C2 C3 1.39(5) . . no
C4 C5 1.38(5) . . no
C5 C6 1.41(5) . . no
C5 C7 1.41(6) . . no
C8 C9 1.54(4) . . no
C9 C10 1.54(5) . . no
C8 H3 0.9500 . . no
C8 H4 0.9500 . . no
C9 H1 0.9500 . . no
C9 H2 0.9500 . . no
C10 H5 0.9500 . . no
C10 H6 0.9500 . . no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 N2 90.4(8) 2_655 . . yes
N2 Co1 N4 86.8(9) . . 3_655 yes
N2 Co1 N4 93.2(9) . . 5_555 yes
N2 Co1 N2 180.00 . . 7_655 yes
O2 Co1 N2 89.6(8) 8_554 . . yes
O2 Co1 N4 91.3(8) 2_655 . 3_655 yes
O2 Co1 N4 88.8(8) 2_655 . 5_555 yes
O2 Co1 N2 89.6(8) 2_655 . 7_655 yes
O2 Co1 O2 180.00 2_655 . 8_554 yes
N4 Co1 N4 180.00 3_655 . 5_555 yes
N2 Co1 N4 93.2(9) 7_655 . 3_655 yes
O2 Co1 N4 88.8(8) 8_554 . 3_655 yes
N2 Co1 N4 86.8(9) 7_655 . 5_555 yes
O2 Co1 N4 91.3(8) 8_554 . 5_555 yes
O2 Co1 N2 90.4(8) 8_554 . 7_655 yes
C7 O1 C8 121(3) . . . yes
Co1 O2 C10 129.9(16) 2_655 . . yes
Co1 N2 C3 160.5(19) . . . yes
Co1 O2 H7 112.00 2_655 . . no
C10 O2 H7 112.00 . . . no
Co1 N4 C6 171(2) 3_655 . . yes
N1 C1 C2 180(4) . . . yes
C3 C2 C7 125(3) . . . no
C1 C2 C7 120(3) . . . no
C1 C2 C3 113(2) . . . no
N2 C3 C2 178(3) . . . yes
N3 C4 C5 179(4) . . . yes
C6 C5 C7 126(3) . . . no
C4 C5 C6 113(3) . . . no
C4 C5 C7 121(3) . . . no
N4 C6 C5 175(3) . . . yes
O1 C7 C5 124(3) . . . yes
C2 C7 C5 123(3) . . . no
O1 C7 C2 113(4) . . . yes
O1 C8 C9 109(2) . . . yes
C8 C9 C10 115(2) . . . no
O2 C10 C9 113(2) . . . yes
O1 C8 H3 101.00 . . . no
O1 C8 H4 115.00 . . . no
C9 C8 H3 107.00 . . . no
C9 C8 H4 113.00 . . . no
H3 C8 H4 111.00 . . . no
C8 C9 H1 112.00 . . . no
C8 C9 H2 108.00 . . . no
C10 C9 H1 102.00 . . . no
C10 C9 H2 113.00 . . . no
H1 C9 H2 107.00 . . . no
O2 C10 H5 101.00 . . . no
O2 C10 H6 109.00 . . . no
C9 C10 H5 113.00 . . . no
C9 C10 H6 113.00 . . . no
H5 C10 H6 107.00 . . . no

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 O1 C8 C9 164(2) . . . . no
C8 O1 C7 C2 -152(2) . . . . no
C8 O1 C7 C5 22(4) . . . . no
Co1 O2 C10 C9 168.2(16) 2_655 . . . no
C3 C2 C7 C5 27(4) . . . . no
C1 C2 C7 C5 -168(3) . . . . no
C1 C2 C7 O1 5(4) . . . . no
C3 C2 C7 O1 -160(3) . . . . no
C4 C5 C7 O1 -153(3) . . . . no
C4 C5 C7 C2 20(4) . . . . no
C6 C5 C7 C2 -161(3) . . . . no
C6 C5 C7 O1 26(4) . . . . no
O1 C8 C9 C10 -73(3) . . . . no
C8 C9 C10 O2 -65(3) . . . . no

