Facile in-situ reduction: Crystal growth and magnetic studies of reduced vanadium (III/IV) silicates CaxLn1−xVSiO5 (Ln = Ce‒Nd, Sm‒Lu, Y)
Abeysinghe, Dileka; Smith, Mark D.; Morrison, Gregory; Yeon, Jeongho; zur Loye, Hans-Conrad; Journal of Solid State Chemistry 260 (2018) 80–86; doi:10.1016/j.jssc.2018.01.004

data_1561158
_publ_section_title
;
 Facile in-situ reduction: Crystal growth and magnetic studies of reduced
 vanadium (III/IV) silicates CaxLn1&#x2212;xVSiO5 (Ln = Ce--Nd, Sm--Lu, Y)
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              80
_journal_page_last               86
_journal_paper_doi               10.1016/j.jssc.2018.01.004
_journal_volume                  260
_journal_year                    2018
_chemical_formula_moiety         'Ca0.72 Gd0.28 O5 Si V'
_chemical_formula_sum            'Ca0.72 Gd0.28 O5 Si V'
_chemical_formula_weight         232.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   .
_cell_angle_alpha                90
_cell_angle_beta                 112.9615(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5371(3)
_cell_length_b                   8.7503(4)
_cell_length_c                   6.9234(4)
_cell_measurement_reflns_used    3659
_cell_measurement_temperature    303(2)
_cell_measurement_theta_max      35.049
_cell_measurement_theta_min      3.196
_cell_volume                     364.65(3)
_computing_cell_refinement       'SAINT Version 8.37a (Bruker, 2014)'
_computing_data_collection       'Bruker APEX3 v2016.5-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT Version 8.37a (Bruker, 2014)'
_computing_molecular_graphics    various
_computing_publication_material  various
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      303(2)
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5720
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        35.049
_diffrn_reflns_theta_max         35.049
_diffrn_reflns_theta_min         4.109
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.985
_exptl_absorpt_correction_T_max  0.1078
_exptl_absorpt_correction_T_min  0.0624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2016/2 (Bruker, 2016)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.228
_exptl_crystal_description       irregular
_exptl_crystal_F_000             438
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       0.0055(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0052P)^2^+2.7810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                688
_reflns_number_total             808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            6.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1561158
_shelx_estimated_absorpt_t_min   0.615
_shelx_estimated_absorpt_t_max   0.715
_shelx_res_checksum              14181
_shelx_hkl_checksum              96970