Novel fully reduced phosphomolybdates for highly efficient removal of inorganic hexavalent chromium and organic dye methylene blue
Tian, Xuerui; Hou, Lin; Wang, Jiaojiao; Xin, Xing; Zhang, Heng; Ma, Yuan-Yuan; Wang, Yali; Zhang, Lina; Han, Zhangang; Dalton Transactions  (2018) –; doi:10.1039/C8DT03250E

data_7047667
_publ_section_title
;
 Novel fully reduced phosphomolybdates for highly efficient removal of
 inorganic hexavalent chromium and organic dye methylene blue
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT03250E
_journal_year                    2018
_chemical_formula_moiety
'0.5(Ca4 Mo48 Na8 O272 P32), 4(C13 H16 N2), 1[C13H18N2], 4[H2O]'
_chemical_formula_sum            'C52 H64 Ca2 Mo24 N8 Na4 O132 P16'
_chemical_formula_weight         5883.31
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d'
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-09-19
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2018.08.29 svn.r3523 for OlexSys, GUI svn.r5535)
;
_audit_update_record
;
2018-09-25 deposited with the CCDC.
2018-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.7770(4)
_cell_length_b                   31.7770(4)
_cell_length_c                   36.0323(8)
_cell_measurement_reflns_used    14907
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2268
_cell_measurement_theta_min      2.8609
_cell_volume                     36384.6(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.2375
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -15.00   72.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9908   57.0000 -120.0000 87
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33861
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.867
_exptl_absorpt_coefficient_mu    1.906
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.148
_exptl_crystal_description       block
_exptl_crystal_F_000             22560
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.253
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         7994
_refine_ls_number_restraints     1327
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+1449.6490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6522
_reflns_number_total             7994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03250e2.cif
_cod_data_source_block           compound-3
_cod_original_cell_volume        36384.6(12)
_cod_database_code               7047667
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C1-C2_$1
 1.65 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C2 \\sim C1 \\sim C3 \\sim C7 \\sim C4 \\sim C5 \\sim C6 \\sim C10 \\sim C11
\\sim C12 \\sim C9 \\sim C8 \\sim C14 \\sim C13: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.02
N1 \\sim N2: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
O5 \\sim O24 \\sim O23 \\sim O28 \\sim O22 \\sim O20 \\sim O8 \\sim O3 \\sim O1
\\sim O10 \\sim O9 \\sim O12 \\sim O18 \\sim O29 \\sim O21 \\sim O13 \\sim O11
\\sim O2 \\sim O6 \\sim O25 \\sim O30 \\sim O17 \\sim O16 \\sim O26 \\sim O31
\\sim O4 \\sim O7 \\sim O33 \\sim O14 \\sim O32 \\sim O15 \\sim O27 \\sim O19
\\sim O35 \\sim O34 \\sim O37 \\sim O36 \\sim O40 \\sim O38 \\sim O39 \\sim O41
\\sim O0AA: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03
Uanis(O14) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(P4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O34) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: P1(0.75) O13(0.75) O16(0.75) O26(0.75) O31(0.75) O33(0.75)
 O14(0.75) H1A(0.5) H1B(0.5) H14A(0.5) H14B(0.5) P4(0.75) O32(0.75) O15(0.75)
 P6(0.25) O35(0.25) O34(0.25) O37(0.25) O36(0.25) P5(0.25) O40(0.25) O38(0.25)
 O39(0.25) O41(0.25) Na2(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C14(H14A,H14B), C13(H13A,H13B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C4(H4), N1(H1), C5(H5), C6(H6), C11(H11), N2(H2), C12(H12), C9(H9),
 C8(H8)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1276 electrons were 
found in a volume of 6448\%A^3 in 1 void. 
This is consistent with the presence of 
1[C13H18N2], 4[H2O] per formula unit 
which account for 1200.0 electrons.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              34086
_shelx_fab_checksum              9296
_olex2_submission_special_instructions 'No special instructions were received'