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
#
#D   H   A   D - H  H...A   D...A    D - H...A  symm(A)
#
O2 H7 N1 0.9700 1.9400 2.86(3) 158.00 6_545 yes
C8 H4 N3 0.9500 2.5000 3.39(3) 156.00 2_655 yes

# Loop Mechanism for Extra Tables(s)

#loop_
#_publ_manuscript_incl_extra_item
#'_geom_extra_tableA_col_1'
#'_geom_extra_tableA_col_2'
#'_geom_extra_tableA_col_3'
#'_geom_extra_table_head_A'
#'_geom_table_footnote_A'
#'_geom_extra_tableB_col_1'
#'_geom_extra_tableB_col_2'
#'_geom_extra_tableB_col_3'
#'_geom_extra_table_head_B'
#'_geom_table_footnote_B'


#
#loop_
#_geom_extra_tableA_col_1
#_geom_extra_tableA_col_2
#_geom_extra_tableA_col_3
# ? ? ?


#
#loop_
#_geom_extra_tableB_col_1
#_geom_extra_tableB_col_2
#_geom_extra_tableB_col_3
# ? ? ?


#
#_geom_table_footnote_A
#;
# ?
#;


#
#_geom_table_footnote_B
#;
# ?
#;


#
#_geom_table_footnote_A
#;
# ?
#;


#
#_geom_table_footnote_B
#;
# ?
#;

####################################################################### 
# 
# 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_ni_hs-topas-7
_database_code_depnum_ccdc_archive 'CCDC 1951491'
loop_
_audit_author_name
_audit_author_address
'Artem Dmitrienko'
;INEOS RAS
Russia
;
_audit_update_record             
;
2019-09-04 deposited with the CCDC.	2020-04-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT341_ni_hs-topas-7       
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.035 Ang.
RESPONSE: Bond precision is typical for Rietveld refined structures
;
# Added during the CSD deposition process: Wednesday 04 September 2019 02:47 PM
# end Validation Reply Form


_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H14 N8 Ni O4'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' 
_chemical_formula_structural     ?
_chemical_formula_sum            'C20 H14 N8 Ni O4'
_chemical_formula_iupac          ?
_chemical_formula_weight         489.08
_chemical_compound_source        'see text'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0179 0.0091 'S.Brennan & P.L.Cowan (1992).Rev.Sci.Instr.,63,650'
H H 0.0000 0.0000 'S.Brennan & P.L.Cowan (1992).Rev.Sci.Instr.,63,650'
N N 0.0311 0.0180 'S.Brennan & P.L.Cowan (1992).Rev.Sci.Instr.,63,650'
Ni Ni -3.0002 0.5100 'S.Brennan & P.L.Cowan (1992).Rev.Sci.Instr.,63,650'
O O 0.0495 0.0323 'S.Brennan & P.L.Cowan (1992).Rev.Sci.Instr.,63,650'

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

# 6. CRYSTAL DATA (replace F000 and xyz with PLATON data, fill exp. details)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_Int_Tables_number      15

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z


_cell_length_a                   13.4879(5)
_cell_length_b                   11.8449(5)
_cell_length_c                   13.4309(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.269(2)
_cell_angle_gamma                90
_cell_volume                     2096.76(14)
_cell_formula_units_Z            4
_diffrn_radiation_wavelength     1.540596



_exptl_crystal_density_diffrn    1.549
_exptl_absorpt_coefficient_mu    1.745
_exptl_crystal_F_000             1000
_exptl_crystal_description       powder


_cell_measurement_temperature    298

_pd_spec_mounting                
; 
deposited on sticky tape 
;
_pd_spec_mount_mode              transmission # options are reflection
# or transmission

_pd_spec_shape                   flat_sheet # options are cylinder
# flat_sheet OR irregular

_pd_char_particle_morphology     round
_pd_char_colour                  white # use ICDD colour descriptions




_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?


