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_1551905
_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(C32 H24 Fe2 N8)'
_chemical_formula_sum            'C16 H12 Fe N4'
_chemical_formula_weight         316.15
_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                 92.418(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2809(6)
_cell_length_b                   8.2718(6)
_cell_length_c                   21.798(3)
_cell_measurement_reflns_used    2187
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      24.3230
_cell_measurement_theta_min      3.6210
_cell_volume                     1491.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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     32.00  78.00   0.50   15.00    --   -7.30  19.00-150.00   92
  2  \w    -89.00 -18.00   0.50   15.00    --   -7.30 -57.00 -90.00  142
  3  \w    -83.00  18.00   0.50   15.00    --   -7.30 -57.00   0.00  202
  4  \w    -39.00   7.00   0.50   15.00    --   -7.30  76.00-150.00   92
  5  \w     57.00  82.00   0.50   15.00    --   -7.30  76.00-150.00   50
  6  \w    -82.00  21.00   0.50   15.00    --   -7.30  19.00-150.00  206
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0116831000
_diffrn_orient_matrix_UB_12      -0.0609196000
_diffrn_orient_matrix_UB_13      -0.0226380000
_diffrn_orient_matrix_UB_21      -0.0432178000
_diffrn_orient_matrix_UB_22      0.0556850000
_diffrn_orient_matrix_UB_23      -0.0192393000
_diffrn_orient_matrix_UB_31      0.0730927000
_diffrn_orient_matrix_UB_32      0.0232343000
_diffrn_orient_matrix_UB_33      -0.0133677000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7862
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.633
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         1537
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0818
_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^)+(0.0647P)^2^+9.4910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1957
_refine_ls_wR_factor_ref         0.2027
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1310
_reflns_number_total             1537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            41557_2018_113_MOESM4_ESM.cif
_cod_data_source_block           rivy2
_cod_original_cell_volume        1491.8(2)
_cod_database_code               1551905
_chemical_oxdiff_formula         FeN3C25H80
_diffrn_oxdiff_ac3_digest_frames
;
01113ee1f60fadada0c178e9a30271dfe8007849be4
;
_diffrn_oxdiff_ac3_digest_hkl
;
015638fe3024bb0ef946f9afe9acacf250b380
;
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: C18(0.5) H18(0.5) C2(0.5) H2(0.5) C8(0.5) C7(0.5) C6(0.5) H6(0.5)
 C5(0.5) C4(0.5) C9(0.5) H9(0.5) C10(0.25) H10A(0.25) H10B(0.25) H10C(0.25)
 C11(0.25) H11A(0.25) H11B(0.25) H11C(0.25) C12(0.5) H12(0.5) C13(0.5) C14(0.5)
 C15(0.5) H15(0.5) C16(0.5) C17(0.5) C19(0.25) H19A(0.25) H19B(0.25) H19C(0.25)
 C20(0.25) H20A(0.25) H20B(0.25) H20C(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C2(H2), C6(H6), C9(H9), C12(H12), C15(H15)
4.b Fitted hexagon refined as free rotating group:
 C8(C7,C6,C5,C4,C9)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C)
;
_shelx_res_checksum              61778
_shelx_hkl_checksum              30690
_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 1.796
_oxdiff_exptl_absorpt_empirical_full_min 0.582