Organic-inorganic haloargentate hybrids of [Me-dabco]Ag<sub>2</sub>X<sub>3</sub> (X = I or Br) with halide ions manipulating the crystal structure, phase transition, and dielectric behavior.
Pan, Xue-Wei; Li, Qing-Qing; Zhai, Lu; Zhang, Jin; Liu, Wen-Long; Ren, Xiao-Ming; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt01366a

data_7713291
_publ_section_title
;
 Organic-inorganic haloargentate hybrids of
 [Me-dabco]Ag<sub>2</sub>X<sub>3</sub> (X = I or Br) with halide ions
 manipulating the crystal structure, phase transition, and dielectric
 behavior.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt01366a
_journal_year                    2023
_chemical_formula_moiety
'4(C7 H15 Ag2 Br3 N2), 2(C7 H15 Ag4 Br6 N2), C7 H14.637 N2, C7 H16 N2'
_chemical_formula_sum            'C56 H120.65 Ag16 Br24 N16'
_chemical_formula_weight         4662.09
_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   geom
_audit_creation_date             2023-03-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-03-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.169(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.6830(17)
_cell_length_b                   7.4510(6)
_cell_length_c                   34.055(3)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.753
_cell_measurement_theta_min      2.660
_cell_volume                     5248.2(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microsource'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            49598
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         1.969
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    12.088
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1467 before and 0.0736 after correction.
The Ratio of minimum to maximum transmission is 0.4339.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.950
_exptl_crystal_description       needle
_exptl_crystal_F_000             4321
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.167
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.230
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.056(10)
_refine_ls_extinction_coef       0.00055(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1129
_refine_ls_number_reflns         22445
_refine_ls_number_restraints     1147
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0380P)^2^+10.2348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.857
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                16452
_reflns_number_total             22445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01366a2.cif
_cod_data_source_block           agbr
_cod_original_cell_volume        5248.1(8)
_cod_database_code               7713291
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.944(10)
 0.056(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C49A)=Sof(H49C)=Sof(H49D)=Sof(C48A)=Sof(H48C)=Sof(C50A)=Sof(H50C)=
 Sof(H50D)=Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C53A)=Sof(H53C)=Sof(H53D)=
 Sof(C52A)=Sof(H52C)=Sof(H52D)=1-FVAR(1)
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=
 Sof(H50B)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=
 Sof(H53A)=Sof(H53B)=FVAR(1)
 Sof(H15A)=Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=
 Sof(C42A)=Sof(H42C)=Sof(H42D)=Sof(C41A)=Sof(H41C)=Sof(H41D)=Sof(C43A)=
 Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(H44C)=Sof(H44D)=1-FVAR(2)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=
 Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=
 Sof(H46A)=Sof(H46B)=Sof(H15)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 N15(H15), N15(H15A)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C15(H15B,H15C), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
  C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B),
 C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B),
  C53(H53A,H53B), C0AA(H0AA,H0AB), C1AA(H1AA,H1AB), C2AA(H2AA,H2AB), C49A(H49C,
 H49D), C50A(H50C,H50D), C51A(H51C,H51D), C53A(H53C,H53D), C52A(H52C,H52D),
 C45A(H45C,H45D), C46A(H46C,H46D), C42A(H42C,H42D), C41A(H41C,H41D), C43A(H43C,
 H43D), C44A(H44C,H44D)
5.c Aromatic/amide H refined with riding coordinates:
 C48A(H48C)
5.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C47(H47A,
 H47B,H47C)
;
_shelx_res_checksum              75279
_shelx_hkl_checksum              82756
_olex2_submission_special_instructions 'No special instructions were received'