A core-shell model of polymetallic hybrid metal halides.
Tian, Dongjie; Lin, Jie; Mesbah, Adel; Zhou, Jiajing; Yang, Mianji; Gautier, Romain; Chen, Xi; Chemical communications (Cambridge, England) 60 (2024) 12924–12927; doi:10.1039/d4cc04454a

data_7133837
_publ_section_title
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 A core-shell model of polymetallic hybrid metal halides.
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_journal_issue                   88
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12924
_journal_page_last               12927
_journal_paper_doi               10.1039/d4cc04454a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'Br10 Pb2, 2(C6 H18 N3), H2 O'
_chemical_formula_sum            'C12 H38 Br10 N6 O Pb2'
_chemical_formula_weight         1495.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-25
_audit_creation_method
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Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-25 deposited with the CCDC.	2024-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.25
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7743(4)
_cell_length_b                   17.5198(7)
_cell_length_c                   13.7748(4)
_cell_measurement_reflns_used    6732
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      2.30
_cell_volume                     3304.42(19)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            57011
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.400
_diffrn_reflns_theta_min         1.888
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.287
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0082
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.007
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.229
_refine_diff_density_min         -1.225
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6748
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0383P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5250
_reflns_number_total             6748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04454a2.cif
_cod_data_source_block           mo_0228_2_0ma
_cod_depositor_comments          'Adding full bibliography for 7133837.cif.'
_cod_original_cell_volume        3304.43(19)
_cod_database_code               7133837
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.469
_shelx_estimated_absorpt_t_min   0.348
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N5-C11 = N3-C13
 1.47 with sigma of 0.01
 C13-C3 = C11-C7
 1.52 with sigma of 0.01
 H6B-H1D
 2.22 with sigma of 0.01
 N2-C7 \\sim N2-C3
 with sigma of 0.02
 C7-N5 \\sim C3-N3
 with sigma of 0.04
 N2-C11 \\sim N2-C13
 with sigma of 0.04
 C7-C11 \\sim C3-C13
 with sigma of 0.02
 N5-C11 \\sim N3-C13
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C7 \\sim N5 \\sim C11 \\sim C3 \\sim N3 \\sim C13 \\sim N2: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(N3)=Sof(H3C)=Sof(H3D)=Sof(H3E)=Sof(C13)=
 Sof(H13A)=Sof(H13B)=1-FVAR(1)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(N5)=Sof(H5C)=Sof(H5D)=Sof(H5E)=Sof(C11)=
 Sof(H11A)=Sof(H11B)=FVAR(1)
 Fixed Sof: H2B(0.33333) H2A(0.6666)
5.a Free rotating group:
 O1(H1C,H1D)
5.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2B), N2(H2A)
5.c Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B), N6(H6A,H6B), C1(H1A,H1B), C4(H4C,H4D), C6(H6C,H6D), C8(H8A,H8B),
 C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B), C7(H7A,H7B), C2(H2C,H2D),
 C9(H9A,H9B), C5(H5A,H5B), C11(H11A,H11B), C3(H3A,H3B), C13(H13A,H13B)
5.d Idealised Me refined as rotating group:
 N7(H7C,H7D,H7E), N5(H5C,H5D,H5E), N3(H3C,H3D,H3E)
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_shelx_res_checksum              79659
_shelx_hkl_checksum              58399
_olex2_submission_special_instructions 'No special instructions were received'