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_7047666
_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         'Mo6 Na2 O38 P4 Sr, C13 H16 N2, H2 O'
_chemical_formula_sum            'C13 H17 Mo6 N2 Na2 O39 P4 Sr'
_chemical_formula_weight         1658.40
_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                69.457(3)
_cell_angle_beta                 72.168(4)
_cell_angle_gamma                69.964(4)
_cell_formula_units_Z            2
_cell_length_a                   13.4222(6)
_cell_length_b                   13.8149(5)
_cell_length_c                   14.9831(6)
_cell_measurement_reflns_used    7870
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2957
_cell_measurement_theta_min      2.9184
_cell_volume                     2388.88(18)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -81.00   18.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.8190  -77.0000 -180.0000 99

  2 omega  -40.00   49.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.8190   57.0000  -30.0000 89

  3 omega  -44.00   51.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.8190   77.0000   60.0000 95
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0482545000
_diffrn_orient_matrix_UB_12      -0.0092678000
_diffrn_orient_matrix_UB_13      0.0154009000
_diffrn_orient_matrix_UB_21      0.0211355000
_diffrn_orient_matrix_UB_22      0.0313257000
_diffrn_orient_matrix_UB_23      -0.0463882000
_diffrn_orient_matrix_UB_31      -0.0231709000
_diffrn_orient_matrix_UB_32      0.0465187000
_diffrn_orient_matrix_UB_33      0.0169217000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15295
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.924
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81256
_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_density_diffrn    2.306
_exptl_crystal_description       block
_exptl_crystal_F_000             1586
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.740
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         8378
_refine_ls_number_restraints     1047
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0548P)^2^+10.8608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7107
_reflns_number_total             8378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03250e2.cif
_cod_data_source_block           compound-2
_cod_depositor_comments
;

2024-03-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C26 H34 Mo12 N4 Na4 O78 P8 Sr2'
_cod_original_formula_weight         3316.81
_cod_original_formula_moiety     'Mo12 Na4 O76 P8 Sr2, 2(C13 H16 N2), 2(H2 O)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        2388.88(19)
_cod_database_code               7047666
_shelx_shelxl_version_number     2018/1
_exptl_absorpt_special_details   block
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C12-N2 = N2-C11
 1.45 with sigma of 0.02
 Na4-O7W
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.03
N1 \\sim N2: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17
\\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25
\\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O31 \\sim O2AA \\sim
O2W \\sim O3AA \\sim O1AA \\sim O8W \\sim O1W \\sim O4W \\sim O3W \\sim O7W:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03
Na1 \\sim O5 \\sim O1 \\sim O2: within 5A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O1W(0.5) Na4(0.5) O7W(0.5)
5.a Free rotating group:
 O3W(H3WA,H3WB)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13), N2(H2A)
;
_shelx_res_checksum              30971
_shelx_fab_checksum              22890
_olex2_submission_special_instructions 'No special instructions were received'