An organic–inorganic hybrid supramolecular framework material based on a [P2W18O62]6−cluster and Yb & Na complexes of pyridine-2,6-dicarboxylic acid: a catalyst for selective oxidation of sulfides in water with H2O2
Reddy, Pulikanti Guruprasad; Mamidi, Narsimha; Pradeep, Chullikkattil P.; CrystEngComm 18 (2016) 4272–; doi:10.1039/C5CE02546J

data_7224542
_publ_section_title
;
 An organic--inorganic hybrid supramolecular framework material based on a
 [P2W18O62]6&#x2212;cluster and Yb &amp; Na complexes of
 pyridine-2,6-dicarboxylic acid: a catalyst for selective oxidation of
 sulfides in water with H2O2
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              4272
_journal_paper_doi               10.1039/C5CE02546J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C56 H80 N8 Na4 O116 P2 W18 Yb2'
_chemical_formula_sum            'C56 H80 N8 Na4 O116 P2 W18 Yb2'
_chemical_formula_weight         6530.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-12-24 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.071(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2405(16)
_cell_length_b                   35.036(2)
_cell_length_c                   22.8447(14)
_cell_measurement_reflns_used    5329
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.9200
_cell_measurement_theta_min      2.3550
_cell_volume                     14327.8(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014) and OlEX2'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0903
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            23691
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.401
_diffrn_reflns_theta_min         1.817
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    15.827
_exptl_absorpt_correction_T_max  0.292
_exptl_absorpt_correction_T_min  0.016
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    3.027
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11784
_exptl_crystal_size_max          0.4668
_exptl_crystal_size_mid          0.0692
_exptl_crystal_size_min          0.0437
_refine_diff_density_max         7.785
_refine_diff_density_min         -4.047
_refine_diff_density_rms         0.657
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     864
_refine_ls_number_reflns         15635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0849
_refine_ls_shift/su_max          0.197
_refine_ls_shift/su_mean         0.065
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1626P)^2^+1120.9960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2288
_refine_ls_wR_factor_ref         0.2872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10879
_reflns_number_total             15635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02546j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
         Adding full bibliography for 7224542.cif.

2024-03-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C28 H40 N4 Na2 O58 P W9 Yb'
_cod_original_formula_weight         3265.28
_cod_original_formula_moiety         'C28 H40 N4 Na2 O58 P W9 Yb'
_cod_original_formula_units_Z            8
_cod_original_cell_volume        14327.7(18)
_cod_database_code               7224542
_shelxl_version_number           2014-3
_shelx_res_checksum              59840