Synthesis, characterization and catalytic epoxidation properties of a new tellurotungstate(iv)-supported rhenium carbonyl derivative.
Lu, Jingkun; Ma, Xinyi; Wang, Ping; Feng, Junwei; Ma, Pengtao; Niu, Jingyang; Wang, Jingping; Dalton transactions (Cambridge, England : 2003) 48 (2019) 628–634; doi:10.1039/c8dt04195d

data_7048310
_publ_section_title
;
 Synthesis, characterization and catalytic epoxidation properties of a new
 tellurotungstate(iv)-supported rhenium carbonyl derivative.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              628
_journal_page_last               634
_journal_paper_doi               10.1039/c8dt04195d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '0.5(C12 Na4 O158 Re4 Te4 W40), 6(C4 H12 N)'
_chemical_formula_sum            'C30 H72 N6 Na2 O79 Re2 Te2 W20'
_chemical_formula_weight         6131.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-21 deposited with the CCDC.
2018-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.0550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.3974(9)
_cell_length_b                   19.6444(11)
_cell_length_c                   17.5409(10)
_cell_measurement_reflns_used    6611
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.38
_cell_volume                     5642.2(5)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0518
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28704
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.954
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.035
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1248 before and 0.0519 after correction.
The Ratio of minimum to maximum transmission is 0.5384.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.609
_exptl_crystal_description       block
_exptl_crystal_F_000             5364
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.811
_refine_diff_density_min         -1.412
_refine_diff_density_rms         0.360
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         10033
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0295P)^2^+268.1531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7724
_reflns_number_total             10033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04195d2.cif
_cod_data_source_block           1863573
_cod_depositor_comments          'Adding full bibliography for 7048310.cif.'
_cod_database_code               7048310
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.086
_shelx_estimated_absorpt_t_min   0.049
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C4 = N1-C5 = N1-C6 = N1-C7
 1.47 with sigma of 0.02
 N2-C8 = N2-C9 = N2-C10 = N2-C11
 1.47 with sigma of 0.02
 N3-C12 = N3-C13 = N3-C14 = N3-C15
 1.47 with sigma of 0.02
 C12-C13 \\sim C12-C14 \\sim C12-C15 \\sim C13-C14 \\sim C13-C15 \\sim C14-C15
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N3 \\sim C12 \\sim C13 \\sim C14 \\sim C15: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(O38) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C10) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(O2W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O2W(0.5)
5.a Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C)
5.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              67095
_shelx_fab_checksum              44297
_olex2_submission_special_instructions 'No special instructions were received'