#------------------------------------------------------------------------------
#$Date: 2023-11-23 11:33:10 +0200 (Thu, 23 Nov 2023) $
#$Revision: 287753 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/23/7702315.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7702315
loop_
_publ_author_name
'Brechin, Euan K.'
'Gilby, Liam M.'
'Gould, Robert O.'
'Harris, Steven G.'
'Parsons, Simon'
'Winpenny, Richard E. P.'
_publ_section_title
;
 Heterobimetallic nickel--sodium and cobalt--sodium complexes of
 pyridonate ligands
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2657
_journal_paper_doi               10.1039/a803442g
_journal_year                    1998
_chemical_formula_sum            'C30 H18 Cl6 Co2 N6 Na2 O6'
_chemical_formula_weight         935.04
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                112.204(10)
_cell_angle_beta                 93.119(14)
_cell_angle_gamma                105.192(13)
_cell_formula_units_Z            1
_cell_length_a                   7.2614(19)
_cell_length_b                   11.316(2)
_cell_length_c                   12.105(3)
_cell_measurement_temperature    220(2)
_cell_volume                     875.5(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_sigmaI/netI    0.1036
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3702
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.981
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_obs          0.0538
_refine_ls_shift/esd_max         0.014
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0502P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1196
_refine_ls_wR_factor_obs         0.1019
_reflns_number_observed          1959
_reflns_number_total             3100
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            g803442.txt
_cod_data_source_block           cosnat
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 

2023-11-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C15 H9 Cl3 Co N3 Na O3'
_cod_original_formula_weight         467.52
_cod_original_formula_units_Z            2
_cod_original_cell_volume        875.5(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702315
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.41994(11) 0.44619(8) 0.59286(7) 0.0218(2) Uani 1 d .
Na1 Na 0.0069(3) 0.4211(2) 0.3606(2) 0.0285(6) Uani 1 d .
N11 N 0.2356(6) 0.2657(4) 0.5934(4) 0.0224(11) Uani 1 d .
C21 C 0.0715(8) 0.2917(5) 0.5621(5) 0.0223(13) Uani 1 d .
O21 O 0.1074(5) 0.3923(4) 0.5320(3) 0.0245(9) Uani 1 d .
C31 C -0.1111(8) 0.2154(6) 0.5690(6) 0.0326(15) Uani 1 d .
H31 H -0.2253 0.2298 0.5444 0.039 Uiso 1 calc R
C41 C -0.1170(8) 0.1202(6) 0.6125(6) 0.0327(16) Uani 1 d .
H41 H -0.2381 0.0692 0.6185 0.039 Uiso 1 calc R
C51 C 0.0479(8) 0.0949(6) 0.6483(6) 0.0302(15) Uani 1 d .
H51 H 0.0430 0.0300 0.6796 0.036 Uiso 1 calc R
C61 C 0.2180(8) 0.1711(6) 0.6350(5) 0.0275(14) Uani 1 d .
Cl1 Cl 0.4352(2) 0.14431(18) 0.67180(16) 0.0400(4) Uani 1 d .
N12 N 0.4357(7) 0.5367(5) 0.7861(4) 0.0252(11) Uani 1 d .
C22 C 0.6335(8) 0.5805(6) 0.8039(5) 0.0261(13) Uani 1 d .
O22 O 0.7037(5) 0.5401(4) 0.7063(4) 0.0299(10) Uani 1 d .
C32 C 0.7382(9) 0.6623(6) 0.9218(5) 0.0337(16) Uani 1 d .
H32 H 0.8741 0.6950 0.9348 0.040 Uiso 1 calc R
C42 C 0.6411(9) 0.6936(7) 1.0169(6) 0.0419(18) Uani 1 d .
H42 H 0.7111 0.7474 1.0956 0.050 Uiso 1 calc R
C52 C 0.4404(9) 0.6471(7) 0.9991(6) 0.0382(17) Uani 1 d .
H52 H 0.3716 0.6671 1.0639 0.046 Uiso 1 calc R
C62 C 0.3478(8) 0.5701(6) 0.8814(6) 0.0296(15) Uani 1 d .
Cl2 Cl 0.0955(2) 0.5054(2) 0.84970(16) 0.0469(5) Uani 1 d .
N13 N 0.6753(6) 0.2471(5) 0.3012(4) 0.0240(11) Uani 1 d .
C23 C 0.5179(8) 0.2666(5) 0.3504(5) 0.0225(13) Uani 1 d .
O23 O 0.5434(5) 0.3830(4) 0.4418(3) 0.0234(9) Uani 1 d .
C33 C 0.3365(8) 0.1695(6) 0.3036(5) 0.0268(14) Uani 1 d .
H33 H 0.2279 0.1834 0.3392 0.032 Uiso 1 calc R
C43 C 0.3197(8) 0.0530(6) 0.2044(6) 0.0317(15) Uani 1 d .
H43 H 0.1977 -0.0119 0.1707 0.038 Uiso 1 calc R
C53 C 0.4788(8) 0.0305(6) 0.1542(6) 0.0284(14) Uani 1 d .
H53 H 0.4712 -0.0492 0.0877 0.034 Uiso 1 calc R
C63 C 0.6495(8) 0.1319(6) 0.2074(5) 0.0252(13) Uani 1 d .
Cl3 Cl 0.8615(2) 0.11267(18) 0.14881(17) 0.0471(5) Uani 1 d .
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'
Cl Cl 0.1484 0.1585 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O23 Co1 O23 83.40(15) . 2_666
O23 Co1 N11 104.14(16) . .
O23 Co1 N11 150.05(16) 2_666 .
O23 Co1 N12 152.05(16) . .
