#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/36/7053669.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_7053669
loop_
_publ_author_name
'Déniz, Mariadel'
'Pasán, Jorge'
'Fabelo, Oscar'
'Cañadillas-Delgado, Laura'
'Lloret, Francesc'
'Julve, Miguel'
'Ruiz-Pérez, Catalina'
_publ_section_title
;
 Metal-organic coordination frameworks based on mixed methylmalonate and
 4,4′-bipiridine ligands: synthesis, crystal structure and magnetic
 properties
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2515
_journal_paper_doi               10.1039/c0nj00436g
_journal_volume                  34
_journal_year                    2010
_chemical_formula_sum            'C9 H8.9 Cl0.1 Fe N O4.9'
_chemical_formula_weight         268.87
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.750(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3274(3)
_cell_length_b                   19.6916(8)
_cell_length_c                   7.3642(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1062.07(8)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10204
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.448
_exptl_absorpt_correction_T_max  0.9181
_exptl_absorpt_correction_T_min  0.6705
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             547
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2435
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0351
_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)+(0.0313P)²+1.0107P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0830
_reflns_number_gt                2008
_reflns_number_total             2435
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00436g.txt
_cod_data_source_block           Compound2
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1062.07(7)
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C9 H8.90 Cl0.10 Fe N O4.90'
_cod_database_code               7053669
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Fe1 Fe 0.46238(4) 0.212483(17) 0.44000(4) 0.01981(11) Uani 1 1 d D . .
N1 N 0.6678(3) 0.13082(11) 0.4630(3) 0.0271(5) Uani 1 1 d . . .
Cl1 Cl 0.2525(2) 0.29105(9) 0.4363(3) 0.0421(4) Uani 0.10 1 d PD . .
O1H O 0.2525(2) 0.29105(9) 0.4363(3) 0.0421(4) Uani 0.90 1 d PD . .
O2 O 0.6227(2) 0.26753(9) 0.6296(2) 0.0293(4) Uani 1 1 d . . .
O4 O 0.6195(2) 0.26425(9) 0.2464(2) 0.0269(4) Uani 1 1 d . . .
O1 O 0.8346(2) 0.34091(9) 0.7219(2) 0.0283(4) Uani 1 1 d . . .
O3 O 0.8284(2) 0.33696(9) 0.1556(2) 0.0297(4) Uani 1 1 d . . .
C1 C 0.7180(3) 0.32009(12) 0.6077(3) 0.0221(5) Uani 1 1 d . A .
C2 C 0.6843(4) 0.36173(13) 0.4341(3) 0.0289(6) Uani 1 1 d . . .
H2 H 0.5540 0.3730 0.4310 0.035 Uiso 1 1 calc R A .
C3 C 0.7141(3) 0.31729(12) 0.2658(3) 0.0220(5) Uani 1 1 d . A .
C4 C 0.7830(6) 0.42801(16) 0.4327(5) 0.0570(9) Uani 1 1 d . A .
H4A H 0.7533 0.4517 0.3217 0.086 Uiso 1 1 calc R . .
H4B H 0.9122 0.4200 0.4414 0.086 Uiso 1 1 calc R . .
H4C H 0.7469 0.4550 0.5342 0.086 Uiso 1 1 calc R . .
C7 C 0.9313(3) 0.02746(13) 0.4933(3) 0.0261(5) Uani 1 1 d . . .
C5A C 0.8374(10) 0.1394(4) 0.4138(13) 0.0384(17) Uani 0.70(2) 1 d P A 1
H5A H 0.8698 0.1816 0.3679 0.046 Uiso 0.70(2) 1 calc PR A 1
C6A C 0.9708(9) 0.0897(4) 0.4260(13) 0.0370(16) Uani 0.70(2) 1 d P A 1
H6A H 1.0880 0.0990 0.3878 0.044 Uiso 0.70(2) 1 calc PR A 1
C8A C 0.7510(12) 0.0180(4) 0.5527(17) 0.055(3) Uani 0.70(2) 1 d P A 1
H8A H 0.7166 -0.0230 0.6044 0.067 Uiso 0.70(2) 1 calc PR A 1
C9A C 0.6284(12) 0.0700(4) 0.5328(17) 0.049(2) Uani 0.70(2) 1 d P A 1
H9A H 0.5099 0.0627 0.5703 0.059 Uiso 0.70(2) 1 calc PR A 1
C5B C 0.798(4) 0.1222(12) 0.339(4) 0.059(7) Uani 0.30(2) 1 d P A 2
H5B H 0.7991 0.1518 0.2409 0.070 Uiso 0.30(2) 1 calc PR A 2
C6B C 0.925(3) 0.0735(12) 0.350(4) 0.058(7) Uani 0.30(2) 1 d P A 2
H6B H 1.0110 0.0704 0.2595 0.070 Uiso 0.30(2) 1 calc PR A 2
C8B C 0.807(3) 0.0367(13) 0.611(3) 0.054(7) Uani 0.30(2) 1 d P A 2
H8B H 0.8057 0.0082 0.7117 0.065 Uiso 0.30(2) 1 calc PR A 2
C9B C 0.675(3) 0.0876(12) 0.594(2) 0.039(5) Uani 0.30(2) 1 d P A 2
H9B H 0.5879 0.0904 0.6824 0.047 Uiso 0.30(2) 1 calc PR A 2
H1 H 0.182(6) 0.277(2) 0.537(6) 0.069(13) Uiso 0.90 1 d P . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
Cl Cl 0.1484 0.1585 '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
O2 Fe1 O1 171.17(7) . 4_565
O2 Fe1 O4 83.94(7) . .
