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_1551906
_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         '2(C7 H4 Br Fe0.5 N2)'
_chemical_formula_sum            'C14 H8 Br2 Fe N4'
_chemical_formula_weight         447.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 92.440(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2958(6)
_cell_length_b                   8.2991(6)
_cell_length_c                   22.299(2)
_cell_measurement_reflns_used    5017
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      26.1220
_cell_measurement_theta_min      3.4540
_cell_volume                     1533.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_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      150.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -17.00  77.00   0.50   20.00    --    5.00  76.00 -30.00  188
  2  \w    -76.00  -1.00   0.50   20.00    --   -7.80 -57.00  90.00  150
  3  \w     35.00  71.00   0.50   20.00    --   -7.80  76.00  30.00   72
  4  \w    -97.00  30.00   0.50   20.00    --   -7.80 -38.00-180.00  254
  5  \w    -48.00  82.00   0.50   20.00    --   -7.80  76.00-150.00  260
  6  \w    -48.00  34.00   0.50   20.00    --   -7.80  76.00  30.00  164
  7  \w    -48.00  71.00   0.50   20.00    --   -7.80  76.00 150.00  238
  8  \w    -48.00  82.00   0.50   20.00    --   -7.80  76.00 -90.00  260
;
_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      -0.0743620000
_diffrn_orient_matrix_UB_12      -0.0413981000
_diffrn_orient_matrix_UB_13      -0.0042705000
_diffrn_orient_matrix_UB_21      -0.0020279000
_diffrn_orient_matrix_UB_22      0.0208201000
_diffrn_orient_matrix_UB_23      -0.0309136000
_diffrn_orient_matrix_UB_31      0.0422996000
_diffrn_orient_matrix_UB_32      -0.0718697000
_diffrn_orient_matrix_UB_33      -0.0062161000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1664
_diffrn_reflns_av_unetI/netI     0.0865
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16753
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.743
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.190
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
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    1.940
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.925
_refine_diff_density_min         -2.100
_refine_diff_density_rms         0.414
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.42(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.445
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3156
_refine_ls_number_restraints     398
_refine_ls_restrained_S_all      2.388
_refine_ls_R_factor_all          0.2505
_refine_ls_R_factor_gt           0.2372
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5361
_refine_ls_wR_factor_ref         0.5506
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2631
_reflns_number_total             3156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            41557_2018_113_MOESM5_ESM.cif
_cod_data_source_block           rivy10
_cod_database_code               1551906
_chemical_oxdiff_formula         FeBrC20H20N2
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.191
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.58(18)
 0.42(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C18-C20
 2.4 with sigma of 0.02
 C19-C20
 1.39 with sigma of 0.02
 C19-C21
