Chain Structures in Alkali Borophosphates: Synthesis and Characterization of K~3~[BP~3~O~9~(OH)~3~] and Rb~3~[B~2~P~3~O~11~(OH)~2~]
Bastian Ewald; Yurii Prots; Prashanth Menezes; Srinivasan Natarajan; Hui Zhang; Rüdiger Kniep; Inorganic Chemistry 44 (2005) 6431–6438; doi:10.1021/ic050441p

data_4309493
_publ_contact_author_address
;
Max-Planck Institut f\"ur Chemische Physik fester Stoffe
N\"othnitzer Str. 40
D-01187 Dresden
Germany
;
_publ_contact_author_email       kniep@cpfs.mpg.de
_publ_contact_author_fax         49(351)46463002
_publ_contact_author_name        'Kniep, R\"udiger'
_publ_contact_author_phone       49(351)46463000
_publ_section_title
;
Chain Structures in Alkali Borophosphates: Synthesis and Characterization of 
K~3~[BP~3~O~9~(OH)~3~] and Rb~3~[B~2~P~3~O~11~(OH)~2~]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6431
_journal_page_last               6438
_journal_paper_doi               10.1021/ic050441p
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'B2 H2 O13 P3 Rb3'
_chemical_formula_weight         580.96
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2005-04-24T09:00:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.88(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.816(2)
_cell_length_b                   6.673(2)
_cell_length_c                   24.248(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1263.1(6)
_computing_cell_refinement       'CSD (Akselrud, 1993)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295.1500
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
scan:
    Number of images: 400
               Slice: -40.0000 - 200.0000
         Image width: 0.6000
            Exp time: 30.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 41.9000
              2theta: -20.0000
scan:
    Number of images: 100
               Slice: -35.0000 - 25.0000
         Image width: 0.6000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: -90.0000
                 Phi: 85.0000
                 XTD: 41.9000
              2theta: -20.0000
;
_diffrn_measurement_device       'Rigaku AFC7'
_diffrn_measurement_method       oscillation
_diffrn_radiation_detector       'Mercury CCD'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            12734
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        30
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         2.61
_diffrn_source_current           40.0000
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    12.024
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4668
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.06
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.854
_refine_ls_extinction_coef       0.00189(18)
_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   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_gt           0.029
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+2.0853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.060
_reflns_number_gt                3021
_reflns_number_total             3523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050441psi20050629_071055_2.cif
_cod_data_source_block           BE_H045a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1263.0(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'H2 B2 O13 P3 Rb3'
_cod_database_code               4309493