#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:19:29 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179322 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/19/4321959.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_4321959
loop_
_publ_author_name
'Giovanni De Munno'
'Donatella Armentano'
'Miguel Julve'
'Francesc Lloret'
'Rodrigue Lescouëzec'
'Juan Faus'
_publ_contact_author
;
     Prof. G. De Munno
     Dipartimento di Chimica
     Universitá della Calabria
     I-87030 Arcavacata di Rende, Cosenza
     Italy
;
_publ_contact_author_email       demunno@unical.it
_publ_contact_author_fax         '39 984 492044'
_publ_contact_author_phone       '39 984 492068'
_publ_section_title
;
 Two-Dimensional Assembling of
 (2,2'-Bipyrimidine)bis(oxalato)chromate(III) Units through Alkaline
 Cations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2234
_journal_page_last               2237
_journal_paper_doi               10.1021/ic981232q
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety         '[CrNa(bpym)(ox)2]5H2O'
_chemical_formula_sum            'C12 H6 Cr N4 Na O13'
_chemical_formula_weight         489.2
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_cell_angle_alpha                90.
_cell_angle_beta                 103.33(2)
_cell_angle_gamma                90.
_cell_formula_units_Z            2
_cell_length_a                   9.886(3)
_cell_length_b                   17.388(5)
_cell_length_c                   6.029(2)
_cell_measurement_radiation      'Mo K\a'
_cell_measurement_temperature    295
_cell_measurement_wavelength     0.710730
_cell_volume                     1008.5(5)
_computing_cell_refinement       'Siemens P3/V'
_computing_data_collection       'Siemens P3/V,(VMS vers 4.21/V, 1990)'
_computing_data_reduction
'Siemens SHELXTL-PLUS,(VMS vers 4.21/V , 1990)'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'Siemens SHELXTL-PLUS and PARST'
_computing_structure_refinement  'Siemens SHELXTL-PLUS'
_computing_structure_solution    'Siemens SHELXTL-PLUS'
_diffrn_ambient_temperature      295
_diffrn_measurement_device       'Siemens R3m/V diffractometer'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  'highly-oriented graphite crystal'
_diffrn_radiation_source         'fine-focus xray_tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.710730
_diffrn_reflns_av_R_equivalents  2.15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2630
_diffrn_reflns_theta_max         27.0
_diffrn_reflns_theta_min         1.5
_exptl_absorpt_coefficient_mu    6.6337
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            pink_violet
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.80
_refine_diff_density_min         -1.93
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   0.89
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2159
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          4.98
_refine_ls_R_factor_obs          4.80
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/(σ²(F)+ 0.0050*F²))'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         6.88
_refine_ls_wR_factor_obs         6.47
_reflns_number_observed          2159
_reflns_number_total             2225
_reflns_observed_criterion       >3\s(I)
_cod_data_source_file            ic981232q_2.cif
_cod_data_source_block           (2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/(\s^2^(F)+ 0.0050*F^2^))' 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^(F)+
0.0050*F^2^))'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1008.4(5)
_cod_original_sg_symbol_H-M      'C 1 2/m 1'
_cod_database_code               4321959
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y,-z
1/2+x,1/2+y,z
1/2-x,1/2+y,-z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
_atom_site_aniso_type_symbol
Cr1 0.0308(3) 0.0264(3) 0.0333(3) 0. 0.0121(2) 0. Cr
N1 0.033(1) 0.034(1) 0.031(1) 0.0002(9) 0.0104(9) 0.0027(9) N
C1 0.040(2) 0.054(2) 0.032(1) -0.002(1) 0.008(1) 0.005(1) C
C2 0.046(2) 0.077(3) 0.038(2) 0.010(2) 0.007(1) 0.009(2) C
C3 0.047(2) 0.059(2) 0.063(2) 0.025(2) 0.016(2) 0.015(2) C
N2 0.040(1) 0.039(1) 0.058(2) 0.013(1) 0.015(1) 0.005(1) N
C4 0.028(1) 0.033(1) 0.041(1) 0.001(1) 0.013(1) 0.002(1) C
Na1 0.0383(9) 0.0324(9) 0.097(2) 0. 0.027(1) 0. Na
O1 0.0393(9) 0.043(1) 0.0436(9) -0.015(1) 0.0203(7) -0.009(1) O
C5 0.037(1) 0.036(1) 0.046(1) -0.007(1) 0.017(1) -0.001(1) C
O4 0.046(1) 0.064(2) 0.070(2) -0.020(1) 0.034(1) -0.017(1) O
C6 0.039(1) 0.032(1) 0.048(2) -0.009(1) 0.017(1) -0.003(1) C
O3 0.055(2) 0.054(2) 0.077(2) -0.031(1) 0.029(1) -0.024(1) O
O2 0.042(1) 0.036(1) 0.049(1) -0.0114(9) 0.022(1) -0.0060(9) O
O5 0.155(6) 0.057(3) 0.127(5) 0. 0.101(5) 0. O
O6 0.093(4) 0.137(5) 0.186(7) -0.065(5) 0.061(4) -0.010(4) O
O7 0.127(6) 0.170(7) 0.162(6) 0.007(5) 0.072(5) 0.010(5) O
loop_
_atom_site_label
_atom_site_occupancy
_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_type_symbol
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_disorder_group
Cr1 1.00 0. 0. 0. 0.0310(2) Uani Cr ? ? ?
N1 1.00 0.0904(3) -0.0919(2) 0.1968(5) 0.0333(7) Uani N ? ? ?
C1 1.00 0.1751(4) -0.0881(2) 0.4072(5) 0.0428(9) Uani C ? ? ?
C2 1.00 0.2143(4) -0.1550(3) 0.5318(6) 0.055(1) Uani C ? ? ?
