V(iv), Fe(ii), Ni(ii) and Cu(ii) complexes bearing 2,2,2-tris(pyrazol-1-yl)ethyl methanesulfonate: application as catalysts for the cyclooctane oxidation
Silva, Telma F. S.; Rocha, Bruno G. M.; Guedes da Silva, M. Fátima C.; Martins, Luísa M. D. R. S.; Pombeiro, Armando J. L.; New J. Chem. 40 (2016) 528–; doi:10.1039/C5NJ01865J

data_7055177
_publ_section_title
;
 V(iv), Fe(ii), Ni(ii) and Cu(ii) complexes bearing
 2,2,2-tris(pyrazol-1-yl)ethyl methanesulfonate: application as catalysts
 for the cyclooctane oxidation
;
_journal_issue                   1
_journal_name_full               'New J. Chem.'
_journal_page_first              528
_journal_paper_doi               10.1039/C5NJ01865J
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C24 H28 Cu N12 O6 S2, 2(C F3 O3 S)'
_chemical_formula_sum            'C26 H28 Cu F6 N12 O12 S4'
_chemical_formula_weight         1006.38
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-10-24 deposited with the CCDC.
2015-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                101.763(3)
_cell_angle_beta                 103.543(2)
_cell_angle_gamma                100.003(3)
_cell_formula_units_Z            1
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_cell_length_b                   9.8695(8)
_cell_length_c                   12.5776(10)
_cell_measurement_reflns_used    3011
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.62
_cell_volume                     945.92(14)
_computing_cell_refinement       'Bruker SAINT'
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_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0320
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_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.964
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_diffrn_reflns_limit_l_min       -17
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_diffrn_reflns_theta_max         30.555
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_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  0.8789
_exptl_absorpt_correction_T_min  0.7672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
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_exptl_crystal_description       prism
_exptl_crystal_F_000             511
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_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.626
_refine_diff_density_min         -0.724
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0679
_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^)+(0.1452P)^2^+1.1242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1943
_refine_ls_wR_factor_ref         0.2237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3812
_reflns_number_total             5584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj01865j2.cif
_cod_data_source_block           Compound4
_cod_depositor_comments          'Adding full bibliography for 7055177.cif.'
_cod_database_code               7055177
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.725
_shelx_estimated_absorpt_t_max   0.854
_shelx_res_checksum              25067