#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:41:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179123 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/85/4308502.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_4308502
loop_
_publ_author_name
'Xin-Yi Wang'
'Hai-Yan Wei'
'Zhe-Ming Wang'
'Zhi-Da Chen'
'Song Gao'
_publ_section_title
;
Formate The Analogue of Azide: Structural and Magnetic Properties of
M(HCOO)2(4,4'-bpy).nH2O (M = Mn, Co, Ni; n= 0, 5)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              572
_journal_page_last               583
_journal_paper_doi               10.1021/ic049170t
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C12 H20 Co N2 O9'
_chemical_formula_weight         395.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.223(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5108(3)
_cell_length_b                   20.2765(7)
_cell_length_c                   8.1309(2)
_cell_measurement_reflns_used    14247
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.61
_cell_volume                     1693.59(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski and Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) and maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14247
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    1.061
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            'pale red'
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.238(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3774
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0436P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                3048
_reflns_number_total             3774
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049170tsi20040625_101613_3.cif
_cod_data_source_block           CO-CHOO-bpy-3-Co
_cod_depositor_comments
;
The following automatic conversions were performed:
'_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 
;
_cod_database_code               4308502
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.94204(8) 0.25379(2) 0.51007(9) 0.02162(10) Uani 1 1 d . . .
O1 O 0.7852(2) 0.20249(11) 0.3612(3) 0.0297(6) Uani 1 1 d . . .
O2 O 0.6063(2) 0.19831(12) 0.1595(3) 0.0319(6) Uani 1 1 d . . .
O3 O 1.0129(2) 0.28389(12) 0.3003(3) 0.0320(6) Uani 1 1 d . . .
O4 O 1.0000(3) 0.28831(14) 0.0250(3) 0.0531(7) Uani 1 1 d . . .
O5 O 0.8806(3) 0.23149(13) 0.7332(3) 0.0376(6) Uani 1 1 d . . .
O6 O 0.7329(3) 0.13534(12) 0.8328(3) 0.0466(6) Uani 1 1 d . . .
O7 O 0.8407(4) 0.09170(15) 0.1523(4) 0.0573(8) Uani 1 1 d . . .
O8 O 0.6762(4) -0.01586(17) 0.1568(5) 0.0931(12) Uani 1 1 d . . .
O9 O 1.0471(4) 0.4235(2) 0.8681(6) 0.1042(16) Uani 1 1 d . . .
N1 N 0.8445(3) 0.34789(13) 0.5035(3) 0.0261(7) Uani 1 1 d . . .
N2 N 0.5399(3) 0.66019(13) 0.5192(4) 0.0273(7) Uani 1 1 d . . .
C1 C 0.8929(4) 0.40251(17) 0.4519(5) 0.0385(10) Uani 1 1 d . . .
H1 H 0.9694 0.3995 0.4122 0.046 Uiso 1 1 calc R . .
C2 C 0.7326(4) 0.35492(17) 0.5581(5) 0.0327(9) Uani 1 1 d . . .
H2 H 0.6956 0.3175 0.5945 0.039 Uiso 1 1 calc R . .
C3 C 0.8356(5) 0.46393(18) 0.4540(6) 0.0402(10) Uani 1 1 d . . .
H3 H 0.8740 0.5007 0.4165 0.048 Uiso 1 1 calc R . .
C4 C 0.6710(4) 0.41338(17) 0.5629(5) 0.0340(9) Uani 1 1 d . . .
H4 H 0.5938 0.4150 0.6014 0.041 Uiso 1 1 calc R . .
C5 C 0.7222(4) 0.47075(17) 0.5110(5) 0.0274(9) Uani 1 1 d . . .
C6 C 0.6592(4) 0.53610(16) 0.5168(4) 0.0279(9) Uani 1 1 d . . .
C7 C 0.7216(4) 0.59439(18) 0.4844(5) 0.0352(9) Uani 1 1 d . . .
H7 H 0.8047 0.5928 0.4619 0.042 Uiso 1 1 calc R . .
C8 C 0.5373(4) 0.54267(18) 0.5533(5) 0.0352(9) Uani 1 1 d . . .
