Systematic study of cr(3+) substitution into octahedra-based microporous aluminoborates.
Li, Qiaoqi; Lin, Cong; Zhou, Zhengyang; Ju, Jing; Li, Guobao; Lin, Jianhua; Gao, Wenliang; Cong, Rihong; Yang, Tao; Inorganic chemistry 53 (2014) 5600–5608; doi:10.1021/ic500352g

data_4338473
_publ_section_title
;
 Systematic study of cr(3+) substitution into octahedra-based microporous
 aluminoborates.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5600
_journal_page_last               5608
_journal_paper_doi               10.1021/ic500352g
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'Al27 H45 B54 O144, 5.76(B0.52 H1.56 O1.56)'
_chemical_formula_sum            'Al27 B57 H54 O153'
_chemical_formula_weight         3847.06
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2014-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   22.031(3)
_cell_length_b                   22.031(3)
_cell_length_c                   7.0266(14)
_cell_measurement_temperature    293(2)
_cell_volume                     2953.5(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9516
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         33.440
_diffrn_reflns_theta_min         3.089
_exptl_absorpt_coefficient_mu    0.392
_exptl_crystal_density_diffrn    2.163
_exptl_crystal_F_000             1914
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Flack x determined using 1952 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.35(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4797
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+2.8058P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.904
_reflns_number_gt                4436
_reflns_number_total             4797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500352g_si_002.cif
_cod_data_source_block           9
_cod_depositor_comments          'Adding full bibliography for 4338473.cif.'
_cod_original_cell_volume        2953.7(10)
_cod_original_sg_symbol_H-M      R3
_cod_original_formula_sum        'H54 Al27 B57 O153'
_cod_database_code               4338473
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2. Others
 U11(O17)=U11(B7)=U11(O18)=U11(B8)=FVAR(1)
 U22(O17)=U22(B7)=U22(O18)=U22(B8)=FVAR(2)
 U33(O17)=U33(B7)=U33(O18)=U33(B8)=FVAR(3)
 U23(O17)=U23(B7)=U23(O18)=U23(B8)=FVAR(4)
 U13(O17)=U13(B7)=U13(O18)=U13(B8)=FVAR(5)
 U12(O17)=U12(B7)=U12(O18)=U12(B8)=FVAR(6)
 Fixed Sof: O17(0.52) H17(0.52) B7(0.1736) O18(0.48) H18(0.48) B8(0.1598)
3.a Everything fixed:
 H11, H12, H13, H14, H15, H17, H18
;
_shelx_res_checksum              89577
_shelx_hkl_checksum              49373