2-Thia-1,3,5-triaza-7-phosphaadamantane-2,2-dioxide Revisited: Computational and Experimental Studies of a Neglected Phosphine
Sternberg, Michelle; Suresh, Cherumuttathu H.; Mohr, Fabian; Organometallics 29 (2010) 3922–; doi:10.1021/om100579e

data_4066700
_publ_section_title
;
 2-Thia-1,3,5-triaza-7-phosphaadamantane-2,2-dioxide Revisited:
 Computational and Experimental Studies of a Neglected Phosphine
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3922
_journal_paper_doi               10.1021/om100579e
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C17.25 H22 Cl2 N4 O2 P Pd S'
_chemical_formula_weight         557.72
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 111.010(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1513(3)
_cell_length_b                   18.4785(4)
_cell_length_c                   12.2060(4)
_cell_measurement_reflns_used    5738
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.3832
_cell_measurement_theta_min      3.0731
_cell_volume                     2137.39(11)
_computing_cell_refinement
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
;
_computing_data_collection
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
;
_computing_molecular_graphics
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 16.2705
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_details
;
 1 omega -90.00 -20.00 1.0000 26.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.5412 -77.0000 60.0000 70
 2 omega -91.00 -32.00 1.0000 26.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.5412 179.0000 30.0000 59
 3 omega -44.00 52.00 1.0000 26.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.5412 37.0000 -30.0000 96
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0304475
_diffrn_orient_matrix_UB_12      -0.0174144
_diffrn_orient_matrix_UB_13      -0.0369339
_diffrn_orient_matrix_UB_21      -0.0510002
_diffrn_orient_matrix_UB_22      0.0163596
_diffrn_orient_matrix_UB_23      -0.0497265
_diffrn_orient_matrix_UB_31      0.0455672
_diffrn_orient_matrix_UB_32      0.0300656
_diffrn_orient_matrix_UB_33      0.0056127
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9779
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         29.45
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    1.313
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.96023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
 (compiled Jan 5 2010,16:28:46)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1122
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.116
_refine_diff_density_min         -1.505
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         5002
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                3908
_reflns_number_total             5002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100579e_si_001.cif
_cod_data_source_block           FM448_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_cell_volume        2137.41(10)
_cod_database_code               4066700