A new phoshotungstate-supported rhenium carbonyl derivative: synthesis, characterization and catalytic selective oxidation of thiophenes
Niu, Jingyang; Lu, Jingkun; Feng, Junwei; Ma, Xinyi; Wang, Ping; Xu, Baijie; He, Peipei; Jia, Jiage; Ma, Pengtao; Wang, Jingping; CrystEngComm  (2019) –; doi:10.1039/C9CE01124B

data_7234764
_publ_section_title
;
 A new phoshotungstate-supported rhenium carbonyl derivative: synthesis,
 characterization and catalytic selective oxidation of thiophenes
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE01124B
_journal_year                    2019
_chemical_formula_moiety         'C6 O68 P2 Re2 W17, 6(C4 N), 7(O)'
_chemical_formula_sum            'C30 H83 N6 O75 P2 Re2 W17'
_chemical_formula_weight         5287.81
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2019-07-11 deposited with the CCDC.    2019-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.1534(16)
_cell_length_b                   13.4987(8)
_cell_length_c                   31.1648(19)
_cell_measurement_reflns_used    7137
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.19
_cell_volume                     11843.7(12)
_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-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0884
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            60380
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         1.587
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.581
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1312 before and 0.0595 after correction.
The Ratio of minimum to maximum transmission is 0.5950.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.966
_exptl_crystal_description       block
_exptl_crystal_F_000             9372
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.608
_refine_diff_density_min         -2.872
_refine_diff_density_rms         0.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         11004
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0606
_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^)+(0.0438P)^2^+476.1622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7540
_reflns_number_total             11004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01124b2.cif
_cod_data_source_block           njy1
_cod_database_code               7234764
_shelx_estimated_absorpt_t_max   0.119
_shelx_estimated_absorpt_t_min   0.090
_olex2_refinement_description
;
1. Restrained distances
 N2-C7 = N2-C8 = N2-C9
 1.47 with sigma of 0.02
 N3-C10 = N3-C11 = N3-C12
 1.47 with sigma of 0.02
 N4-C13 = N4-C14 = N4-C15
 1.47 with sigma of 0.02
 N5-C16 = N5-C17 = N5-C18
 1.47 with sigma of 0.02
 N6-C19 = N6-C20 = N6-C21
 1.47 with sigma of 0.02
 C7-C8 \\sim C7-C9 \\sim C8-C9
 with sigma of 0.02
 C10-C11 \\sim C10-C12 \\sim C11-C12
 with sigma of 0.02
 C13-C14 \\sim C13-C15 \\sim C14-C15 \\sim C13-C15_$1 \\sim C14-C15_$1 \\sim
C15-C15_$1
 with sigma of 0.02
 C16-C17 \\sim C16-C18 \\sim C17-C18
 with sigma of 0.02
 C19-C20 \\sim C19-C21 \\sim C20-C21 \\sim C19-C21_$2 \\sim C20-C21_$2 \\sim
C21-C21_$2
 with sigma of 0.02
2. Others
 Fixed Sof: O4W(0.5) O5W(0.5) O6W(0.5)
 Fixed Uiso: C12(0.19951) C14(0.18735) C16(0.20517) C17(0.2292) C18(0.16317)
 C19(0.1564) C20(0.19532) C21(0.21238)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'