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_1551907
_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 H17 Fe2 N12)'
_chemical_formula_sum            'C14 H8 Fe N6'
_chemical_formula_weight         316.11
_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                 97.66(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2188(19)
_cell_length_b                   8.217(2)
_cell_length_c                   21.481(13)
_cell_measurement_reflns_used    932
_cell_measurement_temperature    149.9(3)
_cell_measurement_theta_max      21.5950
_cell_measurement_theta_min      3.5010
_cell_volume                     1437.7(10)
_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      149.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.576
_diffrn_measured_fraction_theta_max 0.996
_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    -37.00  14.00   0.50   40.00    --   16.40  13.00 158.00  102
  2  \w    -71.00 106.00   0.50   40.00    --   16.40  60.00  30.00  354
  3  \w    -73.00  21.00   0.50   40.00    --   16.40  60.00 -60.00  188
  4  \w     37.00  67.00   0.50   40.00    --   16.40  60.00 -60.00   60
  5  \w     68.00 102.00   0.50   40.00    --   16.40  60.00 -60.00   68
  6  \w    -73.00  50.00   0.50   40.00    --   16.40  60.00 150.00  246
  7  \w     54.00  82.00   0.50   40.00    --   16.40  60.00 150.00   56
  8  \w    -43.00   0.00   0.50   40.00    --   16.40  60.00  90.00   86
  9  \w     63.00 106.00   0.50   40.00    --   16.40  60.00  90.00   86
 10  \w     50.00 104.00   0.50   40.00    --   16.40  13.00 158.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0647976000
_diffrn_orient_matrix_UB_12      0.0372149000
_diffrn_orient_matrix_UB_13      -0.0202557000
_diffrn_orient_matrix_UB_21      0.0567083000
_diffrn_orient_matrix_UB_22      0.0551273000
_diffrn_orient_matrix_UB_23      -0.0106121000
_diffrn_orient_matrix_UB_31      0.0129350000
_diffrn_orient_matrix_UB_32      -0.0549307000
_diffrn_orient_matrix_UB_33      -0.0243696000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_Laue_measured_fraction_full 0.576
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            740
_diffrn_reflns_point_group_measured_fraction_full 0.576
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.800
_diffrn_reflns_theta_min         3.522
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42735
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.267
_refine_diff_density_min         -2.017
_refine_diff_density_rms         0.243
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         740
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.1986
_refine_ls_R_factor_gt           0.1772
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1414P)^2^+83.5170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4110
_refine_ls_wR_factor_ref         0.4268
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                620
_reflns_number_total             740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            41557_2018_113_MOESM6_ESM.cif
_cod_data_source_block           livy3
_cod_original_cell_volume        1437.8(10)
_cod_database_code               1551907
_chemical_oxdiff_usercomment     MJ
_diffrn_oxdiff_ac3_digest_frames
;
0178cc1bc6c15a1d3908b210379485409a01354aee5
;
_diffrn_oxdiff_ac3_digest_hkl
;
01434d45faede29c20c3074044da822b7cf38a
;
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(6)
 0.12(3) 0.14(3) 0.08(3) 0.17(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 N005-C6 \\sim N5-C00C \\sim N00F-C0AA
 with sigma of 0.0002
 N5-C00C \\sim N005-C6 \\sim N00F-C0AA
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
C009 \\sim C00A: within 2A with sigma of 0.0002 and sigma for terminal atoms of
0.0004
N00F \\sim N5 \\sim N005: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
Uanis(Fe00) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 Fe00, N002, N003, C004, N005, C007, C009, C00A, C00B, C00C, C00E, C00D, C008,
 C00G, C5, C0AA, N00F, C6, C3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: C004(0.5) H004(0.5) N005(0.25) C007(0.5) H007(0.5) C009(0.5)
 C00A(0.5) C00B(0.5) H00B(0.5) C00C(0.5) H00C(0.25) C00E(0.5) H00E(0.5)
 C00D(0.5) C008(0.5) C00G(0.5) H00G(0.5) C5(0.5) H5(0.5) C0AA(0.5) H0AA(0.25)
 N00F(0.5) C6(0.5) H6(0.25) C3(0.5) H3(0.5) N5(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C004(H004), C007(H007), C00B(H00B), C00C(H00C), C00E(H00E), C00G(H00G),
 C5(H5), C0AA(H0AA), C6(H6), C3(H3)
7.b Fitted hexagon refined as free rotating group:
 C00E(C00D,C008,C00G,C5,C0AA)
;
_shelx_res_checksum              46502
_shelx_hkl_checksum              90230
_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 2.147
_oxdiff_exptl_absorpt_empirical_full_min 0.510