Isoreticular two-dimensional magnetic coordination polymers prepared through pre-synthetic ligand functionalization
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; Nature Chemistry 10 (2018) 1001–1007; doi:10.1038/s41557-018-0113-9

data_1551904
_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  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -145.00  24.00   1.00    0.20    --   30.00   0.00   0.00  169
  2  \w   -145.00  24.00   1.00    0.20    --   30.00   0.00 120.00  169
  3  \w   -145.00  24.00   1.00    0.20    --   30.00   0.00 240.00  169
  4  \f      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       '\w and \f 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/[\s^2^(Fo^2^)+(0.1459P)^2^+8.7648P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_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)
;
_shelx_res_checksum              1503
_shelx_hkl_checksum              44882
_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