Green solvent free epoxidation of olefins by a heterogenised hydrazone-dioxidotungsten(vi) coordination compound
Heydari, Neda; Bikas, Rahman; Shaterian, Maryam; Lis, Tadeusz; RSC Advances 12 (2022) 4813–4827; doi:10.1039/D1RA09217K

data_7244380
_publ_section_title
;
 Green solvent free epoxidation of olefins by a heterogenised
 hydrazone-dioxidotungsten(vi) coordination compound
;
_journal_issue                   8
_journal_name_full               'RSC Advances'
_journal_page_first              4813
_journal_page_last               4827
_journal_paper_doi               10.1039/D1RA09217K
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C15 H14 Br N3 O5 W'
_chemical_formula_sum            'C15 H14 Br N3 O5 W'
_chemical_formula_weight         580.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2021-11-27 deposited with the CCDC.	2022-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                95.43(3)
_cell_angle_beta                 93.93(3)
_cell_angle_gamma                104.74(4)
_cell_formula_units_Z            2
_cell_length_a                   7.663(2)
_cell_length_b                   10.481(3)
_cell_length_c                   10.845(3)
_cell_measurement_reflns_used    7980
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.9
_cell_volume                     834.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Kuma KM4 kappa-geometry diffractometer with a CCD detector
;
_diffrn_measurement_method       w/
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7989
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.929
_exptl_absorpt_coefficient_mu    9.345
_exptl_absorpt_correction_T_max  0.264
_exptl_absorpt_correction_T_min  0.152
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
	model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.308
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.210
_refine_diff_density_max         1.362
_refine_diff_density_min         -1.723
_refine_diff_density_rms         0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0893P)^2^+0.4292P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3105
_reflns_number_total             3275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra09217k2.cif
_cod_data_source_block           pa107a
_cod_database_code               7244380
_shelx_estimated_absorpt_t_min   0.172
_shelx_estimated_absorpt_t_max   0.244
_shelxl_version_number           2013-2
_shelx_res_checksum              39580