Low-temperature-flux syntheses of ultraviolet-transparent borophosphates Na <sub>4</sub> MB <sub>2</sub> P <sub>3</sub> O <sub>13</sub> (M = Rb, Cs) exhibiting a second-harmonic generation response
Wu, Chao; Li, Longhua; Yang, Gang; Song, Junling; Yan, Bing; Humphrey, Mark G.; Zhang, Long; Shao, Jianda; Zhang, Chi; Dalton Transactions 46 (2017) 12605–12611; doi:10.1039/C7DT02649H

data_1546882
_publ_section_title
;
 Low-temperature-flux syntheses of ultraviolet-transparent borophosphates
 Na <sub>4</sub> MB <sub>2</sub> P <sub>3</sub> O <sub>13</sub> (M = Rb,
 Cs) exhibiting a second-harmonic generation response
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              12605
_journal_page_last               12611
_journal_paper_doi               10.1039/C7DT02649H
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'B2 Cs Na4 O13 P3'
_chemical_formula_weight         547.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-07-20 deposited with the CCDC.
2017-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.5034(9)
_cell_length_b                   6.7673(2)
_cell_length_c                   14.7803(5)
_cell_measurement_reflns_used    8301
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0836
_cell_measurement_theta_min      3.0102
_cell_volume                     2450.90(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  bruker-CCD
_diffrn_measurement_method       'w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14138
_diffrn_reflns_theta_full        27.08
_diffrn_reflns_theta_max         27.08
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    3.626
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.967
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         4997
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+3.1907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                4568
_reflns_number_total             4997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt02649h2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               1546882