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_7047665
_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
'K0.1 Mo6 Na0.9 O31.25 P4, 3(C2 H10 N2), 0.5(H2 O), 0.7(H O), 0.8(O)'
_chemical_formula_sum            'C6 H29.5 K0.1 Mo6 N6 Na0.9 O33.25 P4'
_chemical_formula_weight         1441.97
_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
_audit_creation_date             2018-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-17 deposited with the CCDC.
2018-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                80.601(4)
_cell_angle_beta                 82.922(3)
_cell_angle_gamma                76.161(3)
_cell_formula_units_Z            4
_cell_length_a                   12.138(3)
_cell_length_b                   14.763(4)
_cell_length_c                   21.449(6)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.56
_cell_volume                     3667.6(17)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker SMART'
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1378
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17005
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.735
_exptl_absorpt_coefficient_mu    2.305
_exptl_absorpt_correction_T_max  0.777
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.612
_exptl_crystal_description       block
_exptl_crystal_F_000             2789
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.568
_refine_diff_density_min         -2.373
_refine_diff_density_rms         0.307
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         12505
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0969P)^2^+46.0413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11184
_reflns_number_total             12505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03250e2.cif
_cod_data_source_block           wxx_144_0m
_cod_depositor_comments
;

2024-03-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         5767.90
_cod_original_formula_moiety
'K0.4 Mo24 Na3.6 O125 P16, 12(C2 H10 N2), 2(H2 O), 2.8(H O), 3.2(O)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        3667.4(16)
_cod_original_formula_sum        'C24 H118 K0.40 Mo24 N24 Na3.60 O133 P16'
_cod_database_code               7047665
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.695
_shelx_estimated_absorpt_t_min   0.669
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, {H2C,H2D,H2E} of N2, {H9A,H9B,H9C} of N9, {H10A,H10B,
  H10C} of N10, {H5C,H5D,H5E} of N5
 At 1.5 times of:
  All O(H) groups, {H1C,H1D,H1E} of N1, {H3C,H3D,H3E} of N3, {H8C,H8D,H8E} of
  N8, {H7C,H7D,H7E} of N7, {H12C,H12D,H12E} of N12, {H11C,H11D,H11E} of N11,
  {H4C,H4D,H4E} of N4, {H6C,H6D,H6E} of N6, All O(H,H) groups
2. Shared sites
{K1, Na3}
3. Restrained distances
 C2-N2
 1.55 with sigma of 0.02
 N6-C6
 1.5 with sigma of 0.02
 N10-C10
 1.55 with sigma of 0.02
 C10-C9
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Na1 \\sim O3 \\sim O4 \\sim O1: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C11
\\sim C12 \\sim C9 \\sim C10: within 3.5A with sigma of 0.01 and sigma for
terminal atoms of 0.03
N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8 \\sim N11
\\sim N12 \\sim N9 \\sim N10: within 3.5A with sigma of 0.01 and sigma for
terminal atoms of 0.03
Uanis(C8) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(O6)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O41) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C10) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(O36) = Uanis(O47)
Uanis(O8) = Uanis(O9)
Uanis(K1) = Uanis(Na3)
5. Others
 Fixed Sof: Na3(0.8) O3W(0.6) O3WA(0.4) O4W(0.5) O5W(0.6) O6W(0.4) H6W(0.4)
 K1(0.2)
6.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2W), O6W(H6W)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C9(H9D,H9E),
 C10(H10D,H10E)
6.c Idealised Me refined as rotating group:
 N1(H1C,H1D,H1E), N2(H2C,H2D,H2E), N3(H3C,H3D,H3E), N4(H4C,H4D,H4E), N5(H5C,
 H5D,H5E), N6(H6C,H6D,H6E), N7(H7C,H7D,H7E), N8(H8C,H8D,H8E), N11(H11C,H11D,
 H11E), N12(H12C,H12D,H12E), N9(H9A,H9B,H9C), N10(H10A,H10B,H10C)
;
_shelx_res_checksum              55548
_olex2_submission_special_instructions 'No special instructions were received'