Chiral weak ferromagnets formed in one-dimensional organic–inorganic hybrid manganese chloride hydrates
Taniguchi, Kouji; Huang, Po-Jung; Kimura, Shojiro; Miyasaka, Hitoshi; Dalton Transactions  (2022) –; doi:10.1039/D2DT02928F

data_7711600
_publ_section_title
;
 Chiral weak ferromagnets formed in one-dimensional organic--inorganic
 hybrid manganese chloride hydrates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02928F
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_moiety         '2(Cl4 H2 Mn O), 4(C9 H14 N)'
_chemical_formula_sum            'C18 H30 Cl4 Mn N2 O'
_chemical_formula_weight         487.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-01
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-07-15 deposited with the CCDC.	2022-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.502(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5439(4)
_cell_length_b                   7.2896(2)
_cell_length_c                   17.6559(5)
_cell_measurement_reflns_used    14559
_cell_measurement_temperature    103
_cell_measurement_theta_max      30.8070
_cell_measurement_theta_min      2.3130
_cell_volume                     2257.89(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.840
_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    -14.00  68.00   0.50  277.63    --   -3.97  38.00-150.00  164
  2  \w    -11.00  37.00   0.50  277.63    --    4.28 -99.00-180.00   96
  3  \w    -11.00  37.00   0.50  277.63    --    4.28 -99.00  30.00   96
  4  \w     -7.00  77.00   0.50  277.63    --    4.28  38.00 -30.00  168
  5  \w    -26.00  68.00   0.50  277.63    --   -3.97  77.00-120.00  188
  6  \w    -11.00  32.00   0.50  277.63    --    4.28 -99.00 120.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0110367000
_diffrn_orient_matrix_UB_12      -0.0213487000
_diffrn_orient_matrix_UB_13      -0.0377235000
_diffrn_orient_matrix_UB_21      -0.0133223000
_diffrn_orient_matrix_UB_22      0.0910860000
_diffrn_orient_matrix_UB_23      -0.0050738000
_diffrn_orient_matrix_UB_31      0.0365463000
_diffrn_orient_matrix_UB_32      0.0267501000
_diffrn_orient_matrix_UB_33      -0.0128440000
_diffrn_radiation_collimation    0.3
_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  0.0427
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33573
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.778
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.259
_diffrn_reflns_theta_min         1.629
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       needle
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.009
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 3996 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         11472
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0303P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0644
_reflns_Friedel_coverage         0.732
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.708
_reflns_number_gt                10180
_reflns_number_total             11472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02928f2.cif
_cod_data_source_block           r-mephc2h3nh3mncl4h2o_auto
_cod_database_code               7711600
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C18H30Cl4Mn1N2O1
_diffrn_oxdiff_digest_frames
;
01d61265faf96849d87cffb65b92fa2006000253ca8
;
_diffrn_oxdiff_digest_hkl
;
017b80d0a557134e2145f54ccdd2f35ab1af47
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O2(H2D,H2E), O1(H1F,H1G)
2.b Ternary CH refined with riding coordinates:
 C20(H20), C29(H29), C11(H11), C2(H2)
2.c Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C1(H1D,H1E), C28(H28A,H28B), C10(H10A,H10B)
2.d Aromatic/amide H refined with riding coordinates:
 C33(H33), C32(H32), C27(H27), C36(H36), C26(H26), C23(H23), C5(H5), C35(H35),
 C34(H34), C25(H25), C14(H14), C18(H18), C24(H24), C9(H9), C15(H15), C16(H16),
 C7(H7), C6(H6), C17(H17), C8(H8)
2.e Idealised Me refined as rotating group:
 N4(H4A,H4B,H4C), N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N3(H3D,H3E,H3F), C30(H30A,
 H30B,H30C), C21(H21A,H21B,H21C), C3(H3A,H3B,H3C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              16845
_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 1.499
_oxdiff_exptl_absorpt_empirical_full_min 0.794