Evidence of reaction intermediates in microwave-assisted synthesis of SHG active α La(IO3)3 nanocrystals
Regny, Sylvain; Suffren, Yan; Leynaud, Olivier; Gautier-Luneau, Isabelle; Dantelle, Geraldine; CrystEngComm  (2020) –; doi:10.1039/D0CE00156B

data_7240123
_publ_section_title
;
 Evidence of reaction intermediates in microwave-assisted synthesis of SHG
 active \a La(IO3)3 nanocrystals
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00156B
_journal_year                    2020
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'I3 La O10'
_chemical_formula_sum            'I3 La O10'
_chemical_formula_weight         681.61
_chemical_name_common            La(IO3)3.H2O
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.25505/fiz.icsd.cc247bb2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2010-09-06T22:58:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-12-20 deposited with the CCDC.	2020-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.09(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.177(1)
_cell_length_b                   13.260(1)
_cell_length_c                   9.786(1)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.56087
_cell_volume                     916.90(18)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.025
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14449
_diffrn_reflns_theta_full        21.39
_diffrn_reflns_theta_max         21.39
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    7.827
_exptl_absorpt_correction_T_max  0.731
_exptl_absorpt_correction_T_min  0.391
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Coppens, 1970'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0081P)^2^+4.1233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0436
_reflns_number_gt                1875
_reflns_number_total             2096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0ce00156b2.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        916.89(17)
_cod_database_code               7240123