Mixed guanidinato/alkylimido/azido tungsten(VI) complexes: synthesis and structural characterization.
Rische, Daniel; Baunemann, Arne; Winter, Manuela; Fischer, Roland A.; Inorganic chemistry 45 (2006) 269–277; doi:10.1021/ic0512431

data_4340288
_publ_section_title
;
 Mixed guanidinato/alkylimido/azido tungsten(VI) complexes: synthesis and
 structural characterization.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              269
_journal_page_last               277
_journal_paper_doi               10.1021/ic0512431
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C26 H46 N18 W2'
_chemical_formula_weight         978.51
_chemical_name_systematic
; 
 ? 
;
_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                93.330(5)
_cell_angle_beta                 100.474(5)
_cell_angle_gamma                96.270(5)
_cell_formula_units_Z            3
_cell_length_a                   10.6021(7)
_cell_length_b                   15.9447(10)
_cell_length_c                   16.8824(10)
_cell_measurement_reflns_used    4947
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.57
_cell_volume                     2780.7(3)
_computing_cell_refinement       'CrysAlis RED 1.171.13, Oxford Diffraction'
_computing_data_collection       'CrysAlis CCD 1.171.13, Oxford Diffraction'
_computing_data_reduction        'CrysAlis RED 1.171.13, Oxford Diffraction'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  SHELXTL-PLUS
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      105(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Sapphire2-CCD, Oxford Diffraction'
_diffrn_measurement_method       '560 images at 1.0 deg in \w and 15 sec'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_sigmaI/netI    0.1822
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31605
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    6.245
_exptl_absorpt_correction_T_max  0.743
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_type   'numeric analytical'
_exptl_absorpt_process_details   'Gaussian face-indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.896
_refine_diff_density_min         -1.800
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.666
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         15707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.666
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0059P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0573
_reflns_number_gt                7868
_reflns_number_total             15707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0512431si20050725_093124.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4340288