#------------------------------------------------------------------------------
#$Date: 2019-11-24 06:00:41 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236887 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/98/4349840.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_4349840
loop_
_publ_author_name
'Oliveira, Willian X. C.'
'Pereira, Cynthia L. M.'
'Pinheiro, Carlos B.'
'Lloret, Francesc'
'Julve, Miguel'
_publ_section_title
;
 Towards oxalate-bridged iron(ii), cobalt(ii), nickel(ii) and zinc(ii)
 complexes through oxotris(oxalato)niobate(v): an open air non-oxidizing
 synthetic route
;
_journal_issue                   6
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1294
_journal_paper_doi               10.1039/C8QI00191J
_journal_volume                  5
_journal_year                    2018
_chemical_formula_sum            'C62 H60 Cl2 Co2 N8 O14 S2'
_chemical_formula_weight         1394.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-01-19 deposited with the CCDC.
2018-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                82.207(8)
_cell_angle_beta                 84.709(8)
_cell_angle_gamma                71.837(9)
_cell_formula_units_Z            1
_cell_length_a                   10.3328(10)
_cell_length_b                   12.2165(12)
_cell_length_c                   13.0629(12)
_cell_measurement_reflns_used    4987
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.4790
_cell_measurement_theta_min      2.3460
_cell_volume                     1550.1(3)
_computing_cell_refinement       'CysAlisPro 171.37.34b'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'CysAlisPro 171.37.34b'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SuperFlip (Palatinus & Chapius, 2007)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported S'
_diffrn_measurement_method       'ω and π scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43439
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.282
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Thu Jun 18 12:11:23 2015'
;
_exptl_crystal_colour            Plate
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_meas      Pink
_exptl_crystal_description
;
'Thu Jun 18 12:11:23 2015'
;
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0611P)²+1.3647P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1409
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4523
_reflns_number_total             6331
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8qi00191j2.cif
_cod_data_source_block           shelx_CCDC2
_cod_database_code               4349840
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.863
_shelx_estimated_absorpt_t_max   0.942
loop_
_space_group_symop_operation_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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4267(3) 0.5278(3) 0.4812(2) 0.0302(6) Uani 1 1 d . . . . .
C2 C 0.5562(5) 0.8915(4) 0.1930(3) 0.0679(11) Uani 1 1 d . . . . .
H2A H 0.6265 0.8404 0.2353 0.102 Uiso 1 1 calc R U . . .
H2B H 0.4976 0.9502 0.2326 0.102 Uiso 1 1 calc R U . . .
H2C H 0.5968 0.9274 0.1342 0.102 Uiso 1 1 calc R U . . .
C3 C 0.4750(4) 0.8241(3) 0.1569(3) 0.0514(9) Uani 1 1 d . . . . .
C4 C 0.3753(5) 0.8785(4) 0.0828(3) 0.0681(12) Uani 1 1 d . . . . .
H4 H 0.3594 0.9565 0.0587 0.082 Uiso 1 1 calc R U . . .
C5 C 0.3031(4) 0.8170(4) 0.0471(3) 0.0727(13) Uani 1 1 d . . . . .
H5 H 0.2343 0.8542 0.0018 0.087 Uiso 1 1 calc R U . . .
C6 C 0.3316(3) 0.6990(4) 0.0778(3) 0.0552(10) Uani 1 1 d . . . . .
C7 C 0.2667(4) 0.6266(5) 0.0384(3) 0.0654(12) Uani 1 1 d . . . . .
H7 H 0.1948 0.6604 -0.0049 0.078 Uiso 1 1 calc R U . . .
C8 C 0.3070(4) 0.5120(5) 0.0625(3) 0.0658(12) Uani 1 1 d . . . . .
H8 H 0.2626 0.4674 0.0358 0.079 Uiso 1 1 calc R U . . .
C9 C 0.4174(4) 0.4562(4) 0.1286(3) 0.0507(9) Uani 1 1 d . . . . .
C10 C 0.4705(4) 0.3361(4) 0.1500(3) 0.0612(11) Uani 1 1 d . . . . .
H10 H 0.4291 0.2878 0.1258 0.073 Uiso 1 1 calc R U . . .
C11 C 0.5823(5) 0.2902(4) 0.2060(3) 0.0593(10) Uani 1 1 d . . . . .
H11 H 0.6208 0.2102 0.2170 0.071 Uiso 1 1 calc R U . . .
