#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:31:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179144 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/05/4310576.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_4310576
loop_
_publ_author_name
'Patrice M. T. Piggot'
'Lincoln A. Hall'
'Andrew J. P. White'
'David J. Williams'
'Laurence K. Thompson'
_publ_section_title
;
 Synthesis, Structure, and Magnetochemical Analysis of Selected First-Row
 Transition-Metal Anilino- and Anisolesquarate Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1167
_journal_page_last               1174
_journal_paper_doi               10.1021/ic035193g
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C22 H20 Co N2 O8'
_chemical_formula_weight         499.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.506(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7529(15)
_cell_length_b                   11.3372(12)
_cell_length_c                   9.0443(10)
_cell_measurement_temperature    150(2)
_cell_volume                     991.5(2)
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Nonius Kappa CCD'
_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  0.0763
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6314
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.8973
_exptl_absorpt_correction_T_min  0.8089
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Orange/red
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       needles
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0151(48)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.131
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1606
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.127
_refine_ls_restrained_S_obs      1.130
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_obs          0.0526
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0523P)²+0.7459P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1530
_refine_ls_wR_factor_obs         0.1265
_reflns_number_observed          1212
_reflns_number_total             1744
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic035193gsi20031015_051854_2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.7459P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.7459P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4310576
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_group
Co Co 0.0000 0.0000 0.0000 0.0424(4) Uani 1 d S .
O1 O -0.0415(3) 0.1180(2) 0.1609(3) 0.0478(8) Uani 1 d . .
C1 C 0.0249(5) 0.1489(3) 0.2835(5) 0.0451(12) Uani 1 d . .
O2 O -0.0141(3) 0.3596(2) 0.3465(3) 0.0467(8) Uani 1 d . .
C2 C 0.0398(5) 0.2592(4) 0.3667(4) 0.0442(11) Uani 1 d . .
O3 O 0.2174(3) 0.2367(3) 0.5932(3) 0.0630(11) Uani 1 d . .
C3 C 0.1420(5) 0.2020(4) 0.4794(5) 0.0495(12) Uani 1 d . .
C4 C 0.1218(5) 0.0926(3) 0.3960(5) 0.0439(11) Uani 1 d . .
N5 N 0.1653(4) -0.0187(3) 0.4056(4) 0.0469(10) Uani 1 d D .
H5 H 0.1191(39) -0.0717(27) 0.3439(36) 0.044(12) Uiso 1 d D .
C6 C 0.2672(3) -0.1910(2) 0.5294(3) 0.0524(13) Uani 1 d G .
H6A H 0.1971(3) -0.2366(2) 0.4732(3) 0.063 Uiso 1 calc R .
C7 C 0.3678(4) -0.2460(2) 0.6290(4) 0.064(2) Uani 1 d G .
H7A H 0.3664(5) -0.3292(2) 0.6410(6) 0.076 Uiso 1 calc R .
C8 C 0.4703(4) -0.1792(2) 0.7112(4) 0.073(2) Uani 1 d G .
H8A H 0.5391(5) -0.2168(3) 0.7793(6) 0.088 Uiso 1 calc R .
C9 C 0.4724(4) -0.0575(2) 0.6936(5) 0.100(3) Uani 1 d G .
H9A H 0.5425(5) -0.0118(3) 0.7498(7) 0.120 Uiso 1 calc R .
C10 C 0.3718(4) -0.0025(2) 0.5940(5) 0.085(2) Uani 1 d G .
H10A H 0.3732(6) 0.0808(2) 0.5820(7) 0.102 Uiso 1 calc R .
C11 C 0.2692(3) -0.0692(2) 0.5119(4) 0.0505(13) Uani 1 d G .
O20 O 0.2117(4) 0.0324(3) 0.0547(4) 0.0537(9) Uani 1 d D .
H20 H 0.2280(73) 0.1089(16) 0.0771(70) 0.116(26) Uiso 1 d D .
C21 C 0.2917(7) 0.0288(5) -0.0577(9) 0.088(2) Uani 1 d . .
H21A H 0.3880(7) 0.0453(5) -0.0176(9) 0.132 Uiso 1 calc R .
H21B H 0.2591(7) 0.0882(5) -0.1329(9) 0.132 Uiso 1 calc R .
H21C H 0.2855(7) -0.0497(5) -0.1035(9) 0.132 Uiso 1 calc R .
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'
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
O1 Co O1 180.0 3 . ?
O1 Co O20 90.12(13) 3 . ?
O1 Co O20 89.88(13) . . ?
O1 Co O20 89.88(13) 3 3 ?
O1 Co O20 90.12(13) . 3 ?
O20 Co O20 180.0 . 3 ?
O1 Co O2 88.43(11) 3 2_545 ?
O1 Co O2 91.57(11) . 2_545 ?
O20 Co O2 89.95(12) . 2_545 ?
O20 Co O2 90.05(12) 3 2_545 ?
O1 Co O2 91.57(11) 3 4_565 ?
O1 Co O2 88.43(11) . 4_565 ?
O20 Co O2 90.05(12) . 4_565 ?
O20 Co O2 89.95(12) 3 4_565 ?
O2 Co O2 180.0 2_545 4_565 ?
C1 O1 Co 132.8(3) . . ?
O1 C1 C4 135.4(4) . . ?
O1 C1 C2 134.4(4) . . ?
C4 C1 C2 90.2(3) . . ?
C2 O2 Co 126.8(2) . 2 ?
O2 C2 C1 133.6(3) . . ?
O2 C2 C3 136.7(4) . . ?
C1 C2 C3 89.6(3) . . ?
O3 C3 C4 136.3(4) . . ?
O3 C3 C2 134.6(4) . . ?
C4 C3 C2 89.0(3) . . ?
N5 C4 C1 129.7(3) . . ?
N5 C4 C3 139.1(3) . . ?
C1 C4 C3 91.1(3) . . ?
C4 N5 C11 128.2(3) . . ?
C7 C6 C11 120.0 . . ?
C6 C7 C8 120.0 . . ?
C9 C8 C7 120.0 . . ?
C10 C9 C8 120.0 . . ?
C9 C10 C11 120.0 . . ?
C10 C11 C6 120.0 . . ?
C10 C11 N5 122.8(2) . . ?
C6 C11 N5 117.2(2) . . ?
C21 O20 Co 117.6(3) . . ?
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
Co O1 2.056(3) 3 ?
Co O1 2.056(3) . ?
Co O20 2.092(3) . ?
Co O20 2.092(3) 3 ?
Co O2 2.105(3) 2_545 ?
Co O2 2.105(3) 4_565 ?
O1 C1 1.258(4) . ?
C1 C4 1.445(5) . ?
C1 C2 1.456(6) . ?
O2 C2 1.257(5) . ?
O2 Co 2.105(3) 2 ?
C2 C3 1.479(5) . ?
O3 C3 1.248(4) . ?
C3 C4 1.452(5) . ?
C4 N5 1.330(5) . ?
N5 C11 1.423(4) . ?
C6 C7 1.39 . ?
C6 C11 1.39 . ?
C7 C8 1.39 . ?
C8 C9 1.39 . ?
C9 C10 1.39 . ?
C10 C11 1.39 . ?
O20 C21 1.360(8) . ?
