Crystal structures of hybrid completely reduced phosphomolybdates and catalytic performance applied as molecular catalysts for the reduction of chromium(VI)
Tian, Xuerui; Xin, Xing; Gao, Yuanzhe; Dai, Dandan; Huang, Jinjin; Han, Zhangang; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618013025

data_2021274
_publ_section_title
;
 Crystal structures of hybrid completely reduced phosphomolybdates and
 catalytic performance applied as molecular catalysts for the reduction of
 chromium(VI)
;
_journal_coeditor_code           JR3018
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618013025
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
;
(C13 H16 N2)2 [Na (H2 O) (C2 H5 O)] [Fe (H2 O)2 ] [Ca (H2 O)2]2
{Fe [Mo6 O12 (O H)3 (H2 P O4) (H P O4) (P O4)2]2}, 4H2 O
;
_chemical_formula_moiety
;
2(C13 H16 N2 2+), C2 H7 Na O2, H4 Fe O2 2+, 2(H4 Ca O2 2+),
H12 Fe1 Mo12 O62 P8 10-, 4(H2 O)
;
_chemical_formula_sum            'C28 H70 Ca2 Fe2 Mo12 N4 Na O74 P8'
_chemical_formula_weight         3260.77
_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
_cell_angle_alpha                90
_cell_angle_beta                 95.130(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.317(7)
_cell_length_b                   18.533(6)
_cell_length_c                   22.838(8)
_cell_measurement_reflns_used    9260
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.37
_cell_volume                     8986(5)
_computing_cell_refinement
;
SMART (Bruker, 2008)
;
_computing_data_collection
;
SMART (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         1.756
_exptl_absorpt_coefficient_mu    2.306
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.410
_exptl_crystal_description       block
_exptl_crystal_F_000             6340
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.886
_refine_diff_density_min         -0.733
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         7781
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0626P)^2^+126.1618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                7629
_reflns_number_total             7781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3018sup1.cif
_cod_data_source_block           2
_cod_database_code               2021274
_shelx_hkl_checksum              72448
_shelx_res_checksum              92498
_shelxl_version_number           2.014
_cod_database_fobs_code 2021274