Canting angle dependence of single-chain magnet behaviour in chirality-introduced antiferromagnetic chains of acetate-bridged manganese(III) salen-type complexes.
Huang, Po-Jung; Miyasaka, Hitoshi; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16970–16978; doi:10.1039/d0dt03615c

data_7705866
_publ_section_title
;
 Canting angle dependence of single-chain magnet behaviour in
 chirality-introduced antiferromagnetic chains of acetate-bridged
 manganese(III) salen-type complexes.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16970
_journal_page_last               16978
_journal_paper_doi               10.1039/d0dt03615c
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C30 H23 Br2 Mn N2 O4, 0.5(C2 H3 N)'
_chemical_formula_sum            'C31 H24.5 Br2 Mn N2.5 O4'
_chemical_formula_weight         710.79
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-08 deposited with the CCDC.	2020-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.7928(3)
_cell_length_b                   10.7928(3)
_cell_length_c                   49.2053(11)
_cell_measurement_reflns_used    11049
_cell_measurement_temperature    103
_cell_measurement_theta_max      28.0890
_cell_measurement_theta_min      1.9110
_cell_volume                     5731.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      103
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.626
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.971
_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   -110.00  70.00   0.50   20.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50   20.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'AFC10: Fixed Chi 2 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0608580000
_diffrn_orient_matrix_UB_12      -0.0172715000
_diffrn_orient_matrix_UB_13      -0.0038997000
_diffrn_orient_matrix_UB_21      -0.0197147000
_diffrn_orient_matrix_UB_22      0.0622969000
_diffrn_orient_matrix_UB_23      0.0015119000
_diffrn_orient_matrix_UB_31      0.0150977000
_diffrn_orient_matrix_UB_32      0.0117100000
_diffrn_orient_matrix_UB_33      -0.0137977000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1698
_diffrn_reflns_av_unetI/netI     0.1773
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            56460
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.473
_diffrn_reflns_theta_min         1.655
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.290
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       plate
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Flack x determined using 1232 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.030(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         9044
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1819
_refine_ls_R_factor_gt           0.0749
_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^)+(0.0539P)^2^+0.3465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1451
_reflns_Friedel_coverage         0.677
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                4699
_reflns_number_total             9044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03615c2.cif
_cod_data_source_block           mn-brsal-ssdpeda
_cod_original_formula_sum        'C31 H24.50 Br2 Mn N2.50 O4'
_cod_database_code               7705866
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C31 H24.5 Br2 Mn N2.5 O4'
_reflns_odcompleteness_completeness 97.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.40
_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. Restrained distances
 C31-C32
 1.54 with sigma of 0.02
3. Rigid bond restraints
 N3, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.008
4. Uiso/Uaniso restraints and constraints
N3 \\sim C31 \\sim C32: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
5. Others
 Fixed Sof: C31(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5)
6.a Ternary CH refined with riding coordinates:
 C15(H15), C8(H8)
6.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C26(H26), C7(H7), C11(H11), C17(H17), C10(H10), C2(H2), C18(H18),
 C24(H24), C21(H21), C12(H12), C14(H14), C5(H5), C0AA(H0AA), C13(H13), C20(H20),
  C27(H27), C19(H19)
6.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              3414
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.762
_oxdiff_exptl_absorpt_empirical_full_min 0.779