O1 Fe1 O4 88.00(7) 4_565 .
O2 Fe1 O3 90.09(7) . 4_566
O1 Fe1 O3 97.80(7) 4_565 4_566
O4 Fe1 O3 173.65(7) . 4_566
O2 Fe1 Cl1 91.27(7) . .
O1 Fe1 Cl1 92.73(7) 4_565 .
O4 Fe1 Cl1 92.74(7) . .
O3 Fe1 Cl1 89.57(7) 4_566 .
O2 Fe1 N1 87.63(8) . .
O1 Fe1 N1 88.92(7) 4_565 .
O4 Fe1 N1 91.07(7) . .
O3 Fe1 N1 86.48(7) 4_566 .
Cl1 Fe1 N1 175.90(8) . .
C9B N1 C5A 105.8(9) . .
C9B N1 C9A 28.9(8) . .
C5A N1 C9A 116.0(5) . .
C9B N1 C5B 114.1(11) . .
C5A N1 C5B 30.5(13) . .
C9A N1 C5B 108.2(9) . .
C9B N1 Fe1 123.6(8) . .
C5A N1 Fe1 122.2(4) . .
C9A N1 Fe1 121.8(4) . .
C5B N1 Fe1 122.3(7) . .
C1 O2 Fe1 129.78(15) . .
C3 O4 Fe1 129.11(15) . .
C1 O1 Fe1 128.75(16) . 4_666
C3 O3 Fe1 132.72(16) . 4_665
O1 C1 O2 123.6(2) . .
O1 C1 C2 118.4(2) . .
O2 C1 C2 118.0(2) . .
C4 C2 C1 114.1(2) . .
C4 C2 C3 114.3(2) . .
C1 C2 C3 110.2(2) . .
O3 C3 O4 124.3(2) . .
O3 C3 C2 117.6(2) . .
O4 C3 C2 118.1(2) . .
C8B C7 C6A 106.3(10) . .
C8B C7 C6B 114.4(10) . .
C6A C7 C6B 30.3(12) . .
C8B C7 C8A 29.2(12) . .
C6A C7 C8A 116.3(5) . .
C6B C7 C8A 108.2(9) . .
C8B C7 C7 123.5(8) . 3_756
C6A C7 C7 122.2(4) . 3_756
C6B C7 C7 122.2(7) . 3_756
C8A C7 C7 121.5(4) . 3_756
N1 C5A C6A 124.2(6) . .
C7 C6A C5A 120.3(6) . .
C9A C8A C7 118.9(6) . .
N1 C9A C8A 124.2(7) . .
C6B C5B N1 123.9(14) . .
C5B C6B C7 121.0(14) . .
C7 C8B C9B 122.8(13) . .
N1 C9B C8B 123.8(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O2 2.0986(17) .
Fe1 O1 2.1143(17) 4_565
Fe1 O4 2.1206(16) .
Fe1 O3 2.1280(17) 4_566
Fe1 Cl1 2.1811(18) .
Fe1 N1 2.206(2) .
N1 C9B 1.287(17) .
N1 C5A 1.316(8) .
N1 C9A 1.338(8) .
N1 C5B 1.349(18) .
O2 C1 1.261(3) .
O4 C3 1.259(3) .
O1 C1 1.249(3) .
O1 Fe1 2.1143(17) 4_666
O3 C3 1.245(3) .
O3 Fe1 2.1280(17) 4_665
C1 C2 1.533(3) .
C2 C4 1.492(4) .
C2 C3 1.538(3) .
C7 C8B 1.287(19) .
C7 C6A 1.357(7) .
C7 C6B 1.394(18) .
C7 C8A 1.417(9) .
C7 C7 1.479(5) 3_756
C5A C6A 1.384(11) .
C8A C9A 1.368(13) .
C5B C6B 1.34(2) .
C8B C9B 1.40(3) .
