Oxidations of (R3tach)M(CO)3 Complexes [M = Cr, Mo, W; R3tach = 1,3,5-Trialkyl-1,3,5-triazacyclohexane (R =t-Bu, Bn)]. Crystal Structures of (t-Bu3tach)MO3.15H2O (M = Mo, W)
Murray V. Baker; Michael R. North; Brian W. Skelton; Allan H. White; Inorganic Chemistry 38 (1999) 4515–4521; doi:10.1021/ic990031z

data_4322253
_publ_contact_author
;
     M.V.Baker
     University of Western Australia
     Department of Chemistry
     Nedlands  6907
     Western Australia
     Australia 
;
_publ_contact_author_email       mvb@chem.uwa.edu.au
_publ_contact_author_fax         (61)_8_9380-1005
_publ_contact_author_phone       (61)_8_9380-2576
_publ_section_title
;
 Oxidations of (R3tach)M(CO)3 Complexes [M = Cr, Mo, W; R3tach =
 1,3,5-Trialkyl-1,3,5-triazacyclohexane (R =t-Bu, Bn)]. Crystal Structures
 of (t-Bu3tach)MO3.15H2O (M = Mo, W)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4515
_journal_page_last               4521
_journal_paper_doi               10.1021/ic990031z
_journal_volume                  38
_journal_year                    1999
_chemical_formula_analytical     'C15 H63 N3 Mo O18'
_chemical_formula_structural     (C15H33N3)MoO3.15H2O
_chemical_formula_sum            'C15 H63 Mo N3 O18'
_chemical_formula_weight         669.61
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_audit_creation_date             98-07-12
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.00000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            6
_cell_length_a                   21.026(2)
_cell_length_b                   21.026(2)
_cell_length_c                   13.418(2)
_cell_measurement_reflns_used    4826
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      1.2
_cell_volume                     5137.3(10)
_computing_cell_refinement       'Bruker SAINT software'
_computing_data_collection       'Bruker Smart software'
_computing_data_reduction        'Bruker SAINT software'
_computing_molecular_graphics    xtal
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    xtal
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           Mo-K\a
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_diffrn_reflns_limit_l_min       -18
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_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.50
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
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_exptl_crystal_description       needle
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         .443
_refine_diff_density_min         -.63
_refine_ls_abs_structure_details Flack_xabs_refined
_refine_ls_abs_structure_Flack   0.05(7)
_refine_ls_extinction_coef       9630(513)
_refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   4.328
_refine_ls_goodness_of_fit_obs   3.747
_refine_ls_hydrogen_treatment    noref
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_refine_ls_number_constraints    0
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_refine_ls_number_reflns         1150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .042
_refine_ls_R_factor_obs          .028
_refine_ls_shift/esd_max         .031
_refine_ls_shift/esd_mean        .006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .043
_refine_ls_wR_factor_obs         .032
_reflns_d_resolution_high        .7
_reflns_d_resolution_low         9.993
_reflns_limit_h_max              24
_reflns_limit_h_min              0
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
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_reflns_observed_criterion       refl_observed_if_F____>4.000_sigma(F___)
_cod_data_source_file            ic990031z_2.cif
_cod_data_source_block           n3moo3
_cod_original_cell_volume        5137.3(12)
_cod_original_sg_symbol_Hall     r_3_-2"c
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_original_formula_sum        'C15 H63 N3 Mo O18'
_cod_database_code               4322253