C12 C 0.6408(4) 0.3630(3) 0.2477(3) 0.0475(8) Uani 1 1 d . . . . .
C13 C 0.7714(4) 0.3103(3) 0.3018(3) 0.0618(11) Uani 1 1 d . . . . .
H13A H 0.7978 0.3703 0.3266 0.093 Uiso 1 1 calc R U . . .
H13B H 0.8416 0.2710 0.2543 0.093 Uiso 1 1 calc R U . . .
H13C H 0.7585 0.2559 0.3591 0.093 Uiso 1 1 calc R U . . .
C14 C 0.4796(3) 0.5246(3) 0.1728(2) 0.0406(8) Uani 1 1 d . . . . .
C15 C 0.4346(3) 0.6478(3) 0.1478(2) 0.0429(8) Uani 1 1 d . . . . .
C16 C 0.8685(4) 0.5467(4) 0.1388(3) 0.0531(9) Uani 1 1 d . . . . .
H16A H 0.7737 0.5517 0.1423 0.080 Uiso 1 1 calc R U . . .
H16B H 0.9228 0.4701 0.1250 0.080 Uiso 1 1 calc R U . . .
H16C H 0.8858 0.6024 0.0843 0.080 Uiso 1 1 calc R U . . .
C17 C 0.9047(3) 0.5714(3) 0.2393(2) 0.0397(7) Uani 1 1 d . . . . .
C18 C 1.0419(3) 0.5473(3) 0.2615(3) 0.0507(9) Uani 1 1 d . . . . .
H18 H 1.1104 0.5107 0.2151 0.061 Uiso 1 1 calc R U . . .
C19 C 1.0754(3) 0.5765(3) 0.3492(3) 0.0502(9) Uani 1 1 d . . . . .
H19 H 1.1664 0.5583 0.3643 0.060 Uiso 1 1 calc R U . . .
C20 C 0.9712(3) 0.6349(3) 0.4177(3) 0.0409(8) Uani 1 1 d . . . . .
C21 C 0.9980(4) 0.6746(4) 0.5091(3) 0.0548(10) Uani 1 1 d . . . . .
H21 H 1.0876 0.6585 0.5271 0.066 Uiso 1 1 calc R U . . .
C22 C 0.8953(4) 0.7349(4) 0.5694(3) 0.0543(10) Uani 1 1 d . . . . .
H22 H 0.9149 0.7596 0.6288 0.065 Uiso 1 1 calc R U . . .
C23 C 0.7559(4) 0.7618(3) 0.5438(3) 0.0438(8) Uani 1 1 d . . . . .
C24 C 0.6450(4) 0.8303(3) 0.5999(3) 0.0556(10) Uani 1 1 d . . . . .
H24 H 0.6594 0.8572 0.6598 0.067 Uiso 1 1 calc R U . . .
C25 C 0.5174(4) 0.8574(3) 0.5673(3) 0.0555(10) Uani 1 1 d . . . . .
H25 H 0.4447 0.9055 0.6032 0.067 Uiso 1 1 calc R U . . .
C26 C 0.4941(3) 0.8130(3) 0.4791(3) 0.0458(8) Uani 1 1 d . . . . .
C27 C 0.3533(4) 0.8480(4) 0.4394(3) 0.0616(11) Uani 1 1 d . . . . .
H27A H 0.3441 0.9105 0.3848 0.092 Uiso 1 1 calc R U . . .
H27B H 0.2869 0.8727 0.4947 0.092 Uiso 1 1 calc R U . . .
H27C H 0.3390 0.7830 0.4134 0.092 Uiso 1 1 calc R U . . .
C28 C 0.7262(3) 0.7200(3) 0.4571(2) 0.0343(7) Uani 1 1 d . . . . .
C29 C 0.8363(3) 0.6549(3) 0.3924(2) 0.0332(7) Uani 1 1 d . . . . .
N1 N 0.5884(3) 0.4784(2) 0.23375(19) 0.0375(6) Uani 1 1 d . . . . .
N2 N 0.5010(3) 0.7125(3) 0.1908(2) 0.0415(6) Uani 1 1 d . . . . .
N3 N 0.8039(2) 0.6197(2) 0.30541(19) 0.0347(6) Uani 1 1 d . . . . .
N4 N 0.5970(2) 0.7427(2) 0.42612(19) 0.0358(6) Uani 1 1 d . . . . .
