A 9R-like 2D hybrid metal halide with remarkably low melting temperature.
Wang, Wei; Zhang, Jing-Meng; Jin, Ming-Liang; Jing, Chang-Qing; Zhang, Wen; Chemical communications (Cambridge, England) 61 (2024) 362–365; doi:10.1039/d4cc05616g

data_7134012
_publ_section_title
;
 A 9R-like 2D hybrid metal halide with remarkably low melting temperature.
;
_journal_issue                   2
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              362
_journal_page_last               365
_journal_paper_doi               10.1039/d4cc05616g
_journal_volume                  61
_journal_year                    2024
_chemical_formula_moiety         'Br10 Pb3, 4(C3 H10 N O)'
_chemical_formula_sum            'C12 H40 Br10 N4 O4 Pb3'
_chemical_formula_weight         1725.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2023-12-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-10-18 deposited with the CCDC.	2024-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.785(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6054(10)
_cell_length_b                   8.6447(3)
_cell_length_c                   20.0369(9)
_cell_measurement_reflns_used    9284
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.6260
_cell_measurement_theta_min      2.1910
_cell_volume                     3796.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_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 1.000
_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    -13.00  36.00   0.50    1.60    --    4.83 -99.00   0.00   98
  2  \w    -35.00   7.00   0.50    1.60    --    4.83 -77.00 150.00   84
  3  \w     -8.00  69.00   0.50    1.60    --    4.83  38.00 120.00  154
  4  \w     10.00  77.00   0.50    1.60    --    4.83  57.00 -30.00  134
  5  \w    -15.00  78.00   0.50    1.60    --    4.83  77.00-150.00  186
  6  \w     -8.00  35.00   0.50    1.60    --   -5.61  38.00-180.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0245537000
_diffrn_orient_matrix_UB_12      -0.0445655000
_diffrn_orient_matrix_UB_13      0.0019776000
_diffrn_orient_matrix_UB_21      0.0125899000
_diffrn_orient_matrix_UB_22      -0.0673752000
_diffrn_orient_matrix_UB_23      -0.0093053000
_diffrn_orient_matrix_UB_31      0.0168826000
_diffrn_orient_matrix_UB_32      -0.0145993000
_diffrn_orient_matrix_UB_33      0.0369073000
_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  0.0814
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18759
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.189
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.817
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
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    3.018
_exptl_crystal_description       block
_exptl_crystal_F_000             3072
_refine_diff_density_max         1.893
_refine_diff_density_min         -1.631
_refine_diff_density_rms         0.225
_refine_ls_extinction_coef       0.00034(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3338
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0673P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1112
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2811
_reflns_number_total             3338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05616g2.cif
_cod_data_source_block           (MHEA)4Pb3Br10
_cod_depositor_comments          'Adding full bibliography for 7134012.cif.'
_cod_database_code               7134012
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 H1-H2C
 2.2 with sigma of 0.02
2.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), N2(H2C,H2D), C5(H5A,H5B), C6(H6A,H6B)
2.b Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E), C4(H4A,H4B,H4C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_shelx_res_checksum              17480
_shelx_hkl_checksum              16882
_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 3.214
_oxdiff_exptl_absorpt_empirical_full_min 0.318