_exptl_absorpt_correction_type   none


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

# 7. EXPERIMENTAL DATA (leave as is)


_exptl_special_details           ?

_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a~1~
_diffrn_radiation_source         ?
_diffrn_radiation_monochromator  
;
Ge 111
;
_diffrn_ambient_temperature      298
_diffrn_source                   
;
sealed X-ray tube
;
_diffrn_source_target            Cu
_diffrn_measurement_device_type  
;
Bruker D8 Advance Vario
;
_diffrn_detector                 
;
1D linear
;
_diffrn_detector_type            
;
Bruker LynxEye compound silicon strip 1D linear detector 
;
_pd_meas_scan_method             cont

_computing_data_collection       
;
Bruker XRD Commander 2.6 (Bruker, 2007)
;
_computing_cell_refinement       
;
TOPAS 5.0 (Coelho, 2003; Bruker, 2009)
;
_computing_data_reduction        
;
TOPAS 5.0 (Coelho, 2003; Bruker, 2009)
;
_computing_structure_solution    
;
FOX 1.9.7.0 (Favre-Nicolin, Cerny, 2002)
;
_computing_structure_refinement  
;
TOPAS 5.0 (Coelho, 2003; Bruker, 2009)
;
_computing_molecular_graphics    
;
OLEX2 1.2 (Dolomanov et al., 2009, 2)
;
_computing_publication_material  
;
PLATON (Spek, 2003)
;

#Beware: these are values as defined by start_X and finish_X.
# Real measurerement range may differ
_pd_meas_number_of_points        39131
_pd_meas_2theta_range_min        8.004352
_pd_meas_2theta_range_max        90.011443
_pd_meas_2theta_range_inc        0.002096
#===============================================================================

# 8. REFINEMENT DATA 

_pd_proc_ls_special_details      ?
_pd_proc_ls_profile_function     'fundamental parameters'

_pd_proc_ls_background_function  
;
16
;
_pd_proc_ls_pref_orient_corr     
;

6th order hkl dependent symmetrized spherical harmonics series (Jarvinen 1993).

The coefficients used were:

 
y00   =  1 
y20   =  0.50011
y22m  = -0.60275
y22p  =  0.10176
y40   =  0.16754
y42m  = -0.46047
y42p  = -0.37728
y44m  = -0.36898
y44p  = -0.30576
y60   =  0.34170
y62m  =  0.09603
y62p  = -0.05131
y64m  =  0.15324
y64p  = -0.11661
y66m  =  0.00964
y66p  = -0.31502


;

_pd_proc_ls_prof_R_factor        0.02117
_pd_proc_ls_prof_wR_factor       0.02958
_pd_proc_ls_prof_wR_expected     0.01972
_refine_ls_goodness_of_fit_all   1.500
_refine_ls_R_I_factor            0.00104

_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     1/Yi
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

_refine_ls_number_parameters     112
_refine_ls_number_restraints     32
_refine_ls_number_constraints    0

_pd_proc_2theta_range_min        8.004352
_pd_proc_2theta_range_max        90.011443
_pd_proc_2theta_range_inc        0.002096
_pd_proc_wavelength              1.540596

