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_7705865
_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           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 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                   10.79470(10)
_cell_length_b                   10.79470(10)
_cell_length_c                   49.2881(7)
_cell_measurement_reflns_used    29294
_cell_measurement_temperature    103
_cell_measurement_theta_max      30.9490
_cell_measurement_theta_min      1.6380
_cell_volume                     5743.32(11)
_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 0.956
_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   15.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50   15.00    --  -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      -0.0362570000
_diffrn_orient_matrix_UB_12      -0.0054337000
_diffrn_orient_matrix_UB_13      -0.0119423000
_diffrn_orient_matrix_UB_21      0.0537023000
_diffrn_orient_matrix_UB_22      0.0095842000
_diffrn_orient_matrix_UB_23      -0.0080248000
_diffrn_orient_matrix_UB_31      0.0110180000
_diffrn_orient_matrix_UB_32      -0.0647675000
_diffrn_orient_matrix_UB_33      -0.0001881000
_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  0.0580
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            56610
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.448
_diffrn_reflns_theta_min         1.653
_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    3.283
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75876
_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    1.644
_exptl_crystal_description       plate
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 2495 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         8978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+6.4189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0845
_reflns_Friedel_coverage         0.691
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.922
_reflns_number_gt                7425
_reflns_number_total             8978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03615c2.cif
_cod_data_source_block           mn-oac-brsal-rrdpeda
_cod_original_cell_volume        5743.32(13)
_cod_original_formula_sum        'C31 H24.50 Br2 Mn N2.50 O4'
_cod_database_code               7705865
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C31 H24.5 Br2 Mn N2.5 O4'
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.574
_reflns_odcompleteness_completeness 95.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.38
_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. Others
 Fixed Sof: C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C32(0.5)
3.a Ternary CH refined with riding coordinates:
 C8(H8), C15(H15)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C23(H23), C17(H17), C10(H10), C28(H28), C5(H5), C3(H3), C18(H18),
 C22(H22), C2(H2), C20(H20), C14(H14), C11(H11), C27(H27), C13(H13), C25(H25),
 C21(H21), C12(H12)
3.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              9458
_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 1.460
_oxdiff_exptl_absorpt_empirical_full_min 0.616