Melamine-Induced Synthesis of a Structurally Perfect Kagomé Antiferromagnet
Shen, Yongbing; Sugimoto, Kunihisa; Yamashita, Satoshi; Yoshida, Takefumi; Nakazawa, Yasuhiro; Breedlove, Brian. K.; Zhang, Haitao; Yamashita, Masahiro; Chemical Communications  (2022) –; doi:10.1039/D2CC00416J

data_7129748
_publ_section_title
;
 Melamine-Induced Synthesis of a Structurally Perfect Kagom\'e
 Antiferromagnet
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00416J
_journal_year                    2022
_chemical_formula_moiety         'C60 H48 Cu3 N12, 3(F6 Si), 8(C3 H6 N6)'
_chemical_formula_sum            'C84 H96 Cu3 F18 N60 Si3'
_chemical_formula_weight         2563.09
_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_Hall           '-P 6 2c'
_space_group_name_H-M_alt        'P 6/m c c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-13
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2022-02-14 deposited with the CCDC.	2022-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   21.9791(5)
_cell_length_b                   21.9791(5)
_cell_length_c                   16.7774(5)
_cell_measurement_reflns_used    13679
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.0550
_cell_measurement_theta_min      2.6320
_cell_volume                     7019.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_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    -61.00 -36.00   0.50  119.84    --   -0.30  45.00  90.00   50
  2  \w    -24.00   2.00   0.50  119.84    --   -0.30  45.00  90.00   52
  3  \w      4.00  52.00   0.50  119.84    --   -0.30  45.00 120.00   96
  4  \w    -89.00  23.00   0.50  119.84    --   -0.30  45.00   0.00  224
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0218760000
_diffrn_orient_matrix_UB_12      -0.0003481000
_diffrn_orient_matrix_UB_13      -0.0309074000
_diffrn_orient_matrix_UB_21      0.0250325000
_diffrn_orient_matrix_UB_22      0.0030205000
_diffrn_orient_matrix_UB_23      0.0287379000
_diffrn_orient_matrix_UB_31      -0.0168395000
_diffrn_orient_matrix_UB_32      -0.0371213000
_diffrn_orient_matrix_UB_33      0.0024962000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51851
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.352
_diffrn_reflns_theta_min         2.428
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark purplish'
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             2622
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2493
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+4.6382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2249
_reflns_number_total             2493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00416j2.cif
_cod_data_source_block           exp_1565
_cod_original_cell_volume        7019.0(4)
_cod_database_code               7129748
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Cu B F'
_chemical_oxdiff_usercomment     '120 K'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(N6) \\sim
Ueq, Uanis(N5) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N2) = Uanis(N3) = Uanis(N10) = Uanis(N5) = Uanis(C8) = Uanis(N6) =
Uanis(C7) = Uanis(N7) = Uanis(C9)
3. Rigid body (RIGU) restrains
 N3, N7, C8, C7, N6, N5, N2, C9, N10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N3A, C7A, N5A, N2A, C9A, N10A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: N5(0.25) N2(0.25) H2A(0.25) H2B(0.25) C7(0.25) N3(0.25) C9(0.25)
 N10(0.25) H10A(0.25) H10B(0.25) C9A(0.25) C7A(0.25) N5A(0.25) N2A(0.25)
 H2AA(0.25) H2AB(0.25) N3A(0.25) N10A(0.25) H10C(0.25) H10D(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C1(H1), C2(H2)
5.b X=CH2 refined with riding coordinates:
 N6(H6A,H6B), N8(H8A,H8B), N2(H2A,H2B), N10(H10A,H10B), N2A(H2AA,H2AB),
 N10A(H10C,H10D)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              46400
_shelx_fab_checksum              28366
_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 1.318
_oxdiff_exptl_absorpt_empirical_full_min 0.832