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_7713201
_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         '0.02(Cs144 F288 Ga48)'
_chemical_formula_sum            'Cs3 F6 Ga'
_chemical_formula_weight         582.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_audit_creation_date             2022-02-23
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
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_audit_update_record
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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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            48
_cell_length_a                   13.1762(8)
_cell_length_b                   18.7515(12)
_cell_length_c                   39.488(3)
_cell_measurement_reflns_used    9170
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      36.2981
_cell_measurement_theta_min      2.4048
_cell_volume                     9756.4(11)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      299.26
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_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  0.0403
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            215240
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.334
_diffrn_reflns_theta_min         2.405
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    16.653
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0919 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.7567.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.758
_exptl_crystal_description       shard
_exptl_crystal_F_000             12000
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.519
_refine_diff_density_min         -1.920
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.0000116(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   1.104
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         5926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0180P)^2^+173.9705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5152
_reflns_number_total             5926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00352c2.cif
_cod_data_source_block           mor2123a_b
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7713201
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.389
_shelx_estimated_absorpt_t_min   0.349
_olex2_refinement_description
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1. Uiso/Uaniso restraints and constraints
Uanis(Cs1A) = Uanis(Cs1B)
Uanis(Cs2A) = Uanis(Cs2B)
Uanis(Cs3A) = Uanis(Cs3B)
Uanis(Cs4A) = Uanis(Cs4B)
Uanis(Cs5A) = Uanis(Cs5B)
2. Others
 Sof(Cs4A)=1-FVAR(1)
 Sof(Cs4B)=FVAR(1)
 Sof(Cs1A)=1-FVAR(2)
 Sof(Cs1B)=FVAR(2)
 Sof(Cs3A)=1-FVAR(3)
 Sof(Cs3B)=FVAR(3)
 Sof(Cs2A)=1-FVAR(4)
 Sof(Cs2B)=FVAR(4)
 Sof(Cs5A)=0.5*(1-FVAR(6))
 Sof(Cs5B)=0.5*FVAR(6)
 Sof(F4A)=1-FVAR(6)
 Sof(F4B)=Sof(F4C)=0.5*FVAR(7)
 Fixed Sof: F9(0.5) F10A(0.5) F10B(0.5)
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_shelx_res_checksum              35431
_shelx_hkl_checksum              98290
_olex2_submission_special_instructions 'No special instructions were received'