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_4340284
_publ_section_title
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 Mixed guanidinato/alkylimido/azido tungsten(VI) complexes: synthesis and
 structural characterization.
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_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            'C18 H28 Cl2 N4 W'
_chemical_formula_weight         555.19
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4634(9)
_cell_length_b                   8.8987(4)
_cell_length_c                   14.9136(8)
_cell_measurement_reflns_used    7935
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      36.78
_cell_measurement_theta_min      2.73
_cell_volume                     2184.89(19)
_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      102(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Sapphire2-CCD, Oxford Diffraction'
_diffrn_measurement_method       '1109 images at 1.0 deg in \w and 15 sec'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39211
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    5.540
_exptl_absorpt_correction_T_max  0.526
_exptl_absorpt_correction_T_min  0.467
_exptl_absorpt_correction_type   'numeric analytical'
_exptl_absorpt_process_details   'Gaussian face-indexed'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.491
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.035(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4987
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                4281
_reflns_number_total             4987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0512431si20050725_093124.cif
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
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_cod_original_sg_symbol_H-M      Pna(2)1
_cod_database_code               4340284