An arsenicniobate-based 3D framework with selective adsorption and anion-exchange properties
Li, Ning; Liu, Yiwei; Lu, Ying; He, Danfeng; Liu, Shumei; Wang, Xingquan; Li, Yangguang; Liu, Shuxia; New J. Chem. 40 (2016) 2220–; doi:10.1039/C5NJ02163D

data_7055255
_publ_section_title
;
 An arsenicniobate-based 3D framework with selective adsorption and
 anion-exchange properties
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              2220
_journal_paper_doi               10.1039/C5NJ02163D
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'As Nb12 O44 V4, 2(C12 H40 Cu2 N8), 8(O)'
_chemical_formula_sum            'C24 H95 As Cu4 N16 Nb12 O52 V4'
_chemical_formula_weight         3087.91
_chemical_name_systematic        1
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-26
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2015-12-04 deposited with the CCDC.
2015-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   15.295(5)
_cell_length_b                   15.295(5)
_cell_length_c                   19.430(5)
_cell_measurement_reflns_used    12950
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.995
_cell_measurement_theta_min      1.694
_cell_volume                     4545(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_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    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15760
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.296
_diffrn_reflns_theta_min         1.694
_exptl_absorpt_coefficient_mu    3.205
_exptl_absorpt_correction_T_max  0.681
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    2.245
_exptl_crystal_description       block
_exptl_crystal_F_000             2970
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.211
_refine_diff_density_min         -3.121
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2845
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0544
_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^)+(0.1182P)^2^+37.9480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1863
_refine_ls_wR_factor_ref         0.1956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2466
_reflns_number_total             2845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj02163d2.cif
_cod_data_source_block           y
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7055255.cif.
;
_cod_original_cell_volume        4545(3)
_cod_database_code               7055255
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.553
_olex2_refinement_description
;
1. Fixed Uiso
 At 1 times of:
  All C(H,H) groups, {H2,C3,H3A,H3B,H3C} of C2, {H2AC,C3A,H3AA,H3AB,H3AC} of
  C2A, All N(H,H) groups
2. Restrained distances
 N1-C1 = N2-C2
 1.45 with sigma of 0.01
 C1-C2 = C2-C3
 1.51 with sigma of 0.01
 N2-C3 = C1-N2
 2.42 with sigma of 0.02
 C1-C3
 2.46 with sigma of 0.02
 N1A-C1A = N2A-C2A
 1.45 with sigma of 0.01
 C1A-C2A = C2A-C3A
 1.51 with sigma of 0.01
 N2A-C3A = C1A-N2A
 2.42 with sigma of 0.02
 C1A-C3A
 2.46 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C1A \\sim C2A: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(N1A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C1A) \\sim Ueq,
Uanis(C2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) = Uanis(N2A)
Uanis(N2) = Uanis(N1A)
Uanis(C1) = Uanis(C2A)
Uanis(C2) = Uanis(C1A)
4. Rigid body (RIGU) restrains
 O2, Nb2, O5, O4B, O7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: V2(0.25) O4B(0.5) O6(0.25) O7B(0.5) O8(0.5) N1(0.5) H1A(0.5)
 H1B(0.5) N2(0.5) H2A(0.5) H2B(0.5) C1(0.5) H1C(0.5) H1D(0.5) C2(0.5) H2(0.5)
 C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) N1A(0.5) H1AA(0.5) H1AB(0.5) N2A(0.5)
 H2AA(0.5) H2AB(0.5) C1A(0.5) H1AC(0.5) H1AD(0.5) C2A(0.5) H2AC(0.5) C3A(0.5)
 H3AA(0.5) H3AB(0.5) H3AC(0.5) O111(0.25) O113(0.25) O112(0.25) O114(0.25)
 O7A(0.5) O4A(0.5)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C2A(H2AC)
6.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), N1A(H1AA,H1AB), N2A(H2AA,H2AB),
 C1A(H1AC,H1AD)
6.c Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC)
;
_shelx_res_checksum              3962
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'