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_4003668
_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                 94.108(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   35.450(4)
_cell_length_b                   5.4065(6)
_cell_length_c                   5.3466(6)
_cell_measurement_reflns_used    2069
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.2890
_cell_measurement_theta_min      4.9900
_cell_volume                     1022.1(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.986
_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     -5.00  23.00   1.00    1.00    --  -33.50  57.00-150.00   28
  2  \w     23.00 100.00   1.00    1.00    --   36.65  77.00  90.00   77
  3  \w     81.00 106.00   1.00    1.00    --   36.65  77.00 -60.00   25
  4  \w     24.00  99.00   1.00    1.00    --   36.65  57.00  60.00   75
  5  \w      4.00  31.00   1.00    1.00    --   36.65 -99.00 -60.00   27
  6  \w     12.00  39.00   1.00    1.00    --   36.65  77.00 -60.00   27
  7  \w     25.00  99.00   1.00    1.00    --   36.65  57.00 -60.00   74
  8  \w      6.00  77.00   1.00    1.00    --   36.65 -99.00-180.00   71
  9  \w     44.00  71.00   1.00    1.00    --   36.65 -99.00  60.00   27
 10  \w     42.00  91.00   1.00    1.00    --   36.65  57.00-180.00   49
 11  \w    -22.00  51.00   1.00    1.00    --   36.65 -57.00-180.00   73
 12  \w     18.00 106.00   1.00    1.00    --   36.65  77.00 -30.00   88
 13  \w    133.00 178.00   1.00    1.00    --  108.00   0.00 -30.00   45
 14  \w     37.00 101.00   1.00    1.00    --  108.00   0.00 -30.00   64
 15  \w     89.00 164.00   1.00    1.00    --  108.00  50.00 -90.00   75
 16  \w     38.00 112.00   1.00    1.00    --  108.00-111.00 -30.00   74
 17  \w     88.00 124.00   1.00    1.00    --  108.00  77.00-180.00   36
 18  \w     40.00 127.00   1.00    1.00    --  108.00 -50.00 120.00   87
 19  \w     37.00 109.00   1.00    1.00    --  108.00-111.00  90.00   72
 20  \w     75.00 119.00   1.00    1.00    --  108.00 -77.00-180.00   44
 21  \w    102.00 176.00   1.00    1.00    --  108.00 111.00 120.00   74
 22  \w     99.00 130.00   1.00    1.00    --  108.00 -37.00 -90.00   31
 23  \w     44.00  71.00   1.00    1.00    --  108.00 -37.00 -90.00   27
 24  \w     45.00 125.00   1.00    1.00    --  108.00 -50.00  30.00   80
 25  \w    110.00 135.00   1.00    1.00    --  108.00 111.00 150.00   25
 26  \w    142.00 169.00   1.00    1.00    --  108.00 111.00 150.00   27
 27  \w    142.00 171.00   1.00    1.00    --  108.00  77.00-180.00   29
 28  \w     63.00 108.00   1.00    1.00    --  108.00-111.00-180.00   45
 29  \w    128.00 162.00   1.00    1.00    --  108.00  63.00  90.00   34
;
_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      0.0030156000
_diffrn_orient_matrix_UB_12      0.1164326000
_diffrn_orient_matrix_UB_13      -0.0785391000
_diffrn_orient_matrix_UB_21      -0.1013929000
_diffrn_orient_matrix_UB_22      0.1472281000
_diffrn_orient_matrix_UB_23      0.0344135000
_diffrn_orient_matrix_UB_31      0.1760019000
_diffrn_orient_matrix_UB_32      0.0823176000
_diffrn_orient_matrix_UB_33      0.0154925000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1035
_diffrn_reflns_av_unetI/netI     0.0761
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2996
_diffrn_reflns_point_group_measured_fraction_full 0.701
_diffrn_reflns_point_group_measured_fraction_max 0.686
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.321
_diffrn_reflns_theta_min         5.003
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.342
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37542
_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    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             494
_refine_diff_density_max         1.793
_refine_diff_density_min         -1.291
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.04(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1374
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0772
_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^)+(0.1610P)^2^+1.8594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2080
_refine_ls_wR_factor_ref         0.2256
_reflns_Friedel_coverage         0.251
_reflns_Friedel_fraction_full    0.331
_reflns_Friedel_fraction_max     0.311
_reflns_number_gt                1171
_reflns_number_total             1374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c02729_si_003.cif
_cod_data_source_block           exp_10971
_cod_database_code               4003668
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 98.00
_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:
 C3(H3), C6(H6), C7(H7), C8(H8), C9(H9)
3.e Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_res_checksum              30113
_shelx_hkl_checksum              86139
_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 2.709
_oxdiff_exptl_absorpt_empirical_full_min 0.462