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_7712401
_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 Fe Mg N6 Na2'
_chemical_formula_weight         282.24
_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             2022-05-17T00:19
_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                 91.7480(28)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.43198(18)
_cell_length_b                   7.47537(23)
_cell_length_c                   7.28416(30)
_cell_measurement_temperature    298
_cell_volume                     567.78(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    1.6509
_pd_block_id
2022-05-17T00:19|Na2MgFe(CN)6|XianjiQiao|Na2MgFe(CN)6
_pd_calc_method                  'Rietveld Refinement'
_pd_instr_location               ' ?'
_pd_meas_number_of_points        8757
_pd_phase_name                   'C12 Fe2 Mn N12 Na4 Ni O4'
_pd_proc_info_datetime           2022-05-17T00:19
_pd_proc_info_excluded_regions   ' ?'
_pd_proc_ls_background_function
;
Background function: "chebyschev" function with 24 terms:
    6651(5), -1756(19), -3.6(7)e2, -6.79(9)e3, 1.466(22)e4, 9.13(9)e3, 
    -2.200(8)e4, 5.3(9)e2, 1.077(21)e4, -1.303(8)e4, -1.312(15)e4, 
    2.006(6)e4, 3.75(5)e3, -2.16(8)e3, 9.33(18)e3, -8.31(11)e3, 
    9.80(24)e3, -9.91(11)e3, 4.94(18)e3, -5.91(8)e3, -3.57(4)e3, 
    2.56(5)e3, -1.29(3)e4, 1.308(19)e4, 
;
_pd_proc_ls_pref_orient_corr
;
Simple spherical harmonic correction Order = 24
    Coefficients:  0:0:C(2,-2) = 2.25(31); 0:0:C(2,0) = 0.9(3); 
    0:0:C(2,2) = 1.05(21); 0:0:C(4,-4) = 2.4(3); 0:0:C(4,-2) = 3.20(27); 
    0:0:C(4,0) = 0.0(7); 0:0:C(4,2) = -1.21(28); 0:0:C(4,4) = 1.0(5); 
    0:0:C(6,-6) = -3.7(6); 0:0:C(6,-4) = 0.3(6); 0:0:C(6,-2) = -1.3(7); 
    0:0:C(6,0) = 4.4(7); 0:0:C(6,2) = 0.7(5); 0:0:C(6,4) = 1.0(5); 
    0:0:C(6,6) = -0.9(6); 0:0:C(8,-8) = -5.5(9); 0:0:C(8,-6) = 3.6(6); 
    0:0:C(8,-4) = 0.2(6); 0:0:C(8,-2) = 1.2(9); 0:0:C(8,0) = 5.5(10); 
    0:0:C(8,2) = -1.0(9); 0:0:C(8,4) = 3.5(7); 0:0:C(8,6) = 1.2(6); 
    0:0:C(8,8) = 1.2(9); 0:0:C(10,-10) = -7.2(9); 0:0:C(10,-8) = -6.3(9); 
    0:0:C(10,-6) = -2.2(9); 0:0:C(10,-4) = 0.6(9); 0:0:C(10,-2) = -1.1(12); 
    0:0:C(10,0) = 7.2(14); 0:0:C(10,2) = 2.3(9); 0:0:C(10,4) = 3.1(11); 
    0:0:C(10,6) = -0.2(9); 0:0:C(10,8) = 1.3(10); 0:0:C(10,10) = 7.0(12); 
    0:0:C(12,-12) = 4.6(11); 0:0:C(12,-10) = -0.8(10); 0:0:C(12,-8) = -2.8(8); 
    0:0:C(12,-6) = -1.1(10); 0:0:C(12,-4) = 1.0(12); 0:0:C(12,-2) = -5.6(8); 
    0:0:C(12,0) = 2.6(10); 0:0:C(12,2) = 0.1(7); 0:0:C(12,4) = 6.0(14); 
    0:0:C(12,6) = 1.4(10); 0:0:C(12,8) = 5.4(10); 0:0:C(12,10) = 5.1(10); 
    0:0:C(12,12) = 3.4(11); 0:0:C(14,-14) = 8.9(13); 0:0:C(14,-12) = -12.1(15); 
    0:0:C(14,-10) = 1.0(14); 0:0:C(14,-8) = -0.2(14); 0:0:C(14,-6) = 2.3(10); 
    0:0:C(14,-4) = -2.1(14); 0:0:C(14,-2) = 0.4(19); 0:0:C(14,0) = -3.3(18); 
    0:0:C(14,2) = -1.7(11); 0:0:C(14,4) = 13.0(17); 0:0:C(14,6) = 3.6(9); 
    0:0:C(14,8) = 0.0(12); 0:0:C(14,10) = -0.9(13); 0:0:C(14,12) = -7.7(11); 
    0:0:C(14,14) = 0.3(15); 0:0:C(16,-16) = 12.1(17); 0:0:C(16,-14) = -3.5(13); 
    0:0:C(16,-12) = 1.4(14); 0:0:C(16,-10) = 7.1(11); 0:0:C(16,-8) = 0.1(16); 
    0:0:C(16,-6) = 5.0(17); 0:0:C(16,-4) = -4.7(9); 0:0:C(16,-2) = 1.2(15); 
    0:0:C(16,0) = -4.0(18); 0:0:C(16,2) = 1.2(12); 0:0:C(16,4) = 2.3(16); 
    0:0:C(16,6) = 7.4(14); 0:0:C(16,8) = 12.1(14); 0:0:C(16,10) = -4.0(9); 
    0:0:C(16,12) = -4.1(13); 0:0:C(16,14) = 6.0(16); 0:0:C(16,16) = -10.4(13); 
    0:0:C(18,-18) = -6.5(20); 0:0:C(18,-16) = -0.5(17); 0:0:C(18,-14) = -1.2(18); 
    0:0:C(18,-12) = -5.1(14); 0:0:C(18,-10) = -0.3(18); 0:0:C(18,-8) = 7.6(13); 
    0:0:C(18,-6) = -0.8(20); 0:0:C(18,-4) = -6.7(14); 0:0:C(18,-2) = -7.2(15); 
    0:0:C(18,0) = -9.0(19); 0:0:C(18,2) = 2.3(18); 0:0:C(18,4) = -9.0(17); 
    0:0:C(18,6) = 5.7(20); 0:0:C(18,8) = -5.2(14); 0:0:C(18,10) = -3.1(19); 
    0:0:C(18,12) = -12.3(16); 0:0:C(18,14) = 0.8(17); 0:0:C(18,16) = -5.4(14); 
    0:0:C(18,18) = -17.8(15); 0:0:C(20,-20) = -12.0(18); 0:0:C(20,-18) = 0.8(21); 
    0:0:C(20,-16) = -0.4(16); 0:0:C(20,-14) = -4.4(13); 0:0:C(20,-12) = -12.7(13); 
    0:0:C(20,-10) = -2.6(18); 0:0:C(20,-8) = -0.4(26); 0:0:C(20,-6) = -8.1(15); 
    0:0:C(20,-4) = -1.5(19); 0:0:C(20,-2) = -0.6(15); 0:0:C(20,0) = 1.4(20); 
    0:0:C(20,2) = 0.6(14); 0:0:C(20,4) = -2.3(23); 0:0:C(20,6) = -7.0(16); 
    0:0:C(20,8) = -1.4(20); 0:0:C(20,10) = -4.0(14); 0:0:C(20,12) = -1.6(16); 
    0:0:C(20,14) = 6.6(13); 0:0:C(20,16) = 2.4(15); 0:0:C(20,18) = 11.3(18); 
    0:0:C(20,20) = 8.9(18); 0:0:C(22,-22) = 6.5(25); 0:0:C(22,-20) = 8.2(25); 
    0:0:C(22,-18) = -2.4(19); 0:0:C(22,-16) = -16.8(24); 0:0:C(22,-14) = -17.0(23); 
    0:0:C(22,-12) = -4.3(22); 0:0:C(22,-10) = -15.3(15); 0:0:C(22,-8) = 14.8(23); 
    0:0:C(22,-6) = -5.6(17); 0:0:C(22,-4) = -1.2(25); 0:0:C(22,-2) = 1.4(28); 
    0:0:C(22,0) = 7.6(26); 0:0:C(22,2) = 16.4(26); 0:0:C(22,4) = -2.6(30); 
    0:0:C(22,6) = -1.3(21); 0:0:C(22,8) = -7.1(25); 0:0:C(22,10) = -11.1(17); 
    0:0:C(22,12) = -14.4(23); 0:0:C(22,14) = -0.4(20); 0:0:C(22,16) = 10.4(25); 
    0:0:C(22,18) = -5.4(22); 0:0:C(22,20) = 9.2(29); 0:0:C(22,22) = 7.1(22); 
    0:0:C(24,-24) = -2.8(23); 0:0:C(24,-22) = 2.2(25); 0:0:C(24,-20) = 5.0(19); 
    0:0:C(24,-18) = -2.3(21); 0:0:C(24,-16) = -8.0(16); 0:0:C(24,-14) = 3.0(22); 
    0:0:C(24,-12) = 1.6(23); 0:0:C(24,-10) = 11.3(26); 0:0:C(24,-8) = 2.2(22); 
    0:0:C(24,-6) = 8.4(24); 0:0:C(24,-4) = 2.1(20); 0:0:C(24,-2) = 11.7(27); 
    0:0:C(24,0) = 5.6(22); 0:0:C(24,2) = 7.0(23); 0:0:C(24,4) = 0.6(20); 
    0:0:C(24,6) = 4.3(25); 0:0:C(24,8) = -2.9(26); 0:0:C(24,10) = -10.7(26); 
    0:0:C(24,12) = 7.7(21); 0:0:C(24,14) = -7.9(21); 0:0:C(24,16) = 3.2(20); 
    0:0:C(24,18) = 7.9(21); 0:0:C(24,20) = -4.6(20); 0:0:C(24,22) = -3.0(25); 
    0:0:C(24,24) = 10.1(25); 
;
_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
    64.8(13), -2.000, 0.08(7), 0.65(3), 0.000, 0.03678(14), 
  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        0.01321
_pd_proc_ls_prof_wR_expected     0.01144
_pd_proc_ls_prof_wR_factor       0.01860
_pd_spec_mounting                ' ?'
_refine_ls_goodness_of_fit_all   1.647
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_R_Fsqd_factor         0.84579
_refine_ls_wR_factor_obs         0.01860
_reflns_d_resolution_high        0.891
_reflns_d_resolution_low         6.075
_reflns_limit_h_max              10
_reflns_limit_h_min              10
_reflns_limit_k_max              2
_reflns_limit_k_min              2
_reflns_limit_l_max              -4
_reflns_limit_l_min              -4
_reflns_number_total             850
_cod_data_source_file            d3dt00384a2.cif
_cod_data_source_block           Na2MgFe(CN)6
_cod_original_cell_volume        567.776(28)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7712401
_refine_ls_r_f_factor            0.43511
_gsas_proc_ls_prof_r_b_factor    0.02980
_gsas_proc_ls_prof_wr_b_factor   0.04893