O1 O 0.66691(19) 0.49490(19) 0.46078(15) 0.0361(5) Uani 1 1 d . . . . .
O2 O 0.4139(2) 0.59026(19) 0.39599(16) 0.0371(5) Uani 1 1 d . . . . .
Co1 Co 0.59968(4) 0.61265(4) 0.32512(3) 0.03432(15) Uani 1 1 d . . . . .
Cl1 Cl 0.15677(10) 0.19726(9) 0.11127(8) 0.0593(3) Uani 1 1 d . . . . .
O3 O 0.1921(5) 0.1133(4) 0.1972(3) 0.1245(16) Uani 1 1 d . . . . .
O4 O 0.0434(7) 0.1909(8) 0.0754(6) 0.222(4) Uani 1 1 d . . . . .
O5 O 0.1369(6) 0.3052(4) 0.1449(5) 0.159(2) Uani 1 1 d . . . . .
O6 O 0.2630(5) 0.1799(4) 0.0358(4) 0.1393(19) Uani 1 1 d . . . . .
O7 O 0.7689(5) 1.0200(5) 0.2951(5) 0.164(2) Uani 1 1 d . . . . .
S1A S 0.88038(15) 0.91905(19) 0.28383(15) 0.0759(8) Uani 0.775(6) 1 d . . P A 1
S1B S 0.8806(9) 1.0039(10) 0.2473(11) 0.137(5) Uani 0.225(6) 1 d . . P A 2
C30 C 0.9446(9) 0.9192(9) 0.1586(6) 0.173(4) Uani 1 1 d . . . . .
H30A H 1.0416 0.9038 0.1571 0.260 Uiso 1 1 calc R U . A 1
H30B H 0.9041 0.9935 0.1210 0.260 Uiso 1 1 calc R U . A 1
H30C H 0.9240 0.8603 0.1272 0.260 Uiso 1 1 calc R U . A 1
C31 C 1.0212(9) 0.9408(9) 0.3373(7) 0.191(5) Uani 1 1 d . . . . .
H31A H 1.0358 1.0114 0.3042 0.286 Uiso 1 1 calc R U . A 1
H31B H 1.1014 0.8769 0.3264 0.286 Uiso 1 1 calc R U . A 1
H31C H 1.0026 0.9459 0.4101 0.286 Uiso 1 1 calc R U . A 1
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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
O1 C1 O2 126.7(3) 2_666 .
O1 C1 C1 116.2(3) 2_666 2_666
O2 C1 C1 117.1(3) . 2_666
N2 C3 C4 120.8(4) . .
N2 C3 C2 119.4(3) . .
C4 C3 C2 119.7(4) . .
C5 C4 C3 120.3(4) . .
C4 C5 C6 120.4(4) . .
C5 C6 C15 117.4(4) . .
C5 C6 C7 123.8(4) . .
C15 C6 C7 118.8(4) . .
C8 C7 C6 121.5(4) . .
C7 C8 C9 121.2(4) . .
C10 C9 C14 117.3(3) . .
C10 C9 C8 123.6(4) . .
C14 C9 C8 119.1(4) . .
C11 C10 C9 119.8(3) . .
C10 C11 C12 120.3(4) . .
N1 C12 C11 121.7(3) . .
N1 C12 C13 119.0(3) . .
C11 C12 C13 119.1(4) . .
N1 C14 C9 122.9(3) . .
N1 C14 C15 117.5(3) . .
C9 C14 C15 119.4(3) . .
N2 C15 C6 122.2(4) . .
N2 C15 C14 117.9(3) . .
C6 C15 C14 119.9(3) . .
N3 C17 C18 121.3(3) . .
N3 C17 C16 118.2(3) . .
C18 C17 C16 120.4(3) . .
C19 C18 C17 120.8(3) . .
C18 C19 C20 119.4(3) . .
C29 C20 C19 117.2(3) . .
C29 C20 C21 119.9(3) . .
C19 C20 C21 122.9(3) . .
C22 C21 C20 120.7(3) . .
C21 C22 C23 121.2(3) . .
C28 C23 C24 116.8(3) . .
C28 C23 C22 119.3(3) . .
C24 C23 C22 123.9(3) . .
C25 C24 C23 120.3(3) . .
C24 C25 C26 120.2(3) . .
