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_4066699
_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            'C22 H26 Cl N4 O4 P Pd S'
_chemical_formula_weight         615.35
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.316(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2326(6)
_cell_length_b                   16.3432(8)
_cell_length_c                   10.3295(4)
_cell_measurement_reflns_used    5336
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.4238
_cell_measurement_theta_min      2.8803
_cell_volume                     2363.87(18)
_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 0.999
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_details
;
 1 omega 15.00 47.00 1.0000 120.0000
 omega____ theta____ kappa____ phi______ frames
 - 17.8225 63.0000 -7.0000 32
 2 omega -18.00 11.00 1.0000 120.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.5412 -77.0000 0.0000 29
 3 omega -64.00 -33.00 1.0000 120.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.5412 179.0000 -60.0000 31
 4 omega -90.00 -23.00 1.0000 120.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.5412 -77.0000 0.0000 67
 5 omega -84.00 -32.00 1.0000 120.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.5412 179.0000 30.0000 52
 6 omega -24.00 51.00 1.0000 120.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.5412 77.0000 -90.0000 75
 7 omega -90.00 -46.00 1.0000 120.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.5412 -77.0000 -180.0000 44
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0377452
_diffrn_orient_matrix_UB_12      0.0077567
_diffrn_orient_matrix_UB_13      0.053427
_diffrn_orient_matrix_UB_21      -0.027778
_diffrn_orient_matrix_UB_22      0.0309837
_diffrn_orient_matrix_UB_23      0.0231102
_diffrn_orient_matrix_UB_31      -0.0192414
_diffrn_orient_matrix_UB_32      -0.0293784
_diffrn_orient_matrix_UB_33      0.0385079
_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  0.0692
_diffrn_reflns_av_sigmaI/netI    0.1035
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15402
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         29.49
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.17233
_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    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.852
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0251P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                3625
_reflns_number_total             5656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100579e_si_001.cif
_cod_data_source_block           FM446_3
_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 
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_cod_original_cell_volume        2363.85(18)
_cod_database_code               4066699