Boronic Acid Flux Synthesis and Crystal Growth of Uranium and Neptunium Boronates and Borates: A Low-Temperature Route to the First Neptunium(V) Borate
Shuao Wang; Evgeny V. Alekseev; Hannah M. Miller; Wulf Depmeier; Thomas E. Albrecht-Schmitt; Inorganic Chemistry 49 (2010) 9755–9757; doi:10.1021/ic101678d

data_4317002
_publ_section_title
;
 Boronic Acid Flux Synthesis and Crystal Growth of Uranium and Neptunium
 Boronates and Borates: A Low-Temperature Route to the First Neptunium(V)
 Borate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9755
_journal_page_last               9757
_journal_paper_doi               10.1021/ic101678d
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'NpO2 [B3O4(OH)2]'
_chemical_formula_sum            'B3 Np O8'
_chemical_formula_weight         397.43
_chemical_melting_point          ?
_chemical_name_common            'Neptunium (V) borate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   none
_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                   11.872(11)
_cell_length_b                   9.196(9)
_cell_length_c                   5.620(5)
_cell_measurement_reflns_used    1161
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      2.21
_cell_volume                     613.6(10)
_computing_cell_refinement       'smart saint'
_computing_data_collection       smart
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER apex II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_source         'Imus microfocused'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1414
_diffrn_reflns_av_sigmaI/netI    0.1175
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5736
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    16.937
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELTXPREP
_exptl_crystal_colour            light-green
_exptl_crystal_density_diffrn    4.302
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.059
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.008
_refine_diff_density_max         4.156
_refine_diff_density_min         -3.183
_refine_diff_density_rms         0.465
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(10)
_refine_ls_extinction_coef       0.0039(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         1161
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0379P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                849
_reflns_number_total             1161
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101678d_si_001_1.cif
_cod_data_source_block           Np(V)BO
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'N/a' was changed to '?' - the value
is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4317002