C3 1.00 0.1667(4) -0.2237(3) 0.4305(8) 0.058(1) Uani C ? ? ?
N2 1.00 0.0836(3) -0.2280(2) 0.2209(6) 0.0468(9) Uani N ? ? ?
C4 1.00 0.0490(3) -0.1620(2) 0.1156(5) 0.0344(7) Uani C ? ? ?
Na1 1.00 0. -0.3465(1) 0. 0.0575(8) Uani Na ? ? ?
O1 1.00 0.1420(2) 0.0028(2) -0.1777(3) 0.0428(6) Uani O ? ? ?
C5 1.00 0.2412(3) 0.0509(2) -0.1053(5) 0.0405(9) Uani C ? ? ?
O4 1.00 0.3380(3) 0.0626(2) -0.1924(5) 0.0606(9) Uani O ? ? ?
C6 1.00 0.2282(3) 0.0956(2) 0.1126(6) 0.0406(9) Uani C ? ? ?
O3 1.00 0.3139(3) 0.1430(2) 0.1949(6) 0.063(1) Uani O ? ? ?
O2 1.00 0.1202(3) 0.0768(1) 0.1870(5) 0.0432(7) Uani O ? ? ?
O5 1.00 0.5 -0.3294(3) -0.5 0.115(3) Uani O ? ? ?
O6 1.00 0.5467(6) -0.0523(5) -0.269(2) 0.142(3) Uani O ? ? ?
O7 1.00 0.5844(8) -0.2088(6) -0.144(1) 0.156(4) Uani O ? ? ?
H1 1.00 0.2083(4) -0.0392(2) 0.4708(5) 0.06 Uiso H ? C1 ?
H2 1.00 0.2723(4) -0.1534(3) 0.6833(6) 0.06 Uiso H ? C2 ?
H3 1.00 0.1947(4) -0.2705(3) 0.5126(8) 0.06 Uiso H ? C3 ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C Carbon 0 24 0.0020 0.0020 Internat_Tables_Vol_IV_Table_2.3.1
H Hydrogen 0 12 0.0000 0.0000 Internat_Tables_Vol_IV_Table_2.3.1
N Nitrogen 0 8 0.0040 0.0030 Internat_Tables_Vol_IV_Table_2.3.1
O Oxygen 0 26 0.0080 0.0060 Internat_Tables_Vol_IV_Table_2.3.1
Cr Chromium 0 2 0.2840 0.6240 Internat_Tables_Vol_IV_Table_2.3.1
Na Sodium 0 2 0.0300 0.0250 Internat_Tables_Vol_IV_Table_2.3.1
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
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
O1 Cr1 O2 83.2(1) . . . .
N1 Cr1 O2 94.1(1) . . . .
N1 Cr1 O1 93.7(1) . . . .
N1 Cr1 N1 78.7(1) . . 2_555 .
O1 Cr1 N1 88.6(1) . . 2_555 .
O1 Cr1 O1 177.1(2) . . 2_555 .
O2 Cr1 O1 94.8(1) . . 2_555 .
O2 Cr1 O2 94.2(1) . . 2_555 .
O2 Cr1 N1 168.7(1) . . 2_555 .
N2 Na1 N2 68.2(2) . . 2_555 .
N2 Na1 O4 157.4(1) . . 3_445 .
N2 Na1 O4 100.8(1) . . 4_545 .
O4 Na1 O4 95.7(2) 3_445 . 4_545 .
N2 Na1 O3 89.9(1) . . 3_445 .
N2 Na1 O3 97.3(1) . . 4_545 .
O4 Na1 O3 102.6(1) 3_445 . 4_545 .
O4 Na1 O3 71.4(1) 4_545 . 4_545 .
O3 Na1 O3 171.3(2) 3_445 . 4_545 .
Cr1 N1 C4 116.0(2) . . . .
Cr1 N1 C1 126.4(2) . . . .
C1 N1 C4 117.3(3) . . . .
N1 C1 C2 120.1(3) . . . .
C1 C2 C3 117.6(4) . . . .
C2 C3 N2 122.7(4) . . . .
C3 N2 Na1 127.3(3) . . . .
C3 N2 C4 116.1(3) . . . .
C4 N2 Na1 116.5(2) . . . .
N1 C4 N2 126.3(3) . . . .
N1 C4 C4 114.6(2) . . 2_555 .
N2 C4 C4 119.1(2) . . 2_555 .
Cr1 O1 C5 114.8(2) . . . .
O1 C5 C6 113.9(3) . . . .
O1 C5 O4 125.4(3) . . . .
O4 C5 C6 120.7(3) . . . .
C5 C6 O2 113.7(3) . . . .
C5 C6 O3 120.2(3) . . . .
C5 O4 Na1 114.5(2) . . 3_555 .
O3 C6 O2 126.1(3) . . . .
C6 O3 Na1 113.3(3) . . 3_555 .
Cr1 O2 C6 114.3(2) . . . .
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
Cr1 N1 2.067(3) . . .
Cr1 O1 1.953(2) . . .
Cr1 O2 1.962(2) . . .
Na1 N2 2.489(4) . . .
Na1 O3 2.407(4) . 4_545 .
Na1 O4 2.356(3) . 4_545 .
N1 C1 1.351(4) . . .
N1 C4 1.341(4) . . .
C1 C2 1.391(6) . . .
C2 C3 1.374(6) . . .
C3 N2 1.341(5) . . .
N2 C4 1.318(4) . . .
C4 C4 1.503(5) . 2_555 .
O1 C5 1.286(4) . . .
C5 O4 1.210(5) . . .
C5 C6 1.557(5) . . .
C6 O3 1.204(4) . . .
C6 O2 1.292(5) . . .
