Photochemical and Thermal Reactions of a 2H-Azaphosphirene Complex with Isonitriles
Ionescu, Emanuel; von Frantzius, Gerd; Jones, Peter G.; Streubel, Rainer; Organometallics 24 (2005) 2237–2240; doi:10.1021/om049014u

data_4060308
_publ_section_title
;
 Photochemical and Thermal Reactions of a 2H-Azaphosphirene Complex
 with Isonitriles
;
_journal_coden_ASTM              ORGND7
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2237
_journal_page_last               2240
_journal_paper_doi               10.1021/om049014u
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C13 H20 N O5 P Si2 W'
_chemical_formula_weight         541.30
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.219(3)
_cell_angle_beta                 89.975(3)
_cell_angle_gamma                81.823(3)
_cell_formula_units_Z            2
_cell_length_a                   6.9618(4)
_cell_length_b                   9.6073(8)
_cell_length_c                   16.1541(9)
_cell_measurement_reflns_used    7126
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30.539
_cell_measurement_theta_min      2.242
_cell_volume                     1022.98(12)
_computing_cell_refinement       'Bruker Saint'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker AXS Smart 1000CCD'
_diffrn_measurement_method       '\w- & \f-scan'
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19997
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    5.860
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.7289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    'PH free, rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         5954
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0185
_refine_ls_R_factor_gt           0.0159
_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^)+(0.0177P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0341
_refine_ls_wR_factor_ref         0.0346
_reflns_number_gt                5515
_reflns_number_total             5954
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049014usi20050215_124817.cif
_cod_data_source_block           ch
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'heavy-atom' was changed to
'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4060308