#------------------------------------------------------------------------------
#$Date: 2019-11-23 13:29:27 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233449 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/88/4348871.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_4348871
loop_
_publ_author_name
'Mastropietro, Teresa F.'
'Marino, Nadia'
'Munno, Giovanni De'
'Lloret, Francesc'
'Julve, Miguel'
'Pardo, Emilio'
'Armentano, Donatella'
_publ_section_title
;
 Selective Guest Inclusion in Oxalate-Based Iron(III) Magnetic
 Coordination Polymers.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11160
_journal_page_last               11169
_journal_paper_doi               10.1021/acs.inorgchem.6b01769
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C3 H8 Cl3 Fe K N O5'
_chemical_formula_weight         339.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 112.421(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.725(2)
_cell_length_b                   7.5076(19)
_cell_length_c                   9.026(3)
_cell_measurement_reflns_used    7509
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.44
_cell_volume                     546.5(3)
_computing_cell_refinement       'Bruker APEX'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10066
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.974
_diffrn_reflns_theta_min         2.441
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.487
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.063
_exptl_crystal_description       prism
_exptl_crystal_F_000             338
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       0.020(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1879
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0391
_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)+(0.0593P)²+0.1726P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1738
_reflns_number_total             1879
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01769_si_003.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4348871
_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.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
Fe1 Fe 0.82462(4) 0.7500 0.28027(3) 0.01744(13) Uani 1 2 d S T P
K1 K 0.56905(7) 0.7500 0.57766(8) 0.03143(17) Uani 1 2 d S T P
Cl1 Cl 0.75063(9) 0.7500 0.00497(7) 0.03735(19) Uani 1 2 d S T P
Cl2 Cl 0.65126(5) 0.98811(6) 0.27623(6) 0.03095(15) Uani 1 1 d . . .
O1W O 0.8934(2) 0.7500 0.5321(2) 0.0243(4) Uani 1 2 d DS T P
O1 O 1.01769(14) 0.92389(15) 0.31926(14) 0.0212(2) Uani 1 1 d . . .
O2 O 1.27975(16) 0.93239(19) 0.33329(18) 0.0319(3) Uani 1 1 d . . .
C1 C 1.15459(19) 0.8530(2) 0.32658(18) 0.0190(3) Uani 1 1 d . . .
C2 C 0.1567(4) 0.7500 0.9524(4) 0.0414(7) Uani 1 2 d S T P
H4 H 0.1254 0.8493 0.8799 0.050 Uiso 0.25 1 calc R U P
H5 H 0.1033 0.7596 1.0274 0.050 Uiso 0.5 2 calc R U P
H6 H 0.1234 0.6411 0.8929 0.050 Uiso 0.25 1 calc R U P
N1 N 0.3355(4) 0.7500 1.0385(3) 0.0569(9) Uani 1 2 d S T P
H1 H 0.3668 0.8525 1.0909 0.068 Uiso 0.25 1 calc R U P
H2 H 0.3850 0.7372 0.9693 0.068 Uiso 0.5 2 calc R U P
H3 H 0.3642 0.6602 1.1082 0.068 Uiso 0.25 1 calc R U P
H1W H 0.951(3) 0.848(4) 0.581(4) 0.060 Uiso 1 1 d D U .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
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 Fe1 O1 78.99(7) 4_575 .
O1 Fe1 O1W 86.43(5) 4_575 .
O1 Fe1 O1W 86.43(5) . .
O1 Fe1 Cl1 93.36(4) 4_575 .
O1 Fe1 Cl1 93.36(4) . .
O1W Fe1 Cl1 179.73(6) . .
O1 Fe1 Cl2 167.10(4) 4_575 .
O1 Fe1 Cl2 90.01(4) . .
O1W Fe1 Cl2 86.19(4) . .
Cl1 Fe1 Cl2 93.984(19) . .
O1 Fe1 Cl2 90.01(4) 4_575 4_575
O1 Fe1 Cl2 167.10(4) . 4_575
O1W Fe1 Cl2 86.19(4) . 4_575
Cl1 Fe1 Cl2 93.984(19) . 4_575
Cl2 Fe1 Cl2 100.04(3) . 4_575
O2 K1 O2 124.45(7) 3_776 2_746
O2 K1 O2 143.91(5) 3_776 4_475
O2 K1 O2 89.67(4) 2_746 4_475
O2 K1 O2 89.67(4) 3_776 1_455
O2 K1 O2 143.91(5) 2_746 1_455
O2 K1 O2 54.76(6) 4_475 1_455
O2 K1 O1W 70.25(3) 3_776 .
O2 K1 O1W 70.25(3) 2_746 .
O2 K1 O1W 118.30(5) 4_475 .
O2 K1 O1W 118.30(5) 1_455 .
