Synthesis and structures of sodium containing K2-xNaxMg2(SO4)3 langbeinite phases
Trussov, I.A.; Driscoll, L.L.; Male, L.L.; Sanjuan, M.L.; Orera, A.; Slater, P.R.; Journal of Solid State Chemistry 276 (2019) 37–46; doi:10.1016/j.jssc.2019.04.036

data_1563787
_publ_section_title
;
 Synthesis and structures of sodium containing K2-xNaxMg2(SO4)3
 langbeinite phases
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              37
_journal_page_last               46
_journal_paper_doi               10.1016/j.jssc.2019.04.036
_journal_volume                  276
_journal_year                    2019
_chemical_formula_moiety         '0.0277778(K3.77 Mg72 Na68.23 O432 S108)'
_chemical_formula_sum            'K0.1 Mg2 Na1.9 O12 S3'
_chemical_formula_weight         384.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            36
_cell_length_a                   9.56550(10)
_cell_length_b                   28.3065(3)
_cell_length_c                   30.0116(3)
_cell_measurement_reflns_used    35111
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.6450
_cell_measurement_theta_min      4.6490
_cell_volume                     8126.12(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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      100(2)
_diffrn_detector_area_resol_mean 5.1768
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -96.00  -2.00   1.00    3.63    --  -42.02 125.00 -30.00   94
  2  \w    -67.00  32.00   1.00    3.63    --  -42.02  38.00 150.00   99
  3  \w    -67.00  32.00   1.00    3.63    --  -42.02  38.00   0.00   99
  4  \w     23.00 109.00   1.00   14.53    --  105.92 -94.00   0.00   86
  5  \w     33.00 121.00   1.00   14.53    --  105.92-125.00 150.00   88
  6  \w     78.00 178.00   1.00   14.53    --  105.92  30.00 120.00  100
  7  \w     23.00 109.00   1.00   14.53    --  105.92 -94.00  90.00   86
  8  \w     73.00 178.00   1.00   14.53    --  105.92  77.00 150.00  105
  9  \w     24.00 159.00   1.00   14.53    --  105.92 -15.00 -60.00  135
 10  \w   -118.00  -9.00   1.00    3.63    --  -42.02 -77.00 120.00  109
 11  \w   -116.00 -17.00   1.00    3.63    --  -42.02 -38.00   0.00   99
 12  \w   -114.00 -14.00   1.00    3.63    --  -42.02 -57.00-150.00  100
 13  \w     94.00 178.00   1.00   14.53    --  105.92 125.00  30.00   84
 14  \w     73.00 178.00   1.00   14.53    --  105.92  77.00 -60.00  105
 15  \w     77.00 109.00   1.00   14.53    --  105.92  61.00  60.00   32
 16  \w     77.00 178.00   1.00   14.53    --  105.92  61.00   0.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            77038
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.933
_diffrn_reflns_theta_min         3.453
_exptl_absorpt_coefficient_mu    11.041
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.828
_exptl_crystal_description       block
_exptl_crystal_F_000             6870
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 6517 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1589
_refine_ls_number_reflns         16241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+3.9710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                15394
_reflns_number_total             16241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2010-276-37.cif
_cod_data_source_block           k01na19mg2(so4)3
_cod_original_formula_sum        'K0.10 Mg2 Na1.90 O12 S3'
_cod_database_code               1563787
_olex2_refinement_description
;
1. Shared sites
{K1, Na1}
{Na2, K2}
{Na4, K4}
{Na6, K6}
{Na9, K9}
{Na12, K12}
{K13, Na13}
{K15, Na15}
{Na18, K18}
2. Uiso/Uaniso restraints and constraints
Uanis(K1) = Uanis(Na1)
Uanis(Na2) = Uanis(K2)
Uanis(Na4) = Uanis(K4)
Uanis(Na6) = Uanis(K6)
Uanis(Na9) = Uanis(K9)
Uanis(Na12) = Uanis(K12)
Uanis(K13) = Uanis(Na13)
Uanis(K15) = Uanis(Na15)
Uanis(Na18) = Uanis(K18)
Uanis(O108) = Uanis(O105)
Uanis(O109) = Uanis(O106)
Uanis(O103) = Uanis(O110)
Uanis(O111) = Uanis(O11)
Uanis(O10) = Uanis(O112)
Uanis(O113) = Uanis(O7)
Uanis(O104) = Uanis(O114)
Uanis(O13) = Uanis(O115)
Uanis(O116) = Uanis(O117)
Uanis(O2) = Uanis(O119)
Uanis(O118) = Uanis(O1)
3. Others
 Sof(Na1)=1-FVAR(1)
 Sof(K1)=FVAR(1)
 Sof(Na2)=1-FVAR(2)
 Sof(K2)=FVAR(2)
 Sof(Na4)=1-FVAR(3)
 Sof(K4)=FVAR(3)
 Sof(Na6)=1-FVAR(4)
 Sof(K6)=FVAR(4)
 Sof(Na9)=1-FVAR(5)
 Sof(K9)=FVAR(5)
 Sof(Na12)=1-FVAR(6)
 Sof(K12)=FVAR(6)
 Sof(Na13)=1-FVAR(7)
 Sof(K13)=FVAR(7)
 Sof(Na15)=1-FVAR(8)
 Sof(K15)=FVAR(8)
 Sof(Na18)=1-FVAR(9)
 Sof(K18)=FVAR(9)
 Sof(O108)=Sof(O109)=Sof(O110)=1-FVAR(10)
 Sof(O103)=Sof(O105)=Sof(O106)=FVAR(10)
 Sof(O111)=Sof(O112)=Sof(O113)=1-FVAR(11)
 Sof(O7)=Sof(O10)=Sof(O11)=FVAR(11)
 Sof(O114)=1-FVAR(12)
 Sof(O104)=FVAR(12)
 Sof(O115)=1-FVAR(13)
 Sof(O13)=FVAR(13)
 Sof(O117)=1-FVAR(14)
 Sof(O116)=FVAR(14)
 Sof(O119)=1-FVAR(15)
 Sof(O2)=FVAR(15)
 Sof(O118)=1-FVAR(16)
 Sof(O1)=FVAR(16)
;
_shelx_res_checksum              31628
_shelx_hkl_checksum              65675