Construction of Hydrothermally Stable Beryllium Phosphite Open-Frameworks with High Proton Conductivity
Zhang, Qinghua; Wang, Kangcai; Jin, Yunhe; Jiang, Linhai; Wang, Zhi; CrystEngComm  (2017) –; doi:10.1039/C7CE00948H

data_7228515
_publ_section_title
;
 Construction of Hydrothermally Stable Beryllium Phosphite Open-Frameworks
 with High Proton Conductivity
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00948H
_journal_year                    2017
_chemical_formula_moiety         'Be3 H4 O12 P4, 2(C3 H5 N2)'
_chemical_formula_sum            'C6 H14 Be3 N4 O12 P4'
_chemical_formula_weight         485.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-05-18 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                96.149(3)
_cell_angle_beta                 95.184(3)
_cell_angle_gamma                111.344(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3233(5)
_cell_length_b                   8.4561(6)
_cell_length_c                   13.3101(8)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.65
_cell_volume                     859.02(10)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14302
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.587
_diffrn_reflns_theta_min         1.554
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0485 before and 0.0368 after correction.
The Ratio of minimum to maximum transmission is 0.9124.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3943
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+3.9593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3792
_reflns_number_total             3943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00948h2.cif
_cod_data_source_block           mo_2016313_0m
_cod_database_code               7228515
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H,H) groups, All C(H) groups, All N(H) groups
2. Restrained distances
 P1-H1
 1.3 with sigma of 0.02
3. Restrained planarity
 C4, C5, C6, N3, N4
 with sigma of 0.1
 C1, C2, C3, N1, N2
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C4(H4A), C5(H5), C6(H6), N3(H3B), N4(H4B)
;
_shelx_res_checksum              92673
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'