_pd_block_diffractogram_id       ni_raw

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni Uiso 0.75000 0.25000 0.00000 1.000 0.112(10) . . . .
O1 O Uiso 0.2767(9) 0.2135(13) 0.1107(9) 1.000 0.112(10) . . . .
O2 O Uiso 0.1968(10) 0.2000(13) 0.3583(11) 1.000 0.112(10) . . . .
N1 N Uiso 0.3719(10) 0.4740(15) 0.1588(12) 1.000 0.112(10) . . . .
N2 N Uiso 0.6155(11) 0.2768(13) 0.0619(13) 1.000 0.112(10) . . . .
N3 N Uiso 0.6033(10) 0.0225(15) 0.1554(11) 1.000 0.112(10) . . . .
N4 N Uiso 0.3057(12) -0.1034(19) 0.0386(12) 1.000 0.112(10) . . . .
C1 C Uiso 0.4042(15) 0.386(2) 0.1393(14) 1.000 0.112(10) . . . .
C2 C Uiso 0.4407(15) 0.280(2) 0.1163(16) 1.000 0.112(10) . . . .
C3 C Uiso 0.5345(16) 0.279(2) 0.0853(16) 1.000 0.112(10) . . . .
C4 C Uiso 0.5163(14) 0.046(2) 0.1313(14) 1.000 0.112(10) . . . .
C5 C Uiso 0.4127(16) 0.073(3) 0.1022(14) 1.000 0.112(10) . . . .
C6 C Uiso 0.3523(17) -0.020(2) 0.0674(17) 1.000 0.112(10) . . . .
C7 C Uiso 0.3763(13) 0.185(3) 0.1091(14) 1.000 0.112(10) . . . .
C8 C Uiso 0.2066(14) 0.130(2) 0.1374(15) 1.000 0.112(10) . . . .
C9 C Uiso 0.1208(14) 0.1926(16) 0.1750(17) 1.000 0.112(10) . . . .
C10 C Uiso 0.1570(11) 0.2673(17) 0.2694(17) 1.000 0.112(10) . . . .
H1 H Uiso 0.09130 0.24420 0.12290 1.000 0.1343 . . . .
H2 H Uiso 0.07070 0.13740 0.17890 1.000 0.1343 . . . .
H3 H Uiso 0.18360 0.08600 0.07740 1.000 0.1343 . . . .
H4 H Uiso 0.24110 0.08200 0.19090 1.000 0.1343 . . . .
H5 H Uiso 0.09760 0.29810 0.28610 1.000 0.1343 . . . .
H6 H Uiso 0.20110 0.32840 0.26350 1.000 0.1343 . . . .
H7 H Uiso 0.16190 0.12850 0.35870 1.000 0.1343 . . . .

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

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 2.174(16) . . yes
Ni1 O2 1.977(15) . 2_655 yes
Ni1 N4 1.92(2) . 3_655 yes
Ni1 N4 1.92(2) . 5_555 yes
Ni1 N2 2.174(16) . 7_655 yes
Ni1 O2 1.977(15) . 8_554 yes
O1 C7 1.39(2) . . yes
O1 C8 1.47(3) . . yes
O2 C10 1.44(3) . . yes
N1 C1 1.18(3) . . yes
N2 C3 1.20(3) . . yes
O2 H7 0.9700 . . no
N3 C4 1.18(2) . . yes
N4 C6 1.19(3) . . yes
C1 C2 1.41(3) . . no
C2 C7 1.41(4) . . no
C2 C3 1.41(3) . . no
C4 C5 1.41(3) . . no
C5 C6 1.39(4) . . no
C5 C7 1.43(5) . . no
C8 C9 1.55(3) . . no
C9 C10 1.54(3) . . no
C8 H3 0.9500 . . no
C8 H4 0.9600 . . no
C9 H1 0.9500 . . no
C9 H2 0.9500 . . no
C10 H5 0.9500 . . no
C10 H6 0.9500 . . no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 N2 80.6(6) 2_655 . . yes
N2 Ni1 N4 85.7(6) . . 3_655 yes
N2 Ni1 N4 94.3(6) . . 5_555 yes
N2 Ni1 N2 180.00 . . 7_655 yes
O2 Ni1 N2 99.4(6) 8_554 . . yes
O2 Ni1 N4 91.7(7) 2_655 . 3_655 yes
O2 Ni1 N4 88.3(7) 2_655 . 5_555 yes
O2 Ni1 N2 99.4(6) 2_655 . 7_655 yes
O2 Ni1 O2 180.00 2_655 . 8_554 yes
N4 Ni1 N4 180.00 3_655 . 5_555 yes
N2 Ni1 N4 94.3(6) 7_655 . 3_655 yes
O2 Ni1 N4 88.3(7) 8_554 . 3_655 yes
N2 Ni1 N4 85.7(6) 7_655 . 5_555 yes
O2 Ni1 N4 91.7(7) 8_554 . 5_555 yes
O2 Ni1 N2 80.6(6) 8_554 . 7_655 yes
C7 O1 C8 121.1(19) . . . yes
Ni1 O2 C10 128.8(13) 2_655 . . yes
Ni1 N2 C3 169.8(16) . . . yes
Ni1 O2 H7 109.00 2_655 . . no
C10 O2 H7 113.00 . . . no
Ni1 N4 C6 171.1(18) 3_655 . . yes
N1 C1 C2 179(2) . . . yes
C3 C2 C7 123(2) . . . no
C1 C2 C7 119(2) . . . no
C1 C2 C3 117(2) . . . no
N2 C3 C2 178(2) . . . yes
N3 C4 C5 180(3) . . . yes
C6 C5 C7 125(2) . . . no
C4 C5 C6 113(3) . . . no
C4 C5 C7 122(2) . . . no
N4 C6 C5 176(2) . . . yes
O1 C7 C5 125(2) . . . yes
C2 C7 C5 122.1(19) . . . no
O1 C7 C2 113(3) . . . yes
O1 C8 C9 108.8(17) . . . yes
C8 C9 C10 114.6(16) . . . no
O2 C10 C9 111.2(16) . . . yes
O1 C8 H3 106.00 . . . no
O1 C8 H4 110.00 . . . no
C9 C8 H3 114.00 . . . no
C9 C8 H4 109.00 . . . no
H3 C8 H4 109.00 . . . no
C8 C9 H1 107.00 . . . no
C8 C9 H2 106.00 . . . no
C10 C9 H1 104.00 . . . no
C10 C9 H2 117.00 . . . no
H1 C9 H2 107.00 . . . no
O2 C10 H5 102.00 . . . no
O2 C10 H6 111.00 . . . no
C9 C10 H5 106.00 . . . no
C9 C10 H6 118.00 . . . no
H5 C10 H6 108.00 . . . no

