Synthesis, crystal structure, magnetic and electronic properties of the caesium-based transition metal halide Cs3Fe2Br9
Wei, Fengxia; Brivio, Federico; Wu, Yue; Sun, Shijing; Bristowe, Paul D.; Cheetham, Anthony K.; Journal of Materials Chemistry C 6 (2018) 3573–; doi:10.1039/C7TC04798C

data_7236992
_publ_section_title
;
 Synthesis, crystal structure, magnetic and electronic properties of the
 caesium-based transition metal halide Cs3Fe2Br9
;
_journal_issue                   14
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              3573
_journal_paper_doi               10.1039/C7TC04798C
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         '0.25(Br20 Cs8 Fe4 H8 O4)'
_chemical_formula_sum            'Br5 Cs2 Fe H0.25 O'
_chemical_formula_weight         737.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-05
_audit_creation_method
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Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
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_audit_update_record
;
2017-09-16 deposited with the CCDC.
2017-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6652(3)
_cell_length_b                   10.4144(2)
_cell_length_c                   7.5110(2)
_cell_measurement_reflns_used    2569
_cell_measurement_temperature    298.8(3)
_cell_measurement_theta_max      28.0450
_cell_measurement_theta_min      2.7740
_cell_volume                     1147.15(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.8(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1183
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_details
;
  1 omega -109.00   58.00   1.0000    8.5700
omega____ theta____ kappa____ phi______ frames
    -      -27.2013   19.0000   30.0000 167

  2 omega -120.00  -35.00   1.0000    8.5700
omega____ theta____ kappa____ phi______ frames
    -      -27.2013 -178.0000  -30.0000 85

  3 omega  -17.00   26.00   1.0000    8.5700
omega____ theta____ kappa____ phi______ frames
    -       26.2638   80.0000 -128.0000 43

  4 omega -104.00   11.00   1.0000    8.5700
omega____ theta____ kappa____ phi______ frames
    -      -27.2013  -57.0000  -30.0000 115
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0166792000
_diffrn_orient_matrix_UB_12      0.0577716000
_diffrn_orient_matrix_UB_13      0.0379138000
_diffrn_orient_matrix_UB_21      0.0274898000
_diffrn_orient_matrix_UB_22      -0.0103142000
_diffrn_orient_matrix_UB_23      0.0763606000
_diffrn_orient_matrix_UB_31      0.0361246000
_diffrn_orient_matrix_UB_32      0.0345496000
_diffrn_orient_matrix_UB_33      -0.0406572000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6817
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.362
_diffrn_reflns_theta_min         2.778
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.925
_exptl_absorpt_correction_T_max  0.150
_exptl_absorpt_correction_T_min  0.032
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.270
_exptl_crystal_description       ribbon
_exptl_crystal_F_000             1277
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.2056
_exptl_crystal_size_min          0.095
_refine_diff_density_max         4.578
_refine_diff_density_min         -5.804
_refine_diff_density_rms         0.689
_refine_ls_extinction_coef       0.0010(5)
_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   1.163
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1399
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0816
_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^)+(0.1786P)^2^+36.9643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2927
_refine_ls_wR_factor_ref         0.3075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1140
_reflns_number_total             1399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7tc04798c2.cif
_cod_data_source_block           fw120_1_abs
_cod_original_cell_volume        1147.16(5)
_cod_original_formula_sum        'Br5 H0.25 Cs2 Fe O'
_cod_database_code               7236992
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cs2 Fe Br5 O H2'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 O1-H1
 0.9 with sigma of 0.02
;
_olex2_submission_special_instructions 'No special instructions were received'