Extended π conjugation in 2H-1,4,2-diazaphosphole complexes
Helten, Holger; Daniels, Jörg; Nieger, Martin; Streubel, Rainer; New Journal of Chemistry 34 (2010) 1593–; doi:10.1039/c0nj00151a

data_7053542
_publ_section_title
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 Extended \p conjugation in 2H-1,4,2-diazaphosphole complexes
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_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1593
_journal_paper_doi               10.1039/c0nj00151a
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         'C22 H25 N2 O5 P S2 Si2 W'
_chemical_formula_sum            'C22 H25 N2 O5 P S2 Si2 W'
_chemical_formula_weight         732.56
_chemical_name_common
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(2-Bis(trimethylsilyl)methyl-3,5,-di(2-thienyl)-2H-1,4,2-
diazaphosphole-kappaP)pentacarbonyltungsten(0)
;
_chemical_name_systematic
;
[2-Bis(trimethylsilyl)methyl-3,5,-di(2-thienyl)-2H-1,4,2-diazaphosphole-
kappaP]pentacarbonyltungsten(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                75.868(2)
_cell_angle_beta                 84.937(2)
_cell_angle_gamma                65.551(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5035(3)
_cell_length_b                   10.9580(4)
_cell_length_c                   15.4221(7)
_cell_measurement_reflns_used    3746
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1417.64(10)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 2 deg.'
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13970
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    4.397
_exptl_absorpt_correction_T_max  0.53875
_exptl_absorpt_correction_T_min  0.36309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Platon, cf. Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.268
_refine_diff_density_min         -2.092
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         6484
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0300P)^2^+2.0372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0686
_reflns_number_gt                5969
_reflns_number_total             6484
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00151a.txt
_cod_data_source_block           str010_m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_original_cell_volume        1417.64(9)
_cod_database_code               7053542