Polyoxovanadate catalysts for oxidation of 1-phenyl ethanol: from the discrete [V4O12]4− and [V10O28]6− anions to the anionic [V6O17]n4n− coordination polymer
Wang, Ke; Xu, Qiaofei; Ma, Pengtao; Zhang, Chao; Wang, Jingping; Niu, Jingyang; CrystEngComm 20 (2018) 6273–; doi:10.1039/C8CE01237G

data_7231510
_publ_section_title
;
 Polyoxovanadate catalysts for oxidation of 1-phenyl ethanol: from the
 discrete [V4O12]4&#x2212; and [V10O28]6&#x2212; anions to the anionic
 [V6O17]n4n&#x2212; coordination polymer
;
_journal_issue                   40
_journal_name_full               CrystEngComm
_journal_page_first              6273
_journal_paper_doi               10.1039/C8CE01237G
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         '2(C36 H24 N6 Ru), O12 V4, 26(O)'
_chemical_formula_sum            'C72 H100 N12 O38 Ru2 V4'
_chemical_formula_weight         2147.53
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2018-04-17 deposited with the CCDC.
2018-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                98.3390(10)
_cell_angle_beta                 105.4250(10)
_cell_angle_gamma                104.4740(10)
_cell_formula_units_Z            1
_cell_length_a                   12.1515(10)
_cell_length_b                   13.1137(11)
_cell_length_c                   16.5899(14)
_cell_measurement_reflns_used    8322
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.54
_cell_volume                     2403.3(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0152
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12269
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         1.824
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0579 before and 0.0325 after correction.
The Ratio of minimum to maximum transmission is 0.8403.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.616
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.149
_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     272
_refine_ls_number_reflns         8497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1208P)^2^+10.7403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2037
_refine_ls_wR_factor_ref         0.2151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7402
_reflns_number_total             8497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01237g2.cif
_cod_data_source_block           njy1
_cod_depositor_comments
'Adding full bibliography for 7231510--7231512.cif.'
_cod_database_code               7231510
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.724
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'