Pentacarbonyl{<i>N</i>,<i>N</i>-dimethyl-<i>N</i>'-[4-(pyridin-4-ylethynyl-κ<i>N</i>)benzylidene]benzene-1,4-diamine}tungsten(0)
Huang, Ping-Hsin; Wen, Yuh-Sheng; Acta Crystallographica Section E 63 (2007) m563–m564; doi:10.1107/S1600536807002152

data_2212415
_publ_section_title
Pentacarbonyl{<i>N</i>,<i>N</i>-dimethyl-<i>N</i>'-[4-(pyridin-4-ylethynyl-\k<i>N</i>)benzylidene]benzene-1,4-diamine}tungsten(0)
_journal_coeditor_code           WW2078
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m563
_journal_page_last               m564
_journal_paper_doi               10.1107/S1600536807002152
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[W (C22 H19 N3) (C1 O1)5]'
_chemical_formula_moiety         'C27 H19 N3 O5 W'
_chemical_formula_sum            'C27 H19 N3 O5 W'
_chemical_formula_weight         649.30
_chemical_name_systematic
;Pentacarbonyl{N,N-dimethyl-N'-[4-(pyridin-4-ylethynyl-\kN)benzylidene]benzene-
1,4-diamine}tungsten(0)
;
_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                102.5950(10)
_cell_angle_beta                 95.3620(10)
_cell_angle_gamma                93.2490(10)
_cell_formula_units_Z            4
_cell_length_a                   12.2258(2)
_cell_length_b                   12.5046(2)
_cell_length_c                   17.3157(3)
_cell_measurement_reflns_used    9811
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.3
_cell_measurement_theta_min      2.44
_cell_volume                     2564.09(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39209
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.21
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.546
_exptl_absorpt_correction_T_max  0.9856
_exptl_absorpt_correction_T_min  0.4934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_meas      1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.940
_refine_ls_extinction_coef       0.00043(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         9009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0204P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0485
_reflns_number_gt                7221
_reflns_number_total             9009
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ww2078.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2212415
_cod_database_fobs_code          2212415