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_7705869
_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         '2(C30 H23 Cl2 Mn N2 O4), 0.7(O1)'
_chemical_formula_sum            'C60 H46 Cl4 Mn2 N4 O8.7'
_chemical_formula_weight         1213.89
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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            4
_cell_length_a                   6.5703(2)
_cell_length_b                   17.9817(4)
_cell_length_c                   45.3393(13)
_cell_measurement_reflns_used    16663
_cell_measurement_temperature    103
_cell_measurement_theta_max      30.9780
_cell_measurement_theta_min      1.7460
_cell_volume                     5356.6(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 0.999
_diffrn_measured_fraction_theta_max 0.938
_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   10.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50   10.00    --  -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      0.0431422000
_diffrn_orient_matrix_UB_12      0.0189210000
_diffrn_orient_matrix_UB_13      0.0122083000
_diffrn_orient_matrix_UB_21      -0.0818253000
_diffrn_orient_matrix_UB_22      0.0257541000
_diffrn_orient_matrix_UB_23      -0.0001972000
_diffrn_orient_matrix_UB_31      -0.0557147000
_diffrn_orient_matrix_UB_32      -0.0231633000
_diffrn_orient_matrix_UB_33      0.0097575000
_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  0.1065
_diffrn_reflns_av_unetI/netI     0.1442
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            52231
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.393
_diffrn_reflns_theta_min         1.760
_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    0.734
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52656
_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    1.505
_exptl_crystal_description       needle
_exptl_crystal_F_000             2486
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 3005 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         16175
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0696
_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^)+(0.0449P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1271
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.886
_reflns_number_gt                10522
_reflns_number_total             16175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03615c2.cif
_cod_data_source_block           mn-oac-clsal-ssdpeda
_cod_original_formula_sum        'C60 H46 Cl4 Mn2 N4 O8.70'
_cod_database_code               7705869
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C30 H23.7 Cl2 Mn N2 O4.35'
_reflns_odcompleteness_completeness 93.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.32
_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. Rigid bond restraints
 C31, C36, C37, C32, N3, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.008
 C28, C27, C23, C22, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.008
3. Uiso/Uaniso restraints and constraints
C31 \\sim C36 \\sim C37 \\sim C32 \\sim N3 \\sim O5: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
C28 \\sim C27 \\sim C23 \\sim C22 \\sim O2: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
4. Others
 Fixed Sof: O9(0.7)
5.a Ternary CH refined with riding coordinates:
 C38(H38), C15(H15), C45(H45), C8(H8)
5.b Aromatic/amide H refined with riding coordinates:
 C52(H52), C35(H35), C56(H56), C24(H24), C57(H57), C2(H2), C26(H26), C40(H40),
 C37(H37), C3(H3), C54(H54), C17(H17), C47(H47), C27(H27), C21(H21), C32(H32),
 C44(H44), C5(H5), C22(H22), C18(H18), C19(H19), C7(H7), C10(H10), C41(H41),
 C51(H51), C14(H14), C48(H48), C50(H50), C43(H43), C20(H20), C13(H13), C33(H33),
  C11(H11), C12(H12), C42(H42), C49(H49)
5.c Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              93851
_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 1.790
_oxdiff_exptl_absorpt_empirical_full_min 0.666