O2 K1 Cl2 133.68(4) 3_776 2_646
O2 K1 Cl2 69.67(4) 2_746 2_646
O2 K1 Cl2 64.55(3) 4_475 2_646
O2 K1 Cl2 96.31(4) 1_455 2_646
O1W K1 Cl2 139.79(2) . 2_646
O2 K1 Cl2 69.67(4) 3_776 3_676
O2 K1 Cl2 133.68(4) 2_746 3_676
O2 K1 Cl2 96.31(4) 4_475 3_676
O2 K1 Cl2 64.55(3) 1_455 3_676
O1W K1 Cl2 139.79(2) . 3_676
Cl2 K1 Cl2 71.84(3) 2_646 3_676
O2 K1 Cl2 117.08(4) 3_776 4_575
O2 K1 Cl2 64.15(4) 2_746 4_575
O2 K1 Cl2 64.06(3) 4_475 4_575
O2 K1 Cl2 91.48(4) 1_455 4_575
O1W K1 Cl2 54.55(3) . 4_575
Cl2 K1 Cl2 108.662(19) 2_646 4_575
Cl2 K1 Cl2 155.62(2) 3_676 4_575
O2 K1 Cl2 64.15(4) 3_776 .
O2 K1 Cl2 117.08(4) 2_746 .
O2 K1 Cl2 91.48(4) 4_475 .
O2 K1 Cl2 64.06(3) 1_455 .
O1W K1 Cl2 54.55(3) . .
Cl2 K1 Cl2 155.62(2) 2_646 .
Cl2 K1 Cl2 108.662(19) 3_676 .
Cl2 K1 Cl2 60.48(3) 4_575 .
O2 K1 Cl1 73.29(4) 3_776 1_556
O2 K1 Cl1 73.29(4) 2_746 1_556
O2 K1 Cl1 134.62(3) 4_475 1_556
O2 K1 Cl1 134.62(3) 1_455 1_556
O1W K1 Cl1 95.44(4) . 1_556
Cl2 K1 Cl1 70.09(2) 2_646 1_556
Cl2 K1 Cl1 70.09(2) 3_676 1_556
Cl2 K1 Cl1 133.82(2) 4_575 1_556
Cl2 K1 Cl1 133.82(2) . 1_556
O2 K1 K1 167.40(4) 3_776 3_666
O2 K1 K1 47.67(4) 2_746 3_666
O2 K1 K1 42.00(3) 4_475 3_666
O2 K1 K1 96.56(4) 1_455 3_666
O1W K1 K1 97.15(2) . 3_666
Cl2 K1 K1 56.621(18) 2_646 3_666
Cl2 K1 K1 122.92(3) 3_676 3_666
Cl2 K1 K1 52.041(17) 4_575 3_666
Cl2 K1 K1 108.89(3) . 3_666
Cl1 K1 K1 109.08(2) 1_556 3_666
O2 K1 K1 47.67(4) 3_776 3_676
O2 K1 K1 167.40(4) 2_746 3_676
O2 K1 K1 96.56(4) 4_475 3_676
O2 K1 K1 42.00(3) 1_455 3_676
O1W K1 K1 97.15(2) . 3_676
Cl2 K1 K1 122.92(3) 2_646 3_676
Cl2 K1 K1 56.621(18) 3_676 3_676
Cl2 K1 K1 108.89(3) 4_575 3_676
Cl2 K1 K1 52.042(17) . 3_676
Cl1 K1 K1 109.08(2) 1_556 3_676
K1 K1 K1 137.52(3) 3_666 3_676
Fe1 Cl1 K1 170.69(3) . 1_554
Fe1 Cl2 K1 155.37(2) . 3_676
Fe1 Cl2 K1 85.49(2) . .
K1 Cl2 K1 71.337(19) 3_676 .
Fe1 O1W K1 104.49(7) . .
C1 O1 Fe1 115.52(10) . .
C1 O2 K1 140.44(12) . 3_776
C1 O2 K1 107.50(11) . 1_655
K1 O2 K1 90.33(4) 3_776 1_655
O2 C1 O1 126.43(15) . .
O2 C1 C1 119.12(10) . 4_575
O1 C1 C1 114.45(9) . 4_575
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 2.0527(12) 4_575
Fe1 O1 2.0527(12) .
Fe1 O1W 2.1176(18) .
Fe1 Cl1 2.3168(10) .
Fe1 Cl2 2.3330(6) .
Fe1 Cl2 2.3330(6) 4_575
K1 O2 2.6950(15) 3_776
K1 O2 2.6950(15) 2_746
K1 O2 2.9772(17) 4_475
K1 O2 2.9772(17) 1_455
K1 O1W 3.011(2) .
K1 Cl2 3.3516(9) 2_646
K1 Cl2 3.3516(9) 3_676
K1 Cl2 3.5497(10) 4_575
K1 Cl2 3.5497(10) .
K1 Cl1 3.5671(14) 1_556
K1 K1 4.0273(10) 3_666
K1 K1 4.0273(10) 3_676
Cl1 K1 3.5671(14) 1_554
Cl2 K1 3.3516(9) 3_676
O1 C1 1.2862(19) .
O2 C1 1.225(2) .
O2 K1 2.6950(15) 3_776
O2 K1 2.9772(17) 1_655
C1 C1 1.546(3) 4_575
C2 N1 1.453(4) .
