A novel silver(i)-Keggin-polyoxometalate inorganic‒organic hybrid: a Lewis acid catalyst for cyanosilylation reaction
Hu, Tuo-Ping; Zhao, Ya-Qin; Mei, Kai; Lin, Shu-Jie; Wang, Xing-Po; Sun, Di; CrystEngComm 17 (2015) 5947–; doi:10.1039/C5CE00953G

data_7220884
_publ_section_title
;
 A novel silver(i)-Keggin-polyoxometalate inorganic--organic hybrid: a
 Lewis acid catalyst for cyanosilylation reaction
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              5947
_journal_paper_doi               10.1039/C5CE00953G
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C8 H10 Ag2 N6, C8 H10 Ag2 N6 O40 Si W12'
_chemical_formula_sum            'C16 H20 Ag4 N12 O40 Si W12'
_chemical_formula_weight         3686.21
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-03-21
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.06 svn.r2239, GUI svn.r4109)
;
_audit_update_record
;
2015-04-15 deposited with the CCDC.
2015-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.066(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.476(4)
_cell_length_b                   12.003(4)
_cell_length_c                   17.582(5)
_cell_measurement_reflns_used    5866
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.36
_cell_volume                     2626.3(14)
_computing_data_reduction        'SAINT v7.23A (Bruker, 2003)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.995
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_laue_measured_fraction_full 0.969
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11357
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.697
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    27.740
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.661
_exptl_crystal_description       block
_exptl_crystal_F_000             3220
_refine_diff_density_max         4.725
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.535
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         7563
_refine_ls_number_restraints     206
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1083P)^2^+39.2858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1487
_reflns_Friedel_coverage         0.997
_reflns_friedel_fraction_full    0.969
_reflns_friedel_fraction_max     0.995
_reflns_number_gt                7232
_reflns_number_total             7563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00953g2.cif
_cod_data_source_block           p
_cod_depositor_comments          'Adding full bibliography for 7220884.cif.'
_cod_original_cell_volume        2626.4(13)
_cod_database_code               7220884
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
N2 \\sim C1 \\sim N1 \\sim N3 \\sim C2 \\sim C3 \\sim C4 \\sim N5 \\sim C5
\\sim N6 \\sim C6 \\sim C8 \\sim N4 \\sim C7: within 1.7A with sigma of 0.005
and sigma for terminal atoms of 0.08
N9 \\sim C9 \\sim N7 \\sim C12 \\sim C10 \\sim N8 \\sim C11 \\sim N10 \\sim C14
\\sim C15 \\sim N12 \\sim C16 \\sim N11 \\sim C13: within 1.7A with sigma of
0.005 and sigma for terminal atoms of 0.08
O7 \\sim O12 \\sim O17 \\sim O19: within 1.7A with sigma of 0.005 and sigma for
terminal atoms of 0.08
W1A \\sim W1 \\sim W7A \\sim W7: within 1.7A with sigma of 0.005 and sigma for
terminal atoms of 0.08
W2 \\sim W2A: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.08
W9A \\sim W9: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.08
Uanis(O19) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.2
: with sigma of 0.0005 and sigma for terminal atoms of 0.2
3. Others
 Fixed Sof: W1(0.9) W2(0.5) W7(0.95) W9(0.9) W1A(0.1) W7A(0.05) W2A(0.5)
 W9A(0.1)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16)
4.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N5(H5A,H5B), N9(H9A,H9B), N11(H11A,H11B)
;
_shelx_res_checksum              30251
_shelxl_version_number           2013-4