O23 Co1 N12 98.71(16) 2_666 .
N11 Co1 N12 87.96(17) . .
O23 Co1 O22 90.57(15) . .
O23 Co1 O22 88.72(15) 2_666 .
N11 Co1 O22 119.66(17) . .
N12 Co1 O22 61.74(16) . .
O23 Co1 O21 107.40(15) . .
O23 Co1 O21 88.52(14) 2_666 .
N11 Co1 O21 61.53(15) . .
N12 Co1 O21 100.52(16) . .
O22 Co1 O21 161.36(14) . .
O22 Na1 O21 99.10(16) 2_666 .
O22 Na1 O21 119.23(16) 2_666 2_566
O21 Na1 O21 95.37(14) . 2_566
O22 Na1 N13 140.60(18) 2_666 1_455
O21 Na1 N13 96.60(15) . 1_455
O21 Na1 N13 94.80(15) 2_566 1_455
O22 Na1 Cl2 78.30(12) 2_666 2_566
O21 Na1 Cl2 173.07(14) . 2_566
O21 Na1 Cl2 80.54(11) 2_566 2_566
N13 Na1 Cl2 89.34(13) 1_455 2_566
O22 Na1 Cl3 90.21(12) 2_666 1_455
O21 Na1 Cl3 103.04(13) . 1_455
O21 Na1 Cl3 142.29(12) 2_566 1_455
N13 Na1 Cl3 50.96(12) 1_455 1_455
Cl2 Na1 Cl3 83.47(8) 2_566 1_455
C61 N11 C21 118.2(4) . .
C61 N11 Co1 146.1(4) . .
C21 N11 Co1 92.7(3) . .
O21 C21 N11 112.8(4) . .
O21 C21 C31 126.8(5) . .
N11 C21 C31 120.4(5) . .
C21 O21 Co1 92.0(3) . .
C21 O21 Na1 134.0(4) . .
Co1 O21 Na1 117.91(16) . .
C21 O21 Na1 119.1(3) . 2_566
Co1 O21 Na1 109.60(16) . 2_566
Na1 O21 Na1 84.63(14) . 2_566
C41 C31 C21 117.8(6) . .
C31 C41 C51 122.8(5) . .
C61 C51 C41 115.3(5) . .
N11 C61 C51 125.5(5) . .
N11 C61 Cl1 114.9(4) . .
C51 C61 Cl1 119.6(5) . .
C62 N12 C22 118.7(5) . .
C62 N12 Co1 149.8(4) . .
C22 N12 Co1 91.4(3) . .
O22 C22 N12 113.6(5) . .
O22 C22 C32 126.9(5) . .
N12 C22 C32 119.5(5) . .
C22 O22 Co1 93.1(3) . .
C22 O22 Na1 139.6(4) . 2_666
Co1 O22 Na1 125.68(19) . 2_666
C42 C32 C22 119.6(6) . .
C32 C42 C52 120.9(6) . .
C62 C52 C42 116.3(6) . .
N12 C62 C52 125.0(6) . .
N12 C62 Cl2 115.2(5) . .
C52 C62 Cl2 119.8(5) . .
C62 Cl2 Na1 102.2(2) . 2_566
C63 N13 C23 116.9(5) . .
C63 N13 Na1 117.6(3) . 1_655
C23 N13 Na1 125.2(4) . 1_655
O23 C23 N13 116.6(5) . .
O23 C23 C33 122.2(5) . .
N13 C23 C33 121.1(5) . .
C23 O23 Co1 134.7(3) . .
C23 O23 Co1 119.0(3) . 2_666
Co1 O23 Co1 96.60(15) . 2_666
C43 C33 C23 118.9(5) . .
C53 C43 C33 120.8(6) . .
C63 C53 C43 115.5(6) . .
N13 C63 C53 126.8(5) . .
N13 C63 Cl3 114.4(4) . .
C53 C63 Cl3 118.9(5) . .
C63 Cl3 Na1 76.8(2) . 1_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O23 2.0451(36) .
Co1 O23 2.0831(37) 2_666
Co1 N11 2.1314(43) .
Co1 N12 2.1525(48) .
Co1 O22 2.1682(40) .
Co1 O21 2.1951(36) .
Na1 O22 2.2885(41) 2_666
Na1 O21 2.3270(44) .
Na1 O21 2.4088(44) 2_566
Na1 N13 2.5392(50) 1_455
Na1 Cl2 3.0731(28) 2_566
Na1 Cl3 3.2982(30) 1_455
N11 C61 1.3261(68) .
N11 C21 1.3672(69) .
C21 O21 1.2906(60) .
C21 C31 1.4059(71) .
O21 Na1 2.4088(44) 2_566
C31 C41 1.3592(81) .
C41 C51 1.3853(81) .
C51 C61 1.3647(76) .
C61 Cl1 1.7473(59) .
N12 C62 1.3258(70) .
N12 C22 1.3672(70) .
C22 O22 1.2819(66) .
C22 C32 1.4089(82) .
O22 Na1 2.2885(41) 2_666
C32 C42 1.3632(81) .
C42 C52 1.3871(86) .
C52 C62 1.3759(86) .
C62 Cl2 1.7453(57) .
Cl2 Na1 3.0731(28) 2_566
N13 C63 1.3244(71) .
N13 C23 1.3480(66) .
N13 Na1 2.5392(50) 1_655
C23 O23 1.3196(65) .
C23 C33 1.3978(74) .
O23 Co1 2.0831(36) 2_666
C33 C43 1.3778(81) .
C43 C53 1.3722(78) .
C53 C63 1.3706(78) .
C63 Cl3 1.7602(54) .
Cl3 Na1 3.2982(30) 1_655