H8A H 0.4923 0.5056 0.5770 0.042 Uiso 1 1 calc R . .
C9 C 0.6589(4) 0.65387(16) 0.4863(5) 0.0315(9) Uani 1 1 d . . .
H9 H 0.7015 0.6919 0.4633 0.038 Uiso 1 1 calc R . .
C10 C 0.4825(4) 0.60479(18) 0.5543(5) 0.0358(9) Uani 1 1 d . . .
H10 H 0.4009 0.6080 0.5810 0.043 Uiso 1 1 calc R . .
C11 C 0.6840(4) 0.22743(14) 0.2747(5) 0.0266(7) Uani 1 1 d . . .
H11 H 0.6651 0.2708 0.2976 0.032 Uiso 1 1 calc R . .
C12 C 0.9746(3) 0.26346(16) 0.1522(4) 0.0346(8) Uani 1 1 d . . .
H12 H 0.9221 0.2261 0.1375 0.041 Uiso 1 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
O3 Co1 O5 174.39(11) . . ?
O3 Co1 O1 92.65(10) . . ?
O5 Co1 O1 92.51(11) . . ?
O3 Co1 O2 86.92(10) . 4 ?
O5 Co1 O2 88.03(10) . 4 ?
O1 Co1 O2 177.25(12) . 4 ?
O3 Co1 N2 92.02(11) . 3_545 ?
O5 Co1 N2 90.71(12) . 3_545 ?
O1 Co1 N2 83.93(11) . 3_545 ?
O2 Co1 N2 93.37(11) 4 3_545 ?
O3 Co1 N1 88.36(11) . . ?
O5 Co1 N1 88.87(11) . . ?
O1 Co1 N1 96.46(11) . . ?
O2 Co1 N1 86.25(11) 4 . ?
N2 Co1 N1 179.44(14) 3_545 . ?
C11 O1 Co1 126.4(2) . . ?
C11 O2 Co1 122.3(2) . 4_454 ?
C12 O3 Co1 126.0(2) . . ?
C1 N1 C2 115.8(3) . . ?
C1 N1 Co1 122.3(3) . . ?
C2 N1 Co1 121.8(2) . . ?
C10 N2 C9 116.5(3) . . ?
C10 N2 Co1 121.0(3) . 3_455 ?
C9 N2 Co1 122.5(2) . 3_455 ?
N1 C1 C3 123.5(4) . . ?
N1 C2 C4 123.9(3) . . ?
C5 C3 C1 120.3(4) . . ?
C2 C4 C5 120.5(4) . . ?
C3 C5 C4 116.0(3) . . ?
C3 C5 C6 121.6(3) . . ?
C4 C5 C6 122.4(3) . . ?
C8 C6 C7 116.8(3) . . ?
C8 C6 C5 122.2(3) . . ?
C7 C6 C5 121.1(3) . . ?
C9 C7 C6 119.5(4) . . ?
C10 C8 C6 119.6(4) . . ?
N2 C9 C7 123.7(4) . . ?
N2 C10 C8 123.8(4) . . ?
O2 C11 O1 124.9(3) . . ?
O4 C12 O3 126.0(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
Co1 O3 2.092(3) . ?
Co1 O5 2.099(3) . ?
Co1 O1 2.102(3) . ?
Co1 O2 2.124(3) 4 ?
Co1 N2 2.153(3) 3_545 ?
Co1 N1 2.162(3) . ?
O1 C11 1.251(5) . ?
O2 C11 1.253(4) . ?
O2 Co1 2.124(3) 4_454 ?
O3 C12 1.256(4) . ?
O4 C12 1.230(4) . ?
N1 C1 1.324(5) . ?
N1 C2 1.349(5) . ?
N2 C10 1.334(5) . ?
N2 C9 1.339(5) . ?
N2 Co1 2.153(3) 3_455 ?
C1 C3 1.385(5) . ?
C2 C4 1.355(5) . ?
C3 C5 1.375(6) . ?
C4 C5 1.384(5) . ?
C5 C6 1.487(4) . ?
C6 C8 1.381(6) . ?
C6 C7 1.403(5) . ?
C7 C9 1.376(5) . ?
C8 C10 1.386(5) . ?
