1,3,5-Tris(thiocyanatomethyl)mesitylene as a Ligand. Pseudooctahedral Molybdenum, Manganese, and Rhenium Carbonyl Complexes and Copper and Silver Dimers. Copper-Catalyzed Carbene- and Nitrene-Transfer Reactions
Héctor Martínez-García; Dolores Morales; Julio Pérez; Marcos Puerto; Daniel Miguel; Inorganic Chemistry 49 (2010) 6974–6985; doi:10.1021/ic1006082

data_4316121
_publ_contact_author
;    JULIO PEREZ
     Departamento de Quimica Organica e Inorganica
     IUQOEM - Facultad de Quimica
     Universidad de Oviedo-CSIC
     C/ Julian Claveria s/n
     33006 Oviedo  (ASTURIAS)
     SPAIN
;
_publ_contact_author_email       moralesdolores.uo@uniovi.es
_publ_contact_author_fax         +34-85-103446
_publ_contact_author_phone       +34-85-103467
_publ_section_title
;
 1,3,5-Tris(thiocyanatomethyl)mesitylene as a Ligand. Pseudooctahedral
 Molybdenum, Manganese, and Rhenium Carbonyl Complexes and Copper and
 Silver Dimers. Copper-Catalyzed Carbene- and Nitrene-Transfer Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6974
_journal_page_last               6985
_journal_paper_doi               10.1021/ic1006082
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C47 H27 B Cu F24 N3 S3'
_chemical_formula_weight         1260.25
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.3460(9)
_cell_angle_beta                 84.7997(10)
_cell_angle_gamma                64.6597(11)
_cell_formula_units_Z            2
_cell_length_a                   13.1045(2)
_cell_length_b                   13.1857(2)
_cell_length_c                   16.1827(2)
_cell_measurement_reflns_used    7798
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.0
_cell_measurement_theta_min      2.0
_cell_volume                     2490.84(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor, 1997) 
;
_computing_molecular_graphics    'PLATON (Spek, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
  Patterson methods - DIRDIF-99 (Beurskens, 1999) 
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       '90 mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            39612
_diffrn_reflns_theta_full        68.31
_diffrn_reflns_theta_max         68.31
_diffrn_reflns_theta_min         2.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.982
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.205
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         9011
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0684
_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^)+(0.0823P)^2^+4.8825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1781
_refine_ls_wR_factor_ref         0.1861
_reflns_number_gt                7792
_reflns_number_total             9011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1006082_si_002_6.cif
_cod_data_source_block           Compound_8_hm390
_cod_original_cell_volume        2490.85(7)
_cod_database_code               4316121