 2.4 with sigma of 0.02
 C1-C7 = C1-C2
 2.1 with sigma of 0.02
 C9-C8 = C8-C14
 2.15 with sigma of 0.02
 C15-C21 = C15-C16
 2.1 with sigma of 0.02
 C17-C16 = C21-C20
 1.39 with sigma of 0.02
 C16-C20
 2.4 with sigma of 0.02
 C17-C21
 2.4 with sigma of 0.02
 C17-C20
 2.7 with sigma of 0.02
 C18-C16
 2.4 with sigma of 0.02
 C19-C16
 2.7 with sigma of 0.02
 C18-C17 = C19-C18
 1.39 with sigma of 0.02
 C22-C16
 2.1 with sigma of 0.02
 C22-C23
 2.15 with sigma of 0.02
 C23-C22
 2.15 with sigma of 0.02
 C28-C22
 2.15 with sigma of 0.02
 N4-C15
 1.35 with sigma of 0.02
 N4-C16 = N3-C21
 1.39 with sigma of 0.02
 N4-C22 = N3-C22
 1.35 with sigma of 0.02
 Fe2-C21 = Fe2-C23
 3 with sigma of 0.02
 N3-C23
 1.35 with sigma of 0.02
 N4-C23
 2.15 with sigma of 0.02
 C28-N3
 2.15 with sigma of 0.02
 Br1-C5
 1.9 with sigma of 0.02
 Br2-C10
 2.8 with sigma of 0.02
 Br2-C12
 2.8 with sigma of 0.02
 Br3-C18
 1.9 with sigma of 0.02
 Br3-C19
 2.8 with sigma of 0.02
 C27-Br4 \\sim Br4-C25
 with sigma of 0.002
 C6-Br1 \\sim Br1-C4
 with sigma of 0.002
 C12-Br2 \\sim Br2-C10
 with sigma of 0.002
 C17-Br3 \\sim Br3-C19
 with sigma of 0.002
4. Restrained planarity
 C12, C11, C10, C13, C9, C14
 with sigma of 0.1
 C17, C16, C21, C20, C19
 with sigma of 0.1
 C19, C18, C17, C16, C21, C20
 with sigma of 0.1
 C19, C20, C21, C16, C17, C18
 with sigma of 0.1
 C25, C24, C23, C28, C27, C26
 with sigma of 0.1
 C12, C11, C13, C10, C14, C9, N1, N2
 with sigma of 0.1
 C17, C16, C21, C15, C20, N4, N3
 with sigma of 0.1
 C22, N3, C23, N4
 with sigma of 0.1
 C28, C23, C24, C25, C26, C27, N4, N3, C22
 with sigma of 0.1
 Br4, C26, C25, C24, C23, C28, C27
 with sigma of 0.1
 C16, C21, C20, C19, C18, C17, Br3
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C8 \\sim C1: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
C12 \\sim C11: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(C19) = Uanis(C18) = Uanis(C20)
Uanis(C5) = Uanis(C6) = Uanis(C3) = Uanis(C4) = Uanis(C2)
Uanis(C22) = Uanis(C15)
Uanis(C26) = Uanis(C25) = Uanis(C24) = Uanis(C23) = Uanis(C28) = Uanis(C27)
6. Rigid body (RIGU) restrains
 N1, N2, C1, C8, C9, C14, C13, C10, C7, C2, Br2, C11, C12, Br1, C5, C6, C3, C4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Br4, C28, C27, C24, C23, C22, N4, C15, N3, C18, C16, C21, C20, C17, C19, Br3,
 C26, C25
 with sigma for 1-2 distances of 0.0021 and sigma for 1-3 distances of 0.0021
7. Others
 Fixed Sof: Br1(0.5) Br2(0.5) Br4(0.5) C1(0.5) H1(0.5) C8(0.5) H8(0.5) C9(0.5)
 C14(0.5) C13(0.5) H13(0.5) C12(0.5) H12(0.5) C11(0.5) C10(0.5) H10(0.5)
 C5(0.5) C6(0.5) H6(0.5) C7(0.5) C2(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5)
 C22(0.5) H22(0.5) Br3(0.5) C28(0.5) C27(0.5) H27(0.5) C26(0.5) C25(0.5)
 H25(0.5) C24(0.5) H24(0.5) C23(0.5) C18(0.5) C15(0.5) H15(0.5) C16(0.5)
 C21(0.5) C20(0.5) H20(0.5) C17(0.5) H17(0.5) C19(0.5) H19(0.5)
8.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C13(H13), C12(H12), C10(H10), C6(H6), C3(H3), C4(H4),
 C22(H22), C27(H27), C25(H25), C24(H24), C15(H15), C20(H20), C17(H17), C19(H19)
8.b Fitted hexagon refined as free rotating group:
 C9(C14,C13,C12,C11,C10), C5(C6,C7,C2,C3,C4), C28(C27,C26,C25,C24,C23)
;
_shelx_res_checksum              17029
_shelx_hkl_checksum              43306
_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 3.145
_oxdiff_exptl_absorpt_empirical_full_min 0.576