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_4002886
_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_sum            'Ce4 Mo2 O11'
_chemical_formula_weight         928.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9065(6)
_cell_length_b                   12.9065(6)
_cell_length_c                   5.6194(5)
_cell_measurement_reflns_used    3120
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.3417
_cell_measurement_theta_min      4.9950
_cell_volume                     936.07(10)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.631 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_molecular_graphics    various
_computing_publication_material  various
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            12017
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.23
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    21.690
_exptl_absorpt_correction_T_max  0.6709
_exptl_absorpt_correction_T_min  0.2203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2014/4 (Bruker, 2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    6.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.718
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.422
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+2.9189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                997
_reflns_number_total             1175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm8b00072_si_001.cif
_cod_data_source_block           Ce4Mo2O11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_Hall     '-P 4bc '
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4002886