Spin dynamics in a Heisenberg weak antiferromagnetic chain of an iodide-bridged Cu(II) complex
Wakizaka, Masanori; Arczyński, Mirosław; Gupta, Shraddha; Takaishi, Shinya; Yamashita, Masahiro; Dalton Transactions  (2023) –; doi:10.1039/D3DT01840G

data_7713380
_publ_section_title
;
 Spin dynamics in a Heisenberg weak antiferromagnetic chain of an
 iodide-bridged Cu(II) complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01840G
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(I), C12 H28 Cu N4'
_chemical_formula_sum            'C12 H28 Cu I2 N4'
_chemical_formula_weight         545.72
_chemical_name_systematic        '[Cu(chxn)2I]I'
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-13
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2023-02-20 deposited with the CCDC.	2023-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   9.3636(2)
_cell_length_b                   9.3636(2)
_cell_length_c                   18.1008(3)
_cell_measurement_reflns_used    19945
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.9110
_cell_measurement_theta_min      3.2890
_cell_volume                     1374.40(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_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      120
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.961
_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     -6.00  19.00   0.50    1.00    --    0.00  45.00  18.22   50
  2  \w     20.00  49.00   0.50    1.00    --    0.00  45.00  18.22   58
  3  \w     59.00  89.00   0.50    1.00    --    0.00  45.00  18.22   60
  4  \w    -78.00 -53.00   0.50    1.00    --    0.00  45.00  60.00   50
  5  \w      5.00  34.00   0.50    1.00    --    0.00  45.00  60.00   58
  6  \w    -89.00 -58.00   0.50    1.00    --    0.00  45.00 150.00   62
  7  \w    -89.00  36.00   0.50    1.00    --    0.00  45.00 120.00  250
  8  \w     12.00  37.00   0.50    1.00    --    0.00  45.00   0.00   50
  9  \w     64.00  89.00   0.50    1.00    --    0.00  45.00   0.00   50
 10  \w    -43.00 -18.00   0.50    1.00    --    0.00  45.00  18.22   50
;
_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      -0.0658445000
_diffrn_orient_matrix_UB_12      0.0161975000
_diffrn_orient_matrix_UB_13      0.0046078000
_diffrn_orient_matrix_UB_21      0.0567247000
_diffrn_orient_matrix_UB_22      0.0859563000
_diffrn_orient_matrix_UB_23      -0.0016162000
_diffrn_orient_matrix_UB_31      -0.0103444000
_diffrn_orient_matrix_UB_32      -0.0016813000
_diffrn_orient_matrix_UB_33      -0.0388434000
_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  0.0349
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24499
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.781
_diffrn_reflns_theta_min         3.373
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.556
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_description       needle
_exptl_crystal_F_000             789
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 1179 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(10)
_refine_ls_extinction_coef       0.0009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         2940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0136
_refine_ls_R_factor_gt           0.0132
_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^)+(0.0156P)^2^+0.3201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0318
_refine_ls_wR_factor_ref         0.0320
_reflns_Friedel_coverage         0.695
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                2907
_reflns_number_total             2940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01840g2.cif
_cod_data_source_block           a_120k
_cod_original_cell_volume        1374.40(6)
_cod_database_code               7713380
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu C12 N4 I2 H28'
_chemical_oxdiff_usercomment     '120 K'
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.463
_diffrn_oxdiff_digest_frames
;
015e849c0b1746bba41609c44f1a26e3c400029e280
;
_diffrn_oxdiff_digest_hkl
;
01995236b594a0688454076619de1611d7c476
;
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C4(H4A,H4B)
;
_shelx_res_checksum              37859
_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 1.204
_oxdiff_exptl_absorpt_empirical_full_min 0.874