#------------------------------------------------------------------------------
#$Date: 2019-06-26 10:33:32 +0300 (Wed, 26 Jun 2019) $
#$Revision: 216568 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/19/1551904.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_1551904
loop_
_publ_author_name
'J. Lopez-Cabrelles'
'S. Manas-Valero'
'I. J. Vitorica-Yrezabal'
'P. J. Bereciartua'
'J. A. Rodriguez-Velamazan'
'J. C. Waerenborgh'
'B. J. C. Vieira'
'D. Davidovikj'
'P. G. Steeneken'
'H. S. J. van der Zant'
'G. Minguez Espallargas'
'E. Coronado'
_publ_section_title
;
 Isoreticular two-dimensional magnetic coordination polymers prepared
 through pre-synthetic ligand functionalization
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              1001
_journal_page_last               1007
_journal_paper_doi               10.1038/s41557-018-0113-9
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         '0.5(C28 H20 Fe2 N8)'
_chemical_formula_sum            'C14 H10 Fe N4'
_chemical_formula_weight         290.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 96.965(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3356(14)
_cell_length_b                   8.3352(11)
_cell_length_c                   18.758(3)
_cell_measurement_reflns_used    2694
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.5070
_cell_measurement_theta_min      2.1060
_cell_volume                     1293.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω   -145.00  24.00   1.00    0.20    --   30.00   0.00   0.00  169
  2  ω   -145.00  24.00   1.00    0.20    --   30.00   0.00 120.00  169
  3  ω   -145.00  24.00   1.00    0.20    --   30.00   0.00 240.00  169
  4  φ      0.00 179.00   1.00    0.20   0.00   0.00   0.00    --   179
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0137184000
_diffrn_orient_matrix_UB_12      -0.0813136000
_diffrn_orient_matrix_UB_13      -0.0018748000
_diffrn_orient_matrix_UB_21      0.0052567000
_diffrn_orient_matrix_UB_22      -0.0051066000
_diffrn_orient_matrix_UB_23      0.0368481000
_diffrn_orient_matrix_UB_31      -0.0819956000
_diffrn_orient_matrix_UB_32      -0.0139213000
_diffrn_orient_matrix_UB_33      -0.0025573000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            1167
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         24.532
_diffrn_reflns_theta_min         2.120
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.067
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.531
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1167
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0813
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1459P)²+8.7648P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2198
_refine_ls_wR_factor_ref         0.2275
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1052
_reflns_number_total             1167
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            41557_2018_113_MOESM3_ESM.cif
_cod_data_source_block           m_fe2o_h_collection1_
_cod_database_code               1551904
_chemical_oxdiff_formula         FeC20N2H20
_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.
;
_reflns_odcompleteness_completeness 98.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.51
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.896(9)
 0.104(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid body (RIGU) restrains
 C2, N3, N1, C5, C4, C9, C8, C7, C6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C0AA, C4A, C9A, C8A, C7A, C6A, C5A, N1, N3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C5)=Sof(C9)=Sof(H9)=Sof(C4)=Sof(C6)=Sof(H6)=Sof(C2)=Sof(H2)=Sof(C8)=
 Sof(H8)=Sof(C7)=Sof(H7)=1-FVAR(1)
 Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C6A)=Sof(H6A)=Sof(C9A)=Sof(H9A)=
 Sof(C5A)=Sof(C4A)=Sof(C0AA)=Sof(H0AA)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C7A(H7A), C8A(H8A), C6A(H6A), C9A(H9A), C9(H9), C6(H6), C0AA(H0AA), C2(H2),
 C8(H8), C7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.498
_oxdiff_exptl_absorpt_empirical_full_min 0.705
loop_
_space_group_symop_operation_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'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.18420(12) 0.7500 0.0230(5) Uani 1 2 d S T P A .
N3 N 0.8352(6) 0.5303(5) 0.6967(3) 0.0234(10) Uani 1 1 d . U . . .
N1 N 0.6396(6) 0.3365(6) 0.6989(3) 0.0238(10) Uani 1 1 d . U . . .
C7A C 0.8647(18) 0.1505(18) 0.5567(8) 0.029(3) Uani 0.496(7) 1 d . U . A 1
H7A H 0.8680 0.0626 0.5264 0.035 Uiso 0.496(7) 1 calc R . . A 1
C8A C 0.9818(18) 0.2740(18) 0.5550(7) 0.029(3) Uani 0.496(7) 1 d . U . A 1
H8A H 1.0617 0.2633 0.5248 0.035 Uiso 0.496(7) 1 calc R . . A 1
C6A C 0.7468(14) 0.1576(13) 0.6019(6) 0.023(2) Uani 0.496(7) 1 d . U . A 1
H6A H 0.6718 0.0754 0.6031 0.028 Uiso 0.496(7) 1 calc R . . A 1
C9A C 0.9795(14) 0.4106(14) 0.5977(6) 0.024(2) Uani 0.496(7) 1 d . U . A 1
H9A H 1.0534 0.4935 0.5954 0.029 Uiso 0.496(7) 1 calc R . . A 1
C5 C 0.5859(13) 0.4578(13) 0.6461(6) 0.022(2) Uani 0.504(7) 1 d . U . A 2
C9 C 0.6875(15) 0.7037(13) 0.5978(6) 0.025(2) Uani 0.504(7) 1 d . U . A 2
H9 H 0.7701 0.7781 0.5959 0.030 Uiso 0.504(7) 1 calc R . . A 2
C5A C 0.7436(14) 0.2952(13) 0.6466(6) 0.023(2) Uani 0.496(7) 1 d . U . A 1
C4 C 0.7043(13) 0.5716(13) 0.6439(6) 0.024(2) Uani 0.504(7) 1 d . U . A 2
C6 C 0.4351(14) 0.4708(14) 0.6006(6) 0.027(2) Uani 0.504(7) 1 d . U . A 2
H6 H 0.3551 0.3933 0.6013 0.033 Uiso 0.504(7) 1 calc R . . A 2
C4A C 0.8594(13) 0.4168(13) 0.6444(6) 0.0211(19) Uani 0.496(7) 1 d . U . A 1
C0AA C 0.7092(17) 0.4743(16) 0.7285(8) 0.033(3) Uani 0.496(7) 1 d . U . A 1
H0AA H 0.6725 0.5253 0.7675 0.040 Uiso 0.496(7) 1 calc R . . A 1
C2 C 0.7838(16) 0.4000(16) 0.7298(8) 0.033(3) Uani 0.504(7) 1 d . U . A 2
H2 H 0.8417 0.3561 0.7707 0.040 Uiso 0.504(7) 1 calc R . . A 2
C8 C 0.5385(17) 0.7176(18) 0.5545(7) 0.029(3) Uani 0.504(7) 1 d . U . A 2
H8 H 0.5210 0.8052 0.5239 0.034 Uiso 0.504(7) 1 calc R . . A 2
C7 C 0.4134(18) 0.6018(18) 0.5561(8) 0.028(3) Uani 0.504(7) 1 d . U . A 2
H7 H 0.3161 0.6150 0.5268 0.034 Uiso 0.504(7) 1 calc R . . A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0010 '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'
Fe Fe 0.3520 0.8020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 '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
N3 Fe1 N3 102.5(3) 3_445 4_646
N1 Fe1 N3 103.42(19) . 4_646
N1 Fe1 N3 123.2(2) . 3_445
N1 Fe1 N3 103.42(19) 2_656 3_445
N1 Fe1 N3 123.2(2) 2_656 4_646
N1 Fe1 N1 103.0(3) . 2_656
C4 N3 Fe1 126.9(5) . 3
C4A N3 Fe1 128.5(6) . 3
C0AA N3 Fe1 120.7(6) . 3
C0AA N3 C4A 105.2(8) . .
C2 N3 Fe1 120.8(6) . 3
C2 N3 C4 104.8(8) . .
C5 N1 Fe1 127.6(5) . .
C5A N1 Fe1 127.0(5) . .
C0AA N1 Fe1 124.6(6) . .
C0AA N1 C5A 102.6(8) . .
C2 N1 Fe1 124.1(6) . .
C2 N1 C5 101.6(7) . .
C8A C7A H7A 119.1 . .
C6A C7A H7A 119.1 . .
C6A C7A C8A 121.8(13) . .
C7A C8A H8A 119.3 . .
C9A C8A C7A 121.5(13) . .
C9A C8A H8A 119.3 . .
C7A C6A H6A 121.2 . .
C7A C6A C5A 117.7(12) . .
C5A C6A H6A 121.2 . .
C8A C9A H9A 121.7 . .
C8A C9A C4A 116.6(11) . .
C4A C9A H9A 121.7 . .
C4 C5 N1 109.8(9) . .
C4 C5 C6 120.7(10) . .
C6 C5 N1 129.5(9) . .
C4 C9 H9 122.0 . .
C4 C9 C8 116.0(11) . .
C8 C9 H9 122.0 . .
C6A C5A N1 131.0(10) . .
C4A C5A N1 108.8(9) . .
C4A C5A C6A 120.2(11) . .
C5 C4 N3 107.8(9) . .
C5 C4 C9 123.0(11) . .
C9 C4 N3 129.2(10) . .
C5 C6 H6 121.2 . .
C7 C6 C5 117.6(11) . .
C7 C6 H6 121.2 . .
N3 C4A C9A 129.5(10) . .
N3 C4A C5A 108.1(9) . .
C5A C4A C9A 122.3(10) . .
N3 C0AA N1 115.0(10) . .
N3 C0AA H0AA 122.5 . .
N1 C0AA H0AA 122.5 . .
N3 C2 N1 115.2(9) . .
N3 C2 H2 122.4 . .
N1 C2 H2 122.4 . .
C9 C8 H8 119.0 . .
C9 C8 C7 122.1(13) . .
C7 C8 H8 119.0 . .
C6 C7 C8 120.6(13) . .
C6 C7 H7 119.7 . .
C8 C7 H7 119.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N3 2.049(5) 4_646
Fe1 N3 2.049(5) 3_445
Fe1 N1 2.038(5) 2_656
Fe1 N1 2.038(5) .
N3 Fe1 2.049(5) 3
N3 C4 1.424(12) .
N3 C4A 1.395(12) .
N3 C0AA 1.353(14) .
N3 C2 1.348(13) .
N1 C5 1.448(12) .
N1 C5A 1.428(13) .
N1 C0AA 1.374(13) .
N1 C2 1.376(13) .
C7A H7A 0.9300 .
C7A C8A 1.421(19) .
C7A C6A 1.37(2) .
C8A H8A 0.9300 .
C8A C9A 1.394(19) .
C6A H6A 0.9300 .
C6A C5A 1.423(16) .
C9A H9A 0.9300 .
C9A C4A 1.409(16) .
C5 C4 1.373(16) .
C5 C6 1.435(16) .
C9 H9 0.9300 .
C9 C4 1.397(16) .
C9 C8 1.403(19) .
C5A C4A 1.404(16) .
C6 H6 0.9300 .
C6 C7 1.373(19) .
C0AA H0AA 0.9300 .
C2 H2 0.9300 .
C8 H8 0.9300 .
C8 C7 1.424(19) .
C7 H7 0.9300 .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.896(9)
2 0.104(9)