N4 C26 C25 121.2(3) . .
N4 C26 C27 118.4(3) . .
C25 C26 C27 120.3(3) . .
N4 C28 C23 123.4(3) . .
N4 C28 C29 117.0(3) . .
C23 C28 C29 119.6(3) . .
N3 C29 C20 122.6(3) . .
N3 C29 C28 118.1(2) . .
C20 C29 C28 119.2(3) . .
C12 N1 C14 117.8(3) . .
C12 N1 Co1 131.3(2) . .
C14 N1 Co1 108.1(2) . .
C3 N2 C15 118.6(3) . .
C3 N2 Co1 131.2(2) . .
C15 N2 Co1 109.0(2) . .
C17 N3 C29 118.4(3) . .
C17 N3 Co1 130.2(2) . .
C29 N3 Co1 109.08(18) . .
C26 N4 C28 118.0(3) . .
C26 N4 Co1 131.4(2) . .
C28 N4 Co1 107.95(19) . .
C1 O1 Co1 114.69(18) 2_666 .
C1 O2 Co1 114.48(17) . .
N3 Co1 O2 161.19(9) . .
N3 Co1 N2 105.25(10) . .
O2 Co1 N2 92.54(9) . .
N3 Co1 O1 85.52(9) . .
O2 Co1 O1 77.36(8) . .
N2 Co1 O1 168.16(9) . .
N3 Co1 N4 77.61(10) . .
O2 Co1 N4 92.37(9) . .
N2 Co1 N4 104.10(10) . .
O1 Co1 N4 82.73(9) . .
N3 Co1 N1 106.79(10) . .
O2 Co1 N1 82.65(9) . .
N2 Co1 N1 77.55(10) . .
O1 Co1 N1 94.84(9) . .
N4 Co1 N1 174.85(9) . .
O4 Cl1 O6 111.4(4) . .
O4 Cl1 O5 111.2(5) . .
O6 Cl1 O5 108.0(3) . .
O4 Cl1 O3 108.5(4) . .
O6 Cl1 O3 110.3(3) . .
O5 Cl1 O3 107.4(3) . .
O7 S1A C30 110.3(5) . .
O7 S1A C31 106.5(5) . .
C30 S1A C31 96.8(5) . .
O7 S1B C30 128.3(9) . .
O7 S1B C31 110.5(10) . .
C30 S1B C31 96.9(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.250(3) 2_666
C1 O2 1.254(4) .
C1 C1 1.550(5) 2_666
C2 C3 1.487(6) .
C3 N2 1.325(5) .
C3 C4 1.422(5) .
C4 C5 1.359(7) .
C5 C6 1.388(6) .
C6 C15 1.405(5) .
C6 C7 1.433(6) .
C7 C8 1.332(7) .
C8 C9 1.431(6) .
C9 C10 1.396(6) .
C9 C14 1.407(5) .
C10 C11 1.350(6) .
C11 C12 1.407(5) .
C12 N1 1.337(4) .
C12 C13 1.499(5) .
C14 N1 1.366(4) .
C14 C15 1.430(5) .
C15 N2 1.394(4) .
C16 C17 1.491(5) .
C17 N3 1.330(4) .
C17 C18 1.404(5) .
C18 C19 1.350(5) .
C19 C20 1.409(5) .
C20 C29 1.401(4) .
C20 C21 1.428(5) .
C21 C22 1.343(5) .
C22 C23 1.434(5) .
C23 C28 1.399(4) .
C23 C24 1.401(5) .
C24 C25 1.350(5) .
C25 C26 1.407(5) .
C26 N4 1.343(4) .
C26 C27 1.504(5) .
C28 N4 1.364(4) .
C28 C29 1.443(4) .
C29 N3 1.371(4) .
N1 Co1 2.192(3) .
N2 Co1 2.140(3) .
N3 Co1 2.129(2) .
N4 Co1 2.190(3) .
O1 C1 1.250(3) 2_666
O1 Co1 2.146(2) .
O2 Co1 2.133(2) .
Cl1 O4 1.329(5) .
Cl1 O6 1.391(4) .
Cl1 O5 1.395(4) .
Cl1 O3 1.405(4) .
O7 S1B 1.233(11) .
O7 S1A 1.415(5) .
S1A C30 1.708(8) .
S1A C31 1.777(7) .
S1B C30 1.615(13) .
S1B C31 1.859(12) .