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 O1 C8 C9 157.3(16) . . . . no
C8 O1 C7 C2 -159.8(17) . . . . no
C8 O1 C7 C5 20(3) . . . . no
Ni1 O2 C10 C9 -178.2(11) 2_655 . . . no
C3 C2 C7 C5 21(3) . . . . no
C1 C2 C7 C5 -169.9(18) . . . . no
C1 C2 C7 O1 10(3) . . . . no
C3 C2 C7 O1 -159.7(18) . . . . no
C4 C5 C7 O1 -160.4(18) . . . . no
C4 C5 C7 C2 19(3) . . . . no
C6 C5 C7 C2 -161(2) . . . . no
C6 C5 C7 O1 19(3) . . . . no
O1 C8 C9 C10 -60(2) . . . . no
C8 C9 C10 O2 -68(2) . . . . no

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
#
#D   H   A   D - H  H...A   D...A    D - H...A  symm(A)
#
O2 H7 N1 0.9700 1.8900 2.83(2) 162.00 6_545 yes

# Loop Mechanism for Extra Tables(s)

#loop_
#_publ_manuscript_incl_extra_item
#'_geom_extra_tableA_col_1'
#'_geom_extra_tableA_col_2'
#'_geom_extra_tableA_col_3'
#'_geom_extra_table_head_A'
#'_geom_table_footnote_A'
#'_geom_extra_tableB_col_1'
#'_geom_extra_tableB_col_2'
#'_geom_extra_tableB_col_3'
#'_geom_extra_table_head_B'
#'_geom_table_footnote_B'


#
#loop_
#_geom_extra_tableA_col_1
#_geom_extra_tableA_col_2
#_geom_extra_tableA_col_3
# ? ? ?


#
#loop_
#_geom_extra_tableB_col_1
#_geom_extra_tableB_col_2
#_geom_extra_tableB_col_3
# ? ? ?


#
#_geom_table_footnote_A
#;
# ?
#;


#
#_geom_table_footnote_B
#;
# ?
#;


#
#_geom_table_footnote_A
#;
# ?
#;


#
#_geom_table_footnote_B
#;
# ?
#;

