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_7231511
_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), Cl0.6 O17 V6, 3(O), 0.4(Cl)'
_chemical_formula_sum            'C72 H48 Cl N12 O20 Ru2 V6'
_chemical_formula_weight         1944.45
_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             2017-07-04
_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                104.610(2)
_cell_angle_beta                 116.152(2)
_cell_angle_gamma                91.609(2)
_cell_formula_units_Z            2
_cell_length_a                   16.2890(17)
_cell_length_b                   16.4760(17)
_cell_length_c                   18.003(2)
_cell_measurement_reflns_used    8385
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.67
_cell_measurement_theta_min      2.34
_cell_volume                     4142.5(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21429
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.551
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0431 before and 0.0336 after correction.
The Ratio of minimum to maximum transmission is 0.9246.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1934
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.701
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         14590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0926
_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^)+(0.1676P)^2^+25.6889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2562
_refine_ls_wR_factor_ref         0.2771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11623
_reflns_number_total             14590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01237g2.cif
_cod_data_source_block           njy1_a
_cod_depositor_comments
'Adding full bibliography for 7231510--7231512.cif.'
_cod_original_cell_volume        4142.6(8)
_cod_database_code               7231511
_shelx_estimated_absorpt_t_max   0.826
_shelx_estimated_absorpt_t_min   0.733
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: Cl1(0.6) Cl2(0.2) Cl3(0.2)
3.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),
 C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46),
  C49(H49), C50(H50), C51(H51), C53(H53), C54(H54), C56(H56), C57(H57),
 C58(H58), C61(H61), C62(H62), C63(H63), C65(H65), C66(H66), C68(H68), C69(H69),
  C70(H70)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'