From NaZn4Sb3 to HT-Na1‒xZn4‒ySb3: Panoramic Hydride Synthesis, Structural Diversity, and Thermoelectric Properties
Gvozdetskyi, Volodymyr; Owens-Baird, Bryan; Hong, Sangki; Cox, Tori; Bhaskar, Gourab; Harmer, Colin; Sun, Yang; Zhang, Feng; Wang, Cai-Zhuang; Ho, Kai-Ming; Zaikina, Julia V.; Chemistry of Materials  (2019) –; doi:10.1021/acs.chemmater.9b02239

data_4002930
_publ_section_title
;
 From NaZn4Sb3 to HT-Na1--xZn4--ySb3: Panoramic Hydride Synthesis,
 Structural Diversity, and Thermoelectric Properties
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.9b02239
_journal_year                    2019
_chemical_formula_moiety         'Na1-x, Zn4-ySb3'
_chemical_formula_sum            'Na1.27 Sb4 Zn5.15'
_chemical_formula_weight         853.10
_chemical_name_common            'sodium zinc zntimonide'
_chemical_name_systematic        'sodium zinc zntimonide'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90.402(5)
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   19.508(3)
_cell_length_b                   14.708(3)
_cell_length_c                   20.736(4)
_cell_measurement_reflns_used    104502
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.749
_cell_measurement_theta_min      2.301
_cell_volume                     5949.5(19)
_computing_cell_refinement       'SAINT (8.34a) (Bruker, 2013)'
_computing_data_collection       'Apex3 (2016.9) (Bruker, 2016)'
_computing_data_reduction        'SAINT (8.34a) (Bruker, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker Photon100 CMOS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            104502
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.749
_diffrn_reflns_theta_min         2.301
_diffrn_source                   Micro-source
_exptl_absorpt_coefficient_mu    22.924
_exptl_absorpt_correction_T_max  0.0485
_exptl_absorpt_correction_T_min  0.0178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            'metallic silver'
_exptl_crystal_density_diffrn    5.714
_exptl_crystal_description       block
_exptl_crystal_F_000             8942
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_transmission_factor_max   0.0485
_exptl_transmission_factor_min   0.0178
_refine_diff_density_max         2.987
_refine_diff_density_min         -1.753
_refine_diff_density_rms         0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         15401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+185.1393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13212
_reflns_number_total             15401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b02239_si_002.cif
_cod_data_source_block           HTNa1-xZn4-ySb3
_cod_original_cell_volume        5949.6(19)
_cod_database_code               4002930
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.039
_shelx_estimated_absorpt_t_max   0.091
_shelx_res_checksum              99141
_shelx_hkl_checksum              80675