Synthesis and structure of Sr14Zn1+As11 and Eu14Zn1+As11 (x ≤ 0.5). New members of the family of pnictides isotypic with Ca14AlSb11, exhibiting a new type of structural disorder
Baranets, Sviatoslav; Darone, Gregory M.; Bobev, Svilen; Journal of Solid State Chemistry 280 (2019) 120990–; doi:10.1016/j.jssc.2019.120990

data_1561654
_publ_section_title
;
 Synthesis and structure of Sr14Zn1+As11 and Eu14Zn1+As11 (x &#x2264;
 0.5). New members of the family of pnictides isotypic with Ca14AlSb11,
 exhibiting a new type of structural disorder
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              120990
_journal_paper_doi               10.1016/j.jssc.2019.120990
_journal_volume                  280
_journal_year                    2019
_chemical_formula_sum            'As11 La0.7 Sr13.3 Zn'
_chemical_formula_weight         2152.14
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d :2'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_audit_contact_author_name
;
;
_audit_creation_date             2019-08-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.5000(18)
_cell_length_b                   16.5000(18)
_cell_length_c                   22.039(3)
_cell_measurement_reflns_used    870
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.77
_cell_measurement_theta_min      4.94
_cell_volume                     6000.1(12)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      200.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1498
_diffrn_reflns_av_unetI/netI     0.0801
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24947
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.642
_diffrn_reflns_theta_min         2.469
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    37.214
_exptl_absorpt_correction_T_max  0.0983
_exptl_absorpt_correction_T_min  0.0386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1473 before and 0.0652 after correction. The Ratio of minimum to maximum transmission is 0.3927. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    4.765
_exptl_crystal_description       irregular
_exptl_crystal_F_000             7507
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.074
_refine_diff_density_max         1.390
_refine_diff_density_min         -1.543
_refine_diff_density_rms         0.357
_refine_ls_extinction_coef       0.000033(8)
_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   1.032
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         2135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0266P)^2^+135.8006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1469
_reflns_number_total             2135
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2019-120990.cif
_cod_data_source_block           mo_svib1451_0m
_cod_original_cell_volume        6000.2(15)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_original_formula_sum        'As11 La0.70 Sr13.30 Zn'
_cod_database_code               1561654
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.169
_shelx_estimated_absorpt_t_min   0.148
_olex2_refinement_description
;
1. Shared sites
{Sr1, La1}
{Sr2, La2}
{Sr4, La4}
2. Uiso/Uaniso restraints and constraints
Uanis(Sr1) = Uanis(La1)
Uanis(Sr2) = Uanis(La2)
Uanis(Sr4) = Uanis(La4)
3. Others
 Sof(La1)=1-FVAR(1)
 Sof(Sr1)=FVAR(1)
 Sof(La2)=1-FVAR(2)
 Sof(Sr2)=FVAR(2)
 Sof(La4)=1-FVAR(3)
 Sof(Sr4)=FVAR(3)
 Fixed Sof: As4(0.25)
;
_shelx_res_checksum              13921
_shelx_hkl_checksum              60387