Two-Dimensional Perovskite Chiral Ferromagnets
Sun, Bing; Liu, Xiao-Fei; Li, Xiang-Yang; Zhang, Yamin; Shao, Xiangfeng; Yang, Dezheng; Zhang, Hao-Li; Chemistry of Materials  (2020) –; doi:10.1021/acs.chemmater.0c02729

data_4003669
_publ_section_title
;
 Two-Dimensional Perovskite Chiral Ferromagnets
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c02729
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Cl4 Cu, 2(C9 H14 N)'
_chemical_formula_sum            'C18 H28 Cl4 Cu N2'
_chemical_formula_weight         477.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.150(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   35.470(2)
_cell_length_b                   5.4017(3)
_cell_length_c                   5.3432(3)
_cell_measurement_reflns_used    3374
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.9410
_cell_measurement_theta_min      5.8910
_cell_volume                     1021.06(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1281
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.982
_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     -4.00  36.00   1.00    5.00    --    0.00  57.00  30.00   40
  2  \w    -91.00 -64.00   1.00   11.00    --  -33.50 -57.00 150.00   27
  3  \w     17.00  98.00   1.00   11.00    --   36.57  37.00  90.00   81
  4  \w    -29.00   0.00   1.00   11.00    --   36.57 -57.00 -90.00   29
  5  \w     27.00  90.00   1.00   11.00    --   36.57-125.00 -60.00   63
  6  \w     10.00  87.00   1.00   11.00    --   36.57  77.00 120.00   77
  7  \w     24.00 101.00   1.00   11.00    --   36.57  37.00   0.00   77
  8  \w     34.00  73.00   1.00   11.00    --   36.57 -99.00   0.00   39
  9  \w     25.00  98.00   1.00   11.00    --   36.57  57.00-150.00   73
 10  \w     44.00  70.00   1.00   11.00    --  108.00-111.00 -30.00   26
 11  \w     72.00 127.00   1.00   11.00    --  108.00 -63.00-180.00   55
 12  \w     39.00 127.00   1.00   11.00    --  108.00 -50.00  30.00   88
 13  \w     36.00 137.00   1.00   11.00    --  108.00 -25.00 -60.00  101
 14  \w    104.00 147.00   1.00   11.00    --  108.00 111.00   0.00   43
 15  \w    102.00 127.00   1.00   11.00    --  108.00 -50.00 120.00   25
 16  \w     43.00  76.00   1.00   11.00    --  108.00 -50.00 120.00   33
 17  \w     54.00 125.00   1.00   11.00    --  108.00 -91.00  60.00   71
 18  \w     37.00 112.00   1.00   11.00    --  108.00-111.00-120.00   75
 19  \w     99.00 136.00   1.00   11.00    --  108.00  63.00-180.00   37
 20  \w     90.00 155.00   1.00   11.00    --  108.00  50.00 120.00   65
 21  \w     74.00 112.00   1.00   11.00    --  108.00-111.00 -30.00   38
 22  \w     38.00  64.00   1.00   11.00    --  108.00-111.00   0.00   26
 23  \w     40.00 114.00   1.00   11.00    --  108.00 -63.00 -60.00   74
 24  \w     41.00 160.00   1.00   11.00    --  108.00 -12.00-180.00  119
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0203641000
_diffrn_orient_matrix_UB_12      -0.1009914000
_diffrn_orient_matrix_UB_13      0.0814906000
_diffrn_orient_matrix_UB_21      -0.0184509000
_diffrn_orient_matrix_UB_22      -0.1766886000
_diffrn_orient_matrix_UB_23      -0.0307298000
_diffrn_orient_matrix_UB_31      0.2012885000
_diffrn_orient_matrix_UB_32      -0.0268119000
_diffrn_orient_matrix_UB_33      0.0005006000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2879
_diffrn_reflns_point_group_measured_fraction_full 0.820
_diffrn_reflns_point_group_measured_fraction_max 0.803
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.091
_diffrn_reflns_theta_min         2.498
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             494
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1599
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1091P)^2^+1.0814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1362
_reflns_Friedel_coverage         0.468
_reflns_Friedel_fraction_full    0.603
_reflns_Friedel_fraction_max     0.578
_reflns_number_gt                1579
_reflns_number_total             1599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c02729_si_002.cif
_cod_data_source_block           exp_10972
_cod_database_code               4003669
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 97.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Others
 Fixed Sof: Cl2(0.5) Cl3(0.25) Cl4(0.25)
3.a Riding coordinates:
 N1(H1A,H1B,H1C)
3.b Ternary CH refined with riding coordinates:
 C2(H2)
3.c Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E)
3.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
3.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              49814
_shelx_hkl_checksum              71085
_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 5.608
_oxdiff_exptl_absorpt_empirical_full_min 0.491