Synthesis, Crystal Structures and Semiconducting Properties of New Hexacyanidomettallates
Qiao, Xianji; Qiu, Yi; Xin, Junjie; Da, Chen; Ma, Zili; Corkett, Alex; Cai, Guohong; Cai, Guanqun; Qu, Shangqing; Wang, Yuchao; Zhu, Zhenyu; Gao, Yiman; Wang, Zhigang; Dronskowski, Richard; Li, Guobao; Sun, Junliang; Dalton Transactions  (2023) –; doi:10.1039/D3DT00384A

data_7712406
_publ_section_title
;
 Synthesis, Crystal Structures and Semiconducting Properties of New
 Hexacyanidomettallates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00384A
_journal_year                    2023
_chemical_formula_sum            'C6 Ca Fe K2 N6'
_chemical_formula_weight         330.23
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2022-04-06T13:22
_audit_creation_method           'created in GSAS-II'
_audit_update_record
;
2022-06-16 deposited with the CCDC.	2023-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3221(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.30124(29)
_cell_length_b                   7.51475(23)
_cell_length_c                   7.06772(21)
_cell_measurement_temperature    298
_cell_volume                     547.11(3)
_computing_structure_refinement
'GSAS-II (Toby & Von Dreele, J. Appl. Cryst. 46, 544-549, 2013)'
_diffrn_ambient_pressure         100
_diffrn_ambient_temperature      300
_diffrn_measurement_device_type  Rigaku
_diffrn_radiation_polarisn_ratio 0.7000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_exptl_crystal_density_diffrn    2.0046
_pd_block_id
2022-04-06T13:22|K2CaFe(CN)6|XianjiQiao|K2CaFe(CN)6
_pd_calc_method                  'Rietveld Refinement'
_pd_instr_location               ' ?'
_pd_meas_2theta_range_inc        0.01300
_pd_meas_2theta_range_max        119.98357
_pd_meas_2theta_range_min        5.01157
_pd_phase_name                   'Potassium manganese(II) hexacyanomanga'
_pd_proc_2theta_range_inc        0.01300
_pd_proc_2theta_range_max        119.91352
_pd_proc_2theta_range_min        4.94152
_pd_proc_info_datetime           2022-04-06T13:22
_pd_proc_info_excluded_regions   ' ?'
_pd_proc_ls_background_function
;
Background function: "chebyschev" function with 12 terms:
    1402.2(13), -146(7), -40(19), -4.2(6)e2, 2.14(7)e3, 1.03(16)e3, 
    -6.37(5)e3, -2.0(8)e2, 9.70(7)e3, -4.35(18)e3, -4.51(7)e3, 
    3.19(14)e3, 
;
_pd_proc_ls_pref_orient_corr
;
Simple spherical harmonic correction Order = 12
    Coefficients:  0:0:C(2,-2) = -0.35(3); 0:0:C(2,0) = -0.32(4); 
    0:0:C(2,2) = 0.038(30); 0:0:C(4,-4) = -0.13(6); 0:0:C(4,-2) = 0.65(5); 
    0:0:C(4,0) = -0.99(7); 0:0:C(4,2) = 1.48(6); 0:0:C(4,4) = 0.71(7); 
    0:0:C(6,-6) = -0.28(11); 0:0:C(6,-4) = -0.76(8); 0:0:C(6,-2) = -0.56(8); 
    0:0:C(6,0) = 0.77(9); 0:0:C(6,2) = -0.52(11); 0:0:C(6,4) = -1.19(9); 
    0:0:C(6,6) = -0.79(10); 0:0:C(8,-8) = -0.79(13); 0:0:C(8,-6) = -0.37(11); 
    0:0:C(8,-4) = -0.48(13); 0:0:C(8,-2) = -0.50(10); 0:0:C(8,0) = 0.36(12); 
    0:0:C(8,2) = 0.58(11); 0:0:C(8,4) = 1.18(11); 0:0:C(8,6) = 1.41(12); 
    0:0:C(8,8) = 0.77(15); 0:0:C(10,-10) = -0.75(22); 0:0:C(10,-8) = -0.41(14); 
    0:0:C(10,-6) = -1.21(16); 0:0:C(10,-4) = 0.13(15); 0:0:C(10,-2) = -0.01(17); 
    0:0:C(10,0) = -0.62(18); 0:0:C(10,2) = -0.05(17); 0:0:C(10,4) = -1.28(13); 
    0:0:C(10,6) = -1.14(14); 0:0:C(10,8) = -0.29(14); 0:0:C(10,10) = -0.52(17); 
    0:0:C(12,-12) = -0.05(22); 0:0:C(12,-10) = 0.14(23); 0:0:C(12,-8) = 0.79(19); 
    0:0:C(12,-6) = 1.00(24); 0:0:C(12,-4) = -1.20(23); 0:0:C(12,-2) = -0.12(20); 
    0:0:C(12,0) = 0.50(18); 0:0:C(12,2) = -1.40(18); 0:0:C(12,4) = -0.19(20); 
    0:0:C(12,6) = -1.29(20); 0:0:C(12,8) = 0.90(15); 0:0:C(12,10) = -0.03(24); 
    0:0:C(12,12) = -1.26(20); 
;
_pd_proc_ls_profile_function
;
Finger-Cox-Jephcoat function parameters U, V, W, X, Y, SH/L:
  peak variance(Gauss) = Utan(Th)^2^+Vtan(Th)+W:
  peak HW(Lorentz) = X/cos(Th)+Ytan(Th); SH/L = S/L+H/L
  U, V, W in (centideg)^2^, X & Y in centideg
    8.8(19), -2.000, 2.30(13), 1.09(14), 2.8(6), 0.0131(11), 
  Crystallite size in microns with "isotropic" model:
  parameters: Size, G/L mix
    1.000, 1.000, 
  Microstrain, "isotropic" model (10^6^ * delta Q/Q)
    parameters: Mustrain, G/L mix
    1000.000, 1.000, 

;
_pd_proc_ls_prof_R_factor        0.02002
_pd_proc_ls_prof_wR_expected     0.02428
_pd_proc_ls_prof_wR_factor       0.02602
_pd_proc_number_of_points        8845
_pd_spec_mounting                ' ?'
_refine_ls_goodness_of_fit_all   1.077
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_R_Fsqd_factor         0.14682
_refine_ls_wR_factor_obs         0.02602
_reflns_d_resolution_high        0.890
_reflns_d_resolution_low         6.071
_reflns_limit_h_max              8
_reflns_limit_h_min              8
_reflns_limit_k_max              6
_reflns_limit_k_min              6
_reflns_limit_l_max              1
_reflns_limit_l_min              1
_reflns_number_total             813
_cod_data_source_file            d3dt00384a2.cif
_cod_data_source_block           K2CaFe(CN)6
_cod_original_cell_volume        547.11(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7712406
_refine_ls_r_f_factor            0.14598
_gsas_proc_ls_prof_r_b_factor    0.02988
_gsas_proc_ls_prof_wr_b_factor   0.04486