Polymorphism in A3MF6 (A = Rb, Cs; M = Al, Ga) Grown using Mixed Halide Fluxes
Morrison, Gregory; Masachchi, Lakshani W.; Tisdale, Hunter B.; Chang, Tieyan; Jones, Virginia G.; Zamorano, K. Pilar; Breton, Logan S.; Smith, Mark D.; Chen, Yu-Sheng; Zur Loye, Hans-Conrad; Dalton Transactions  (2023) –; doi:10.1039/D3DT00352C

data_7713199
_publ_section_title
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 Polymorphism in A3MF6 (A = Rb, Cs; M = Al, Ga) Grown using Mixed Halide
 Fluxes
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00352C
_journal_year                    2023
_chemical_formula_moiety         '0.08(Cs36 F72 Ga12)'
_chemical_formula_sum            'Cs3 F6 Ga'
_chemical_formula_weight         582.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-12
_audit_creation_method
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Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
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_audit_update_record
;
2022-07-28 deposited with the CCDC.	2023-05-19 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 109.7000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   11.3996(3)
_cell_length_b                   19.7132(4)
_cell_length_c                   11.4551(4)
_cell_measurement_reflns_used    9626
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      36.1275
_cell_measurement_theta_min      3.2644
_cell_volume                     2423.55(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX3 v2016.5-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 013)'
_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_temperature      299.94
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            102291
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.137
_diffrn_reflns_theta_min         2.161
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    16.760
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0971 before and 0.0580 after correction.
The Ratio of minimum to maximum transmission is 0.8360.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.789
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.065
_refine_diff_density_min         -3.099
_refine_diff_density_rms         0.243
_refine_ls_extinction_coef       0.000159(14)
_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   1.160
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         4759
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+25.0230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4466
_reflns_number_total             4759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00352c2.cif
_cod_data_source_block           Cs3GaF6_C2_m
_cod_database_code               7713199
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.554
_shelx_estimated_absorpt_t_min   0.387
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.9297(14)
 0.0703(14)
2. Uiso/Uaniso restraints and constraints
Uanis(F2A) = Uanis(F2B) = Uanis(F2C)
Uanis(Cs1A) = Uanis(Cs1B)
Uanis(F1A) = Uanis(F1B)
3. Others
 2*[Sof(Cs1A)+Sof(Cs1B)+Sof(F1A)+Sof(F2A)+Sof(F2C)]+1*[Sof(F1B)+Sof(F2B)]=1
 with esd of 0.001
 Sof(Cs1A)=1-FVAR(1)
 Sof(Cs1B)=Sof(F1A)=Sof(F2A)=Sof(F2C)=FVAR(1)
 Sof(F1B)=0.5*FVAR(3)
 Sof(F2B)=FVAR(2)
;
_shelx_res_checksum              73933
_shelx_hkl_checksum              40828
_olex2_submission_special_instructions 'No special instructions were received'