In Situ Neutron Diffraction Studies of the Flux Crystal Growth of the Reduced Molybdates La4Mo2O11 and Ce4Mo2O11: Revealing Unexpected Mixed-Valent Transient Intermediates and Determining the Sequence of Events during Crystal Growth
Abeysinghe, Dileka; Huq, Ashfia; Yeon, Jeongho; Smith, Mark D.; zur Loye, Hans-Conrad; Chemistry of Materials  (2018) –; doi:10.1021/acs.chemmater.8b00072

data_4002887
_publ_section_title
;
 In Situ Neutron Diffraction Studies of the Flux Crystal Growth of the
 Reduced Molybdates La4Mo2O11 and Ce4Mo2O11: Revealing Unexpected
 Mixed-Valent Transient Intermediates and Determining the Sequence of
 Events during Crystal Growth
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.8b00072
_journal_year                    2018
_chemical_formula_moiety         'La5 Mo3 O16'
_chemical_formula_sum            'La5 Mo3 O16'
_chemical_formula_weight         1238.37
_space_group_crystal_system      cubic
_space_group_IT_number           222
_space_group_name_Hall           '-P 4a 2bc 3'
_space_group_name_H-M_alt        'P n -3 n'
_symmetry_space_group_name_Hall  '-P 4a 2bc 3'
_symmetry_space_group_name_H-M   'P n -3 n :2'
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2272(3)
_cell_length_b                   11.2272(3)
_cell_length_c                   11.2272(3)
_cell_measurement_reflns_used    7583
_cell_measurement_temperature    303(2)
_cell_measurement_theta_max      40.209
_cell_measurement_theta_min      2.565
_cell_volume                     1415.19(7)
_computing_cell_refinement       'SAINT Version 8.34a (Bruker, 2014)'
_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT Version 8.34a (Bruker, 2014)'
_computing_molecular_graphics    various
_computing_publication_material  various
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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  0.0594
_diffrn_reflns_av_unetI/netI     0.0102
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49027
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        40.209
_diffrn_reflns_theta_max         40.209
_diffrn_reflns_theta_min         2.566
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    17.388
_exptl_absorpt_correction_T_max  0.1174
_exptl_absorpt_correction_T_min  0.0598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2014/4 (Bruker, 2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.812
_exptl_crystal_description       'cube-shaped block'
_exptl_crystal_F_000             2156
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.484
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       0.00419(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     21
_refine_ls_number_reflns         757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0290P)^2^+2.0514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                539
_reflns_number_total             757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm8b00072_si_001.cif
_cod_data_source_block           da2053b_1
_cod_original_cell_volume        1415.19(11)
_cod_database_code               4002887
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.337
_shelx_estimated_absorpt_t_max   0.477
_shelx_res_checksum              98122
_shelx_